#"Weakferromagnetism and Strong Spin-Spin Interaction
# Mediated by the Mixed-Valence Ethynyl-TTF type Ligand"
#J. Nishijo, K. Judai and N. Nishi
 
data_[CrCyclam(C2MeEDT)2][ClO4]2(PhCl)2(MeCN) 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             '[CrCyclam(C2MeEDT)2][ClO4]2(PhCl)2(MeCN)' 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C46 H51 Cl4 Cr N5 O8 S12' 
_chemical_formula_weight          1380.44 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0033   0.0016 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0106   0.0060 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'N'  'N'   0.0061   0.0033 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'S'  'S'   0.1246   0.1234 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Cl'  'Cl'   0.1484   0.1585 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Cr'  'Cr'   0.3209   0.6236 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            'Monoclinic' 
_symmetry_space_group_name_H-M    'C2/c' 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y, -z+1/2' 
 'x+1/2, y+1/2, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y, z-1/2' 
 '-x+1/2, -y+1/2, -z' 
 'x+1/2, -y+1/2, z-1/2' 
 
_cell_length_a                    32.921(4) 
_cell_length_b                    11.8484(11) 
_cell_length_c                    16.1400(16) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  103.151(3) 
_cell_angle_gamma                 90.00 
_cell_volume                      6130.4(11) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     9580 
_cell_measurement_theta_min       1.2703 
_cell_measurement_theta_max       30.5746 
 
_exptl_crystal_description        Rod 
_exptl_crystal_colour             Black 
_exptl_crystal_size_max           1.4 
_exptl_crystal_size_mid           0.2 
_exptl_crystal_size_min           0.15 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.496 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              2840 
_exptl_absorpt_coefficient_mu     0.822 
_exptl_absorpt_correction_type    'Numerical' 
_exptl_absorpt_correction_T_min   0.7113 
_exptl_absorpt_correction_T_max   0.9222 
_exptl_absorpt_process_details    ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       293(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'Rotating Anode' 
_diffrn_radiation_monochromator   'Graphite Monochromator' 
_diffrn_measurement_device_type   'Rigaku AFC7R with CCD detector' 
_diffrn_radiation_detector              'CCD'
_diffrn_measurement_device        'Mercury (2x2 bin mode)'
_diffrn_measurement_method        ω-2θ 
_diffrn_detector_area_resol_mean  14.6306 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             30420 
_diffrn_reflns_av_R_equivalents   0.0360 
_diffrn_reflns_av_sigmaI/netI     0.0340 
_diffrn_reflns_limit_h_min        -45 
_diffrn_reflns_limit_h_max        36 
_diffrn_reflns_limit_k_min        -15 
_diffrn_reflns_limit_k_max        15 
_diffrn_reflns_limit_l_min        -15 
_diffrn_reflns_limit_l_max        20 
_diffrn_reflns_theta_min          1.27 
_diffrn_reflns_theta_max          30.67 
_reflns_number_total              7593 
_reflns_number_gt                 5697 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'CrystalClear (Rigaku/MSC Inc., 2006)' 
_computing_cell_refinement        'CrystalClear (Rigaku/MSC Inc., 2006)' 
_computing_data_reduction         'CrystalClear (Rigaku/MSC Inc., 2006)' 
_computing_structure_solution     'SIR2004 (M. C. Burla et al.)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
; 
 
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc  
_refine_ls_weighting_details 
 'calc w=1/[σ²(Fo²)+(0.1944P)²+5.3182P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     constr 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          7593 
_refine_ls_number_parameters      331 
_refine_ls_number_restraints      3 
_refine_ls_R_factor_all           0.1125 
_refine_ls_R_factor_gt            0.0946 
_refine_ls_wR_factor_ref          0.3172 
_refine_ls_wR_factor_gt           0.2882 
_refine_ls_goodness_of_fit_ref    1.142 
_refine_ls_restrained_S_all       1.143 
_refine_ls_shift/su_max           0.009 
_refine_ls_shift/su_mean          0.000 
 
