#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:10:53 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179470 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/67/4336772.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4336772
loop_
_publ_author_name
'Junichi Nishijo'
'Masaya Enomoto'
_publ_section_title
;
 A Series of Weak Ferromagnets Based on a Chromium-Acetylide-TTF Type
 Complex: Correlation of the Structures and Magnetic Properties and Origin
 of the Weak Ferromagnetism
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              13263
_journal_page_last               13268
_journal_paper_doi               10.1021/ic402217c
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety
'C32 H38 Cr N4 S12 2+, (Cl O4 1-)2, (C6 H5 I)3'
_chemical_formula_sum            'C50 H53 Cl2 Cr I3 N4 O8 S12'
_chemical_formula_weight         1726.28
_chemical_name_common            '[CrCyclam(C2MeEDT-TTF)2][ClO4]2(PhI)3'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.1024(41)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   32.9459(67)
_cell_length_b                   12.0437(22)
_cell_length_c                   16.3178(33)
_cell_measurement_reflns_used    11351
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.3391
_cell_measurement_theta_min      2.0198
_cell_volume                     6280(2)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR2004 (M. C. Burla et al.)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 14.7059
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
scan:
    Number of images: 360
               Slice: -80.0000 - 100.0000
         Image width: 0.5000
            Exp time: 6.0000
       Rotation axis: Phi
               Omega: 0.0000
                 Chi: 0.0000
                 Phi: 0.0000
                 XTD: 35.1020
              2theta: 10.2714
scan:
    Number of images: 98
               Slice: -29.5000 - 19.5000
         Image width: 0.5000
            Exp time: 6.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 0.0000
                 XTD: 35.1020
              2theta: 10.2714
scan:
    Number of images: 98
               Slice: -29.5000 - 19.5000
         Image width: 0.5000
            Exp time: 6.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 90.0000
                 XTD: 35.1020
              2theta: 10.2714
scan:
    Number of images: 98
               Slice: -29.5000 - 19.5000
         Image width: 0.5000
            Exp time: 6.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 180.0000
                 XTD: 35.1020
              2theta: 10.2714

;
_diffrn_measurement_device_details
;
AFC7: Eulerian 3 circle
;
_diffrn_measurement_device_type  'Rigaku AFC7R with CCD detector'
_diffrn_measurement_method       dtprofit.ref
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.0208
_diffrn_orient_matrix_UB_12      -0.0216
_diffrn_orient_matrix_UB_13      -0.0092
_diffrn_orient_matrix_UB_21      0.0237
_diffrn_orient_matrix_UB_22      -0.0494
_diffrn_orient_matrix_UB_23      0.0624
_diffrn_orient_matrix_UB_31      -0.0526
_diffrn_orient_matrix_UB_32      0.0148
_diffrn_orient_matrix_UB_33      0.0317
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0617
_diffrn_reflns_av_sigmaI/netI    0.0404
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            29800
_diffrn_reflns_theta_full        28.7
_diffrn_reflns_theta_max         28.7
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    2.195
_exptl_absorpt_correction_T_max  0.8274
_exptl_absorpt_correction_T_min  0.5878
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 CrystalClear-SM 1.3.6 SP3 r6 (Rigaku/MSC Inc., 2006) 
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.826
_exptl_crystal_description       block
_exptl_crystal_F_000             3416
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.832
_refine_diff_density_min         -3.436
_refine_diff_density_rms         0.244
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.207
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         8108
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.207
_refine_ls_R_factor_all          0.1030
_refine_ls_R_factor_gt           0.0972
_refine_ls_shift/su_max          0.032
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2697
_refine_ls_wR_factor_ref         0.2785
_reflns_number_gt                7130
_reflns_number_total             8108
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402217c_si_001_4.cif
_cod_data_source_block           '[CrCyclam(C2MeEDT-TTF)2][ClO4]2(PhI)3'
_cod_original_cell_volume        6279.6(1)
_cod_database_code               4336772
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'
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 0.2500 0.2500 0.5000 0.0339(3) Uani 1 2 d S . .
S1 S 0.42545(4) 0.16665(13) 0.50708(8) 0.0452(4) Uani 1 1 d . . .
S2 S 0.42486(4) 0.06446(14) 0.34449(8) 0.0471(4) Uani 1 1 d . . .