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Cr1 Cr 0.7500 0.2500 0.5000 0.0397(3) Uani 1 2 d S . . 
S1 S 0.92354(3) 0.33344(12) 0.50332(7) 0.0623(4) Uani 1 1 d . . . 
S2 S 0.92639(3) 0.43441(13) 0.33956(7) 0.0634(4) Uani 1 1 d . . . 
S3 S 1.02451(4) 0.31265(14) 0.54885(8) 0.0722(4) Uani 1 1 d . . . 
S4 S 1.02618(3) 0.41491(16) 0.38393(8) 0.0768(5) Uani 1 1 d . . . 
S5 S 1.11515(4) 0.27452(16) 0.59978(10) 0.0794(4) Uani 1 1 d . . . 
S6 S 1.11611(4) 0.39725(18) 0.40185(10) 0.0875(5) Uani 1 1 d . . . 
N1 N 0.77546(11) 0.0932(3) 0.5348(2) 0.0490(7) Uani 1 1 d . . . 
H1 H 0.7567 0.0546 0.5574 0.059 Uiso 1 1 calc R . . 
N2 N 0.73421(11) 0.1851(3) 0.3778(2) 0.0486(7) Uani 1 1 d . . . 
H2 H 0.7541 0.2087 0.3508 0.058 Uiso 1 1 calc R . . 
C1 C 0.80684(15) 0.2785(4) 0.6756(3) 0.0590(10) Uani 1 1 d . . . 
H1A H 0.8099 0.3090 0.7325 0.071 Uiso 1 1 calc R . . 
H1B H 0.8290 0.3096 0.6519 0.071 Uiso 1 1 calc R . . 
C2 C 0.81144(17) 0.1520(5) 0.6812(3) 0.0659(12) Uani 1 1 d . . . 
H2A H 0.7874 0.1211 0.6987 0.079 Uiso 1 1 calc R . . 
H2B H 0.8359 0.1342 0.7253 0.079 Uiso 1 1 calc R . . 
C3 C 0.81540(15) 0.0934(4) 0.5999(3) 0.0599(11) Uani 1 1 d . . . 
H3A H 0.8366 0.1312 0.5770 0.072 Uiso 1 1 calc R . . 
H3B H 0.8244 0.0161 0.6128 0.072 Uiso 1 1 calc R . . 
C4 C 0.77763(15) 0.0348(4) 0.4537(3) 0.0586(10) Uani 1 1 d . . . 
H4A H 0.7802 -0.0460 0.4630 0.070 Uiso 1 1 calc R . . 
H4B H 0.8019 0.0608 0.4345 0.070 Uiso 1 1 calc R . . 
C5 C 0.73867(15) 0.0604(4) 0.3874(3) 0.0562(10) Uani 1 1 d . . . 
H5A H 0.7404 0.0266 0.3336 0.067 Uiso 1 1 calc R . . 
H5B H 0.7146 0.0291 0.4045 0.067 Uiso 1 1 calc R . . 
C6 C 0.80614(11) 0.3040(3) 0.4765(2) 0.0441(8) Uani 1 1 d . . . 
C7 C 0.83837(13) 0.3311(4) 0.4578(3) 0.0497(9) Uani 1 1 d . . . 
C8 C 0.84011(14) 0.4377(5) 0.2878(3) 0.0610(11) Uani 1 1 d . . . 
H8A H 0.8334 0.3756 0.2490 0.091 Uiso 1 1 calc R . . 
H8B H 0.8464 0.5031 0.2578 0.091 Uiso 1 1 calc R . . 
H8C H 0.8168 0.4537 0.3124 0.091 Uiso 1 1 calc R . . 
C9 C 0.87581(12) 0.3608(4) 0.4326(3) 0.0490(9) Uani 1 1 d . . . 
C10 C 0.87704(12) 0.4081(4) 0.3564(3) 0.0513(9) Uani 1 1 d . . . 
C11 C 0.95422(13) 0.3783(5) 0.4356(3) 0.0630(12) Uani 1 1 d . . . 
C12 C 0.99646(13) 0.3706(5) 0.4550(3) 0.0654(13) Uani 1 1 d . . . 
C13 C 1.07312(14) 0.3251(5) 0.5216(3) 0.0633(12) Uani 1 1 d . . . 
C14 C 1.07390(14) 0.3706(5) 0.4476(3) 0.0656(13) Uani 1 1 d . . . 
C15 C 1.15358(18) 0.2587(5) 0.5354(5) 0.0808(17) Uani 1 1 d . . . 
H15A H 1.1801 0.2374 0.5720 0.097 Uiso 1 1 calc R . . 
H15B H 1.1449 0.1981 0.4948 0.097 Uiso 1 1 calc R . . 
C16 C 1.15952(16) 0.3659(5) 0.4873(4) 0.0745(14) Uani 1 1 d . . . 
H16A H 1.1843 0.3578 0.4648 0.089 Uiso 1 1 calc R . . 
H16B H 1.1641 0.4288 0.5268 0.089 Uiso 1 1 calc R . . 
Cl2 Cl 0.76918(4) -0.18315(10) 0.66725(8) 0.0624(3) Uani 1 1 d . . . 
O1 O 0.74082(15) -0.0958(4) 0.6361(4) 0.1038(15) Uani 1 1 d . . . 
O2 O 0.79025(19) -0.1513(6) 0.7506(3) 0.121(2) Uani 1 1 d . . . 
O3 O 0.7997(2) -0.1917(5) 0.6186(4) 0.128(2) Uani 1 1 d . . . 
O4 O 0.74753(19) -0.2853(4) 0.6747(4) 0.119(2) Uani 1 1 d . . . 
C93 C 0.9212(3) 0.0567(7) 0.4158(7) 0.160(5) Uani 1 1 d G . . 
C94 C 0.9616(3) 0.0818(9) 0.4096(8) 0.184(6) Uani 1 1 d G . . 
H94 H 0.9839 0.0691 0.4557 0.221 Uiso 1 1 calc R . . 
C95 C 0.9688(3) 0.1258(9) 0.3344(11) 0.232(10) Uani 1 1 d G . . 
H95 H 0.9959 0.1426 0.3303 0.279 Uiso 1 1 calc R . . 
C96 C 0.9356(5) 0.1448(9) 0.2654(8) 0.219(8) Uani 1 1 d G . . 
H96 H 0.9404 0.1743 0.2151 0.263 Uiso 1 1 calc R . . 
C97 C 0.8952(4) 0.1197(9) 0.2716(8) 0.187(7) Uani 1 1 d G . . 
H97 H 0.8729 0.1324 0.2255 0.225 Uiso 1 1 calc R . . 
C98 C 0.8879(2) 0.0757(8) 0.3468(9) 0.229(11) Uani 1 1 d G . . 
H98 H 0.8609 0.0589 0.3510 0.275 Uiso 1 1 calc R . . 
Cl1 Cl 0.91426(19) 0.0047(5) 0.5119(4) 0.224(2) Uani 1 1 d . . . 
C90 C 0.9245(4) 0.2636(12) 0.7171(9) 0.088(3) Uiso 0.50 1 d PD . . 
H90A H 0.9125 0.2196 0.6676 0.133 Uiso 0.50 1 calc PR . . 
H90B H 0.9155 0.3406 0.7079 0.133 Uiso 0.50 1 calc PR . . 
H90C H 0.9156 0.2339 0.7654 0.133 Uiso 0.50 1 calc PR . . 
C91 C 0.9686(7) 0.259(2) 0.7323(17) 0.158(9) Uiso 0.50 1 d PD . . 
N92 N 1.0000 0.312(4) 0.7500 0.44(3) Uiso 1 2 d SD . . 
 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
 
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
Cr1 N1 2.063(3) 7_656 ? 
Cr1 N1 2.063(3) . ? 
Cr1 C6 2.070(3) 7_656 ? 
Cr1 C6 2.070(3) . ? 
Cr1 N2 2.070(3) 7_656 ? 
Cr1 N2 2.070(3) . ? 
S1 C11 1.732(4) . ? 
S1 C9 1.750(4) . ? 
S2 C10 1.735(4) . ? 
S2 C11 1.743(5) . ? 
S3 C12 1.726(5) . ? 
S3 C13 1.760(5) . ? 
S4 C12 1.750(4) . ? 
S4 C14 1.751(5) . ? 
S5 C13 1.752(5) . ? 
S5 C15 1.821(6) . ? 
S6 C14 1.744(5) . ? 
S6 C16 1.785(6) . ? 
N1 C3 1.484(6) . ? 
N1 C4 1.496(6) . ? 
N2 C5 1.489(6) . ? 
N2 C1 1.492(6) 7_656 ? 
C1 N2 1.492(6) 7_656 ? 
C1 C2 1.507(7) . ? 
C2 C3 1.517(7) . ? 
C4 C5 1.502(7) . ? 
C6 C7 1.211(5) . ? 
C7 C9 1.427(5) . ? 
C8 C10 1.488(6) . ? 
C9 C10 1.360(6) . ? 
C11 C12 1.357(6) . ? 
C13 C14 1.317(7) . ? 
C15 C16 1.523(9) . ? 
Cl2 O1 1.408(5) . ? 
Cl2 O3 1.413(5) . ? 
Cl2 O2 1.418(5) . ? 
Cl2 O4 1.424(5) . ? 
C93 C94 1.3900 . ? 
C93 C98 1.3900 . ? 
C93 Cl1 1.732(12) . ? 
C94 C95 1.3900 . ? 
C95 C96 1.3900 . ? 
C96 C97 1.3900 . ? 
C97 C98 1.3900 . ? 
C90 C91 1.418(17) . ? 
C91 N92 1.188(17) . ? 
C91 C91 2.02(4) 2_756 ? 
N92 C91 1.188(17) 2_756 ? 
 