S3 S 0.52749(4) 0.18547(15) 0.54633(9) 0.0511(4) Uani 1 1 d . . .
S4 S 0.52440(4) 0.08234(17) 0.38230(9) 0.0557(4) Uani 1 1 d . . .
S5 S 0.61941(5) 0.21808(18) 0.59055(11) 0.0602(4) Uani 1 1 d . . .
S6 S 0.61411(5) 0.0921(2) 0.39395(11) 0.0667(5) Uani 1 1 d . . .
N1 N 0.27446(14) 0.4053(4) 0.5397(3) 0.0421(9) Uani 1 1 d . . .
H1 H 0.2546 0.4422 0.5593 0.050 Uiso 1 1 calc R . .
N2 N 0.26352(14) 0.1829(4) 0.6208(3) 0.0409(9) Uani 1 1 d . . .
H2 H 0.2427 0.2052 0.6449 0.049 Uiso 1 1 calc R . .
C1 C 0.31310(19) 0.4056(5) 0.6085(4) 0.0511(12) Uani 1 1 d . . .
H1A H 0.3214 0.4817 0.6233 0.061 Uiso 1 1 calc R . .
H1B H 0.3354 0.3701 0.5889 0.061 Uiso 1 1 calc R . .
C2 C 0.3069(2) 0.3449(6) 0.6867(4) 0.0571(14) Uani 1 1 d . . .
H2A H 0.3304 0.3622 0.7338 0.069 Uiso 1 1 calc R . .
H2B H 0.2818 0.3733 0.7003 0.069 Uiso 1 1 calc R . .
C3 C 0.3032(2) 0.2188(6) 0.6780(4) 0.0518(13) Uani 1 1 d . . .
H3A H 0.3263 0.1908 0.6568 0.062 Uiso 1 1 calc R . .
H3B H 0.3054 0.1865 0.7333 0.062 Uiso 1 1 calc R . .
C4 C 0.2594(2) 0.0605(5) 0.6102(4) 0.0504(12) Uani 1 1 d . . .
H4A H 0.2561 0.0266 0.6621 0.060 Uiso 1 1 calc R . .
H4B H 0.2843 0.0301 0.5969 0.060 Uiso 1 1 calc R . .
C5 C 0.2217(2) 0.0363(5) 0.5395(4) 0.0525(13) Uani 1 1 d . . .
H5A H 0.1966 0.0612 0.5551 0.063 Uiso 1 1 calc R . .
H5B H 0.2193 -0.0431 0.5295 0.063 Uiso 1 1 calc R . .
C6 C 0.30721(15) 0.1990(4) 0.4824(3) 0.0408(10) Uani 1 1 d . . .
C7 C 0.33995(16) 0.1720(4) 0.4634(3) 0.0415(10) Uani 1 1 d . . .
C8 C 0.33832(19) 0.0652(6) 0.2957(4) 0.0554(14) Uani 1 1 d . . .
H8A H 0.3251 0.0011 0.3126 0.083 Uiso 1 1 calc R . .
H8B H 0.3463 0.0495 0.2441 0.083 Uiso 1 1 calc R . .
H8C H 0.3191 0.1266 0.2870 0.083 Uiso 1 1 calc R . .
C9 C 0.37633(14) 0.1408(4) 0.4386(3) 0.0390(9) Uani 1 1 d . . .
C10 C 0.37615(14) 0.0940(5) 0.3628(3) 0.0406(10) Uani 1 1 d . . .
C11 C 0.45454(15) 0.1198(5) 0.4386(3) 0.0433(11) Uani 1 1 d . . .
C12 C 0.49713(16) 0.1275(5) 0.4552(3) 0.0465(11) Uani 1 1 d . . .
C13 C 0.57491(17) 0.1689(5) 0.5173(4) 0.0458(11) Uani 1 1 d . . .
C14 C 0.57377(17) 0.1216(6) 0.4422(3) 0.0474(12) Uani 1 1 d . . .
C15 C 0.6548(2) 0.2318(6) 0.5220(5) 0.0599(16) Uani 1 1 d . . .
H15A H 0.6445 0.2895 0.4806 0.072 Uiso 1 1 calc R . .
H15B H 0.6821 0.2548 0.5554 0.072 Uiso 1 1 calc R . .
C16 C 0.65950(19) 0.1262(6) 0.4769(5) 0.0556(14) Uani 1 1 d . . .