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
N1 Cr1 N1 179.997(1) 7_656 . ? 
N1 Cr1 C6 90.20(15) 7_656 7_656 ? 
N1 Cr1 C6 89.80(15) . 7_656 ? 
N1 Cr1 C6 89.80(15) 7_656 . ? 
N1 Cr1 C6 90.20(15) . . ? 
C6 Cr1 C6 179.999(1) 7_656 . ? 
N1 Cr1 N2 85.57(14) 7_656 7_656 ? 
N1 Cr1 N2 94.43(14) . 7_656 ? 
C6 Cr1 N2 88.95(14) 7_656 7_656 ? 
C6 Cr1 N2 91.05(14) . 7_656 ? 
N1 Cr1 N2 94.43(14) 7_656 . ? 
N1 Cr1 N2 85.56(14) . . ? 
C6 Cr1 N2 91.05(14) 7_656 . ? 
C6 Cr1 N2 88.95(14) . . ? 
N2 Cr1 N2 179.999(1) 7_656 . ? 
C11 S1 C9 95.6(2) . . ? 
C10 S2 C11 96.5(2) . . ? 
C12 S3 C13 94.8(2) . . ? 
C12 S4 C14 95.0(2) . . ? 
C13 S5 C15 99.3(3) . . ? 
C14 S6 C16 102.1(3) . . ? 
C3 N1 C4 114.1(3) . . ? 
C3 N1 Cr1 115.5(3) . . ? 
C4 N1 Cr1 106.0(3) . . ? 
C5 N2 C1 113.7(3) . 7_656 ? 
C5 N2 Cr1 105.8(3) . . ? 
C1 N2 Cr1 116.2(3) 7_656 . ? 
N2 C1 C2 112.8(4) 7_656 . ? 
C1 C2 C3 115.6(4) . . ? 
N1 C3 C2 112.1(4) . . ? 
N1 C4 C5 109.1(4) . . ? 
N2 C5 C4 108.8(3) . . ? 
C7 C6 Cr1 175.5(3) . . ? 
C6 C7 C9 177.7(4) . . ? 
C10 C9 C7 124.3(4) . . ? 
C10 C9 S1 117.3(3) . . ? 
C7 C9 S1 118.3(3) . . ? 
C9 C10 C8 125.6(4) . . ? 
C9 C10 S2 115.9(3) . . ? 
C8 C10 S2 118.5(3) . . ? 
C12 C11 S1 123.2(4) . . ? 
C12 C11 S2 122.4(4) . . ? 
S1 C11 S2 114.5(2) . . ? 
C11 C12 S3 123.0(4) . . ? 
C11 C12 S4 121.6(4) . . ? 
S3 C12 S4 115.3(2) . . ? 
C14 C13 S5 128.2(4) . . ? 
C14 C13 S3 117.9(4) . . ? 
S5 C13 S3 113.9(3) . . ? 
C13 C14 S6 129.8(4) . . ? 
C13 C14 S4 117.1(3) . . ? 
S6 C14 S4 113.1(3) . . ? 
C16 C15 S5 113.1(4) . . ? 
C15 C16 S6 113.2(4) . . ? 
O1 Cl2 O3 110.6(4) . . ? 
O1 Cl2 O2 106.6(4) . . ? 
O3 Cl2 O2 106.9(4) . . ? 
O1 Cl2 O4 110.6(3) . . ? 
O3 Cl2 O4 114.8(4) . . ? 
O2 Cl2 O4 107.0(4) . . ? 
C94 C93 C98 120.0 . . ? 
C94 C93 Cl1 117.6(9) . . ? 
C98 C93 Cl1 122.4(9) . . ? 
C95 C94 C93 120.0 . . ? 
C94 C95 C96 120.0 . . ? 
C97 C96 C95 120.0 . . ? 
C96 C97 C98 120.0 . . ? 
C97 C98 C93 120.0 . . ? 
N92 C91 C90 145(3) . . ? 
N92 C91 C91 32(2) . 2_756 ? 
C90 C91 C91 173(3) . 2_756 ? 
C91 N92 C91 116(4) 2_756 . ? 
 
_diffrn_measured_fraction_theta_max    30.5746 
_diffrn_reflns_theta_full              30.5746 
_diffrn_measured_fraction_theta_full   80.1000 
_refine_diff_density_max    1.750 
_refine_diff_density_min   -0.802 
_refine_diff_density_rms    0.152 

#===END 

data_[CrCyclam(C2MeEDT)2][BF4]2(PhCl)2(MeCN) 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             '[CrCyclam(C2MeEDT)2][BF4]2(PhCl)2(MeCN)' 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C46 H51 B2 Cl2 Cr F8 N5 S12' 
_chemical_formula_weight          1355.16 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0033   0.0016 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'B'  'B'   0.0013   0.0007 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'N'  'N'   0.0061   0.0033 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'F'  'F'   0.0171   0.0103 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'S'  'S'   0.1246   0.1234 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Cl'  'Cl'   0.1484   0.1585 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Cr'  'Cr'   0.3209   0.6236 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            'Monoclinic' 
_symmetry_space_group_name_H-M    'C2/c' 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y, -z+1/2' 
 'x+1/2, y+1/2, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y, z-1/2' 
 '-x+1/2, -y+1/2, -z' 
 'x+1/2, -y+1/2, z-1/2' 
 
_cell_length_a                    32.828(3) 
_cell_length_b                    11.8716(11) 
_cell_length_c                    16.1111(16) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  103.469(3) 
_cell_angle_gamma                 90.00 
_cell_volume                      6106.1(10) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     11244 
_cell_measurement_theta_min       1.2756 
_cell_measurement_theta_max       30.5214 
 
_exptl_crystal_description        Rod 
_exptl_crystal_colour             Black 
_exptl_crystal_size_max           0.5 
_exptl_crystal_size_mid           0.2 
_exptl_crystal_size_min           0.2 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.474 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              2776 
_exptl_absorpt_coefficient_mu     0.747 
_exptl_absorpt_correction_type    'Numerical' 
_exptl_absorpt_correction_T_min   0.8017 
_exptl_absorpt_correction_T_max   0.9565 
_exptl_absorpt_process_details    ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       293(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'Rotating Anode' 
_diffrn_radiation_monochromator   'Graphite Monochromator' 
_diffrn_measurement_device_type   'Rigaku AFC7R with CCD detector' 
_diffrn_radiation_detector              'CCD'
_diffrn_measurement_device        'Mercury (2x2 bin mode)'
_diffrn_measurement_method        ω-2θ 
_diffrn_detector_area_resol_mean  14.6306 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             30415 
_diffrn_reflns_av_R_equivalents   0.0292 
_diffrn_reflns_av_sigmaI/netI     0.0292 
_diffrn_reflns_limit_h_min        -39 
_diffrn_reflns_limit_h_max        42 
_diffrn_reflns_limit_k_min        -15 
_diffrn_reflns_limit_k_max        14 
_diffrn_reflns_limit_l_min        -17 
_diffrn_reflns_limit_l_max        20 
_diffrn_reflns_theta_min          1.28 
_diffrn_reflns_theta_max          30.64 
_reflns_number_total              7850 
_reflns_number_gt                 6150 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'CrystalClear (Rigaku/MSC Inc., 2006)' 
_computing_cell_refinement        'CrystalClear (Rigaku/MSC Inc., 2006)' 
_computing_data_reduction         'CrystalClear (Rigaku/MSC Inc., 2006)' 
_computing_structure_solution     'SIR2004 (M. C. Burla et al.)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
; 
 
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc  
_refine_ls_weighting_details 
 'calc w=1/[σ²(Fo²)+(0.1878P)²+7.8404P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     constr 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          7850 
_refine_ls_number_parameters      331 
_refine_ls_number_restraints      3 
_refine_ls_R_factor_all           0.1052 
_refine_ls_R_factor_gt            0.0901 
_refine_ls_wR_factor_ref          0.3082 
_refine_ls_wR_factor_gt           0.2844 
_refine_ls_goodness_of_fit_ref    1.129 
_refine_ls_restrained_S_all       1.131 
_refine_ls_shift/su_max           0.023 
_refine_ls_shift/su_mean          0.001 
 