H16A H 0.6649 0.0659 0.5175 0.067 Uiso 1 1 calc R . .
H16B H 0.6836 0.1326 0.4527 0.067 Uiso 1 1 calc R . .
Cl1 Cl 0.26905(5) 0.31693(13) 0.16567(10) 0.0541(4) Uani 1 1 d . . .
O1 O 0.2890(3) 0.3431(9) 0.2515(4) 0.096(2) Uani 1 1 d . . .
O2 O 0.2471(3) 0.2144(6) 0.1652(7) 0.096(2) Uani 1 1 d . . .
O3 O 0.3004(3) 0.3117(7) 0.1198(5) 0.092(2) Uani 1 1 d . . .
O4 O 0.2399(2) 0.4020(6) 0.1341(6) 0.093(2) Uani 1 1 d . . .
I1 I 0.41512(3) 0.49694(7) 0.52806(6) 0.0949(4) Uani 1 1 d . . .
C93 C 0.3874(3) 0.4151(10) 0.3452(8) 0.088(3) Uani 1 1 d . . .
H93 H 0.3604 0.4314 0.3497 0.106 Uiso 1 1 calc R . .
C94 C 0.3941(4) 0.3734(12) 0.2756(10) 0.101(4) Uani 1 1 d . . .
H94 H 0.3709 0.3627 0.2306 0.122 Uiso 1 1 calc R . .
C95 C 0.4321(5) 0.3446(13) 0.2637(9) 0.105(4) Uani 1 1 d . . .
H95 H 0.4347 0.3129 0.2133 0.126 Uiso 1 1 calc R . .
C96 C 0.4678(5) 0.3644(13) 0.3310(10) 0.105(4) Uani 1 1 d . . .
H96 H 0.4944 0.3460 0.3253 0.126 Uiso 1 1 calc R . .
C97 C 0.4627(3) 0.4102(13) 0.4032(9) 0.098(3) Uani 1 1 d . . .
H97 H 0.4859 0.4259 0.4469 0.118 Uiso 1 1 calc R . .
C98 C 0.4222(3) 0.4346(9) 0.4129(7) 0.081(2) Uani 1 1 d . . .
I2 I 0.57693(5) 0.2741(3) 0.77097(14) 0.1050(9) Uani 0.50 1 d PD A -1
C100 C 0.5125(3) 0.2710(10) 0.7584(6) 0.061(3) Uani 0.50 1 d PD A -1
C102 C 0.4938(5) 0.1697(10) 0.7346(5) 0.062(5) Uani 0.50 1 d PD A -1
H102 H 0.5096 0.1085 0.7265 0.074 Uiso 0.50 1 calc PR A -1
C103 C 0.4508(5) 0.1617(16) 0.7231(9) 0.078(5) Uani 0.50 1 d PD A -1
H103 H 0.4382 0.0924 0.7124 0.094 Uiso 0.50 1 calc PR A -1
C104 C 0.4916(5) 0.3621(11) 0.7759(10) 0.071(4) Uani 0.50 1 d PD A -1
H104 H 0.5053 0.4286 0.7936 0.086 Uiso 0.50 1 calc PR A -1
C105 C 0.4264(6) 0.252(2) 0.7270(8) 0.17(2) Uani 0.50 1 d PD A -1
H105 H 0.3975 0.2498 0.7058 0.160 Uiso 0.50 1 calc PR A -1
C101 C 0.4476(5) 0.3500(15) 0.7656(11) 0.097(8) Uani 0.50 1 d PD A -1
H101 H 0.4324 0.4060 0.7840 0.117 Uiso 0.50 1 calc PR A -1
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'
N N 0.0061 0.0033 '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'
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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
C6 Cr1 C6 180.000(1) . 7_556
C6 Cr1 N2 91.42(19) . .
C6 Cr1 N2 88.58(19) 7_556 .
C6 Cr1 N2 88.58(19) . 7_556
C6 Cr1 N2 91.42(19) 7_556 7_556
N2 Cr1 N2 180.0 . 7_556
C6 Cr1 N1 90.8(2) . .
C6 Cr1 N1 89.2(2) 7_556 .
N2 Cr1 N1 94.42(19) . .
N2 Cr1 N1 85.58(19) 7_556 .