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Cr1 Cr 0.7500 0.2500 0.5000 0.0380(2) Uani 1 2 d S . . 
S1 S 0.92479(3) 0.33404(11) 0.50567(7) 0.0570(3) Uani 1 1 d . . . 
S2 S 0.92625(3) 0.43442(12) 0.34061(7) 0.0584(3) Uani 1 1 d . . . 
S3 S 1.02605(3) 0.31189(13) 0.54884(7) 0.0654(4) Uani 1 1 d . . . 
S4 S 1.02649(3) 0.41344(14) 0.38312(7) 0.0690(4) Uani 1 1 d . . . 
S5 S 1.11732(4) 0.27566(14) 0.59927(9) 0.0712(4) Uani 1 1 d . . . 
S6 S 1.11671(4) 0.39762(17) 0.39989(9) 0.0796(5) Uani 1 1 d . . . 
N1 N 0.77455(10) 0.0921(3) 0.5367(2) 0.0470(7) Uani 1 1 d . . . 
H1 H 0.7551 0.0547 0.5581 0.056 Uiso 1 1 calc R . . 
N2 N 0.73533(10) 0.1839(3) 0.3770(2) 0.0470(7) Uani 1 1 d . . . 
H2 H 0.7557 0.2064 0.3509 0.056 Uiso 1 1 calc R . . 
C1 C 0.80534(14) 0.2799(4) 0.6777(3) 0.0599(11) Uani 1 1 d . . . 
H1A H 0.8083 0.3116 0.7343 0.072 Uiso 1 1 calc R . . 
H1B H 0.8279 0.3092 0.6543 0.072 Uiso 1 1 calc R . . 
C2 C 0.80939(16) 0.1516(5) 0.6850(3) 0.0671(12) Uani 1 1 d . . . 
H2A H 0.7847 0.1221 0.7010 0.081 Uiso 1 1 calc R . . 
H2B H 0.8334 0.1337 0.7308 0.081 Uiso 1 1 calc R . . 
C3 C 0.81432(14) 0.0908(4) 0.6042(3) 0.0608(11) Uani 1 1 d . . . 
H3A H 0.8363 0.1270 0.5826 0.073 Uiso 1 1 calc R . . 
H3B H 0.8227 0.0134 0.6181 0.073 Uiso 1 1 calc R . . 
C4 C 0.77744(15) 0.0330(4) 0.4569(3) 0.0583(10) Uani 1 1 d . . . 
H4A H 0.7793 -0.0477 0.4667 0.070 Uiso 1 1 calc R . . 
H4B H 0.8024 0.0572 0.4393 0.070 Uiso 1 1 calc R . . 
C5 C 0.73915(15) 0.0598(4) 0.3884(3) 0.0571(10) Uani 1 1 d . . . 
H5A H 0.7413 0.0248 0.3352 0.069 Uiso 1 1 calc R . . 
H5B H 0.7144 0.0303 0.4041 0.069 Uiso 1 1 calc R . . 
C6 C 0.80728(11) 0.3022(3) 0.4794(2) 0.0442(7) Uani 1 1 d . . . 
C7 C 0.83899(12) 0.3297(3) 0.4605(3) 0.0485(8) Uani 1 1 d . . . 
C8 C 0.83989(13) 0.4337(5) 0.2885(3) 0.0623(11) Uani 1 1 d . . . 
H8A H 0.8320 0.3682 0.2534 0.093 Uiso 1 1 calc R . . 
H8B H 0.8467 0.4940 0.2544 0.093 Uiso 1 1 calc R . . 
H8C H 0.8170 0.4560 0.3126 0.093 Uiso 1 1 calc R . . 
C9 C 0.87631(11) 0.3598(3) 0.4348(2) 0.0452(8) Uani 1 1 d . . . 
C10 C 0.87723(11) 0.4067(4) 0.3586(2) 0.0475(8) Uani 1 1 d . . . 
C11 C 0.95462(12) 0.3800(4) 0.4364(3) 0.0554(10) Uani 1 1 d . . . 
C12 C 0.99729(12) 0.3712(5) 0.4548(3) 0.0576(10) Uani 1 1 d . . . 
C13 C 1.07453(12) 0.3243(4) 0.5216(3) 0.0567(10) Uani 1 1 d . . . 
C14 C 1.07479(13) 0.3705(5) 0.4464(3) 0.0589(11) Uani 1 1 d . . . 
C15 C 1.15437(15) 0.2585(5) 0.5339(4) 0.0750(15) Uani 1 1 d . . . 
H15A H 1.1811 0.2363 0.5700 0.090 Uiso 1 1 calc R . . 
H15B H 1.1449 0.1979 0.4937 0.090 Uiso 1 1 calc R . . 
C16 C 1.16071(14) 0.3642(5) 0.4844(4) 0.0688(13) Uani 1 1 d . . . 
H16A H 1.1851 0.3536 0.4608 0.083 Uiso 1 1 calc R . . 
H16B H 1.1664 0.4273 0.5236 0.083 Uiso 1 1 calc R . . 
B1 B 0.76861(18) -0.1829(5) 0.6672(4) 0.0618(12) Uani 1 1 d . . . 
F1 F 0.74120(13) -0.0969(3) 0.6355(3) 0.1062(13) Uani 1 1 d . . . 
F2 F 0.78797(14) -0.1550(5) 0.7502(2) 0.1171(16) Uani 1 1 d . . . 
F3 F 0.79959(17) -0.1902(5) 0.6243(3) 0.1264(17) Uani 1 1 d . . . 
F4 F 0.74795(15) -0.2813(4) 0.6699(4) 0.1250(18) Uani 1 1 d . . . 
C93 C 0.9212(2) 0.0569(6) 0.4192(5) 0.129(3) Uani 1 1 d G . . 
C94 C 0.96136(19) 0.0839(7) 0.4115(6) 0.145(4) Uani 1 1 d G . . 
H94 H 0.9842 0.0719 0.4571 0.174 Uiso 1 1 calc R . . 
C95 C 0.9674(2) 0.1287(8) 0.3355(7) 0.179(6) Uani 1 1 d G . . 
H95 H 0.9943 0.1467 0.3304 0.215 Uiso 1 1 calc R . . 
C96 C 0.9333(4) 0.1465(7) 0.2673(6) 0.186(6) Uani 1 1 d G . . 
H96 H 0.9374 0.1765 0.2165 0.223 Uiso 1 1 calc R . . 
C97 C 0.8932(3) 0.1195(7) 0.2750(6) 0.156(5) Uani 1 1 d G . . 
H97 H 0.8704 0.1314 0.2294 0.188 Uiso 1 1 calc R . . 
C98 C 0.88712(17) 0.0747(6) 0.3509(7) 0.147(5) Uani 1 1 d G . . 
H98 H 0.8602 0.0566 0.3561 0.177 Uiso 1 1 calc R . . 
Cl1 Cl 0.91397(15) 0.0051(4) 0.5132(3) 0.1969(18) Uani 1 1 d . . . 
C90 C 0.9260(4) 0.2535(10) 0.7190(8) 0.079(3) Uiso 0.50 1 d PD . . 
H90A H 0.9160 0.1946 0.6785 0.118 Uiso 0.50 1 calc PR . . 
H90B H 0.9132 0.3236 0.6974 0.118 Uiso 0.50 1 calc PR . . 
H90C H 0.9189 0.2361 0.7721 0.118 Uiso 0.50 1 calc PR . . 
C91 C 0.9706(6) 0.263(2) 0.7323(18) 0.162(9) Uiso 0.50 1 d PD . . 
N92 N 1.0000 0.3257(16) 0.7500 0.189(6) Uiso 1 2 d SD . . 
 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
 
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
Cr1 N1 2.071(3) . ? 
Cr1 N1 2.071(3) 7_656 ? 
Cr1 C6 2.078(4) . ? 
Cr1 C6 2.079(4) 7_656 ? 
Cr1 N2 2.080(3) . ? 
Cr1 N2 2.080(3) 7_656 ? 
S1 C11 1.736(4) . ? 
S1 C9 1.756(4) . ? 
S2 C10 1.732(4) . ? 
S2 C11 1.731(4) . ? 
S3 C12 1.736(4) . ? 
S3 C13 1.753(4) . ? 
S4 C12 1.738(4) . ? 
S4 C14 1.749(4) . ? 
S5 C13 1.747(4) . ? 
S5 C15 1.796(6) . ? 
S6 C14 1.743(4) . ? 
S6 C16 1.784(5) . ? 
N1 C4 1.487(5) . ? 
N1 C3 1.492(5) . ? 
N2 C1 1.482(6) 7_656 ? 
N2 C5 1.486(6) . ? 
C1 N2 1.483(6) 7_656 ? 
C1 C2 1.531(7) . ? 
C2 C3 1.529(7) . ? 
C4 C5 1.502(7) . ? 
C6 C7 1.196(5) . ? 
C7 C9 1.427(5) . ? 
C8 C10 1.496(5) . ? 
C9 C10 1.354(5) . ? 
C11 C12 1.366(6) . ? 
C13 C14 1.332(7) . ? 
C15 C16 1.526(8) . ? 
B1 F3 1.358(7) . ? 
B1 F4 1.357(7) . ? 
B1 F1 1.377(7) . ? 
B1 F2 1.381(7) . ? 
C93 C94 1.3900 . ? 
C93 C98 1.3900 . ? 
C93 Cl1 1.702(9) . ? 
C94 C95 1.3900 . ? 
C95 C96 1.3900 . ? 
C96 C97 1.3900 . ? 
C97 C98 1.3900 . ? 
C90 C91 1.434(16) . ? 
C91 N92 1.203(15) . ? 
C91 C91 1.88(4) 2_756 ? 
N92 C91 1.202(15) 2_756 ? 
 
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
N1 Cr1 N1 179.997(2) . 7_656 ? 
N1 Cr1 C6 90.52(14) . . ? 
N1 Cr1 C6 89.48(14) 7_656 . ? 
N1 Cr1 C6 89.48(14) . 7_656 ? 
N1 Cr1 C6 90.52(14) 7_656 7_656 ? 
C6 Cr1 C6 180.0 . 7_656 ? 
N1 Cr1 N2 85.33(13) . . ? 
N1 Cr1 N2 94.67(13) 7_656 . ? 
C6 Cr1 N2 88.74(14) . . ? 
C6 Cr1 N2 91.26(14) 7_656 . ? 
N1 Cr1 N2 94.67(13) . 7_656 ? 
N1 Cr1 N2 85.33(13) 7_656 7_656 ? 
C6 Cr1 N2 91.26(14) . 7_656 ? 
C6 Cr1 N2 88.74(14) 7_656 7_656 ? 
N2 Cr1 N2 179.997(1) . 7_656 ? 
C11 S1 C9 95.10(18) . . ? 
C10 S2 C11 96.19(19) . . ? 
C12 S3 C13 95.1(2) . . ? 
C12 S4 C14 95.4(2) . . ? 
C13 S5 C15 99.1(2) . . ? 
C14 S6 C16 102.2(2) . . ? 
C4 N1 C3 113.8(3) . . ? 
C4 N1 Cr1 106.3(3) . . ? 
C3 N1 Cr1 115.7(3) . . ? 
C1 N2 C5 113.5(3) 7_656 . ? 
C1 N2 Cr1 115.7(3) 7_656 . ? 
C5 N2 Cr1 105.2(2) . . ? 
N2 C1 C2 112.6(4) 7_656 . ? 
C1 C2 C3 115.4(4) . . ? 
N1 C3 C2 111.6(4) . . ? 
N1 C4 C5 108.9(3) . . ? 
N2 C5 C4 109.5(3) . . ? 
C7 C6 Cr1 174.4(3) . . ? 
C6 C7 C9 177.7(4) . . ? 
C10 C9 C7 124.6(3) . . ? 
C10 C9 S1 116.9(3) . . ? 
C7 C9 S1 118.5(3) . . ? 
C9 C10 C8 125.8(4) . . ? 
C9 C10 S2 116.6(3) . . ? 
C8 C10 S2 117.5(3) . . ? 
C12 C11 S2 122.3(3) . . ? 
C12 C11 S1 122.7(3) . . ? 
S2 C11 S1 115.1(2) . . ? 
C11 C12 S3 122.8(3) . . ? 
C11 C12 S4 122.0(3) . . ? 
S3 C12 S4 115.1(2) . . ? 
C14 C13 S5 127.8(3) . . ? 
C14 C13 S3 117.5(3) . . ? 
S5 C13 S3 114.7(3) . . ? 
C13 C14 S6 129.8(3) . . ? 
C13 C14 S4 116.9(3) . . ? 
S6 C14 S4 113.3(3) . . ? 
C16 C15 S5 114.0(4) . . ? 
C15 C16 S6 113.4(3) . . ? 
F3 B1 F4 113.6(6) . . ? 
F3 B1 F1 111.2(5) . . ? 
F4 B1 F1 111.2(5) . . ? 
F3 B1 F2 106.1(5) . . ? 
F4 B1 F2 107.2(5) . . ? 
F1 B1 F2 107.2(5) . . ? 
C94 C93 C98 120.0 . . ? 
C94 C93 Cl1 119.6(6) . . ? 
C98 C93 Cl1 120.3(6) . . ? 
C95 C94 C93 120.0 . . ? 
C94 C95 C96 120.0 . . ? 
C97 C96 C95 120.0 . . ? 
C96 C97 C98 120.0 . . ? 
C97 C98 C93 120.0 . . ? 
N92 C91 C90 145(2) . . ? 
N92 C91 C91 38.5(14) . 2_756 ? 
C90 C91 C91 170(3) . 2_756 ? 
C91 N92 C91 103(3) 2_756 . ? 
 
_diffrn_measured_fraction_theta_max    30.5214
_diffrn_reflns_theta_full              30.5214
_diffrn_measured_fraction_theta_full   83.3000
_refine_diff_density_max    2.037 
_refine_diff_density_min   -0.730 
_refine_diff_density_rms    0.140 