C6 Cr1 N1 89.3(2) . 7_556
C6 Cr1 N1 90.8(2) 7_556 7_556
N2 Cr1 N1 85.58(19) . 7_556
N2 Cr1 N1 94.42(19) 7_556 7_556
N1 Cr1 N1 179.997(1) . 7_556
C11 S1 C9 95.8(2) . .
C10 S2 C11 96.5(2) . .
C12 S3 C13 95.1(3) . .
C12 S4 C14 95.7(3) . .
C13 S5 C15 99.6(3) . .
C14 S6 C16 101.5(3) . .
C1 N1 C5 114.4(5) . 7_556
C1 N1 Cr1 115.9(4) . .
C5 N1 Cr1 105.1(4) 7_556 .
C3 N2 C4 114.0(4) . .
C3 N2 Cr1 116.0(4) . .
C4 N2 Cr1 106.4(3) . .
N1 C1 C2 111.6(5) . .
C3 C2 C1 115.0(5) . .
N2 C3 C2 112.9(5) . .
N2 C4 C5 108.5(5) . .
C4 C5 N1 109.9(5) . 7_556
C7 C6 Cr1 173.5(5) . .
C6 C7 C9 177.8(6) . .
C10 C9 C7 123.9(4) . .
C10 C9 S1 116.9(4) . .
C7 C9 S1 119.2(4) . .
C9 C10 C8 125.8(5) . .
C9 C10 S2 116.2(4) . .
C8 C10 S2 118.0(4) . .
C12 C11 S1 123.5(4) . .
C12 C11 S2 122.0(4) . .
S1 C11 S2 114.4(3) . .
C11 C12 S3 123.4(4) . .
C11 C12 S4 121.2(4) . .
S3 C12 S4 115.3(3) . .
C14 C13 S3 117.8(4) . .
C14 C13 S5 126.7(4) . .
S3 C13 S5 115.5(3) . .
C13 C14 S6 130.1(4) . .
C13 C14 S4 116.1(4) . .
S6 C14 S4 113.7(3) . .
C16 C15 S5 112.7(5) . .
C15 C16 S6 113.4(5) . .
O4 Cl1 O3 111.0(5) . .
O4 Cl1 O1 107.9(6) . .
O3 Cl1 O1 107.8(5) . .
O4 Cl1 O2 109.0(5) . .
O3 Cl1 O2 113.1(6) . .
O1 Cl1 O2 107.9(6) . .
C94 C93 C98 117.9(11) . .
C93 C94 C95 125.3(12) . .
C94 C95 C96 117.8(14) . .
C97 C96 C95 119.2(13) . .
C96 C97 C98 120.4(12) . .
C93 C98 C97 119.3(12) . .
C93 C98 I1 121.2(8) . .
C97 C98 I1 119.4(8) . .
C104 C100 C102 124.0(12) . .
C104 C100 I2 121.3(10) . .
C102 C100 I2 114.6(10) . .
C100 C102 C103 118.0(13) . .
C105 C103 C102 122.3(14) . .
C100 C104 C101 116.4(12) . .
C103 C105 C101 116.5(15) . .
C104 C101 C105 120.4(14) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cr1 C6 2.068(5) .
Cr1 C6 2.068(5) 7_556
Cr1 N2 2.076(4) .
Cr1 N2 2.076(4) 7_556
Cr1 N1 2.076(5) .
Cr1 N1 2.076(5) 7_556
S1 C11 1.734(5) .
S1 C9 1.756(5) .
S2 C10 1.739(5) .
S2 C11 1.740(5) .
S3 C12 1.725(5) .
S3 C13 1.751(6) .
S4 C12 1.743(6) .
S4 C14 1.746(6) .
S5 C13 1.754(6) .
S5 C15 1.810(8) .
S6 C14 1.738(6) .
S6 C16 1.803(7) .
N1 C1 1.478(8) .
N1 C5 1.504(8) 7_556
N2 C3 1.473(8) .
N2 C4 1.487(8) .
C1 C2 1.526(10) .
C2 C3 1.528(10) .
C4 C5 1.503(9) .
C5 N1 1.504(8) 7_556
C6 C7 1.236(7) .
C7 C9 1.406(7) .
C8 C10 1.486(7) .
C9 C10 1.358(7) .
C11 C12 1.366(7) .
C13 C14 1.345(8) .
C15 C16 1.497(11) .
Cl1 O4 1.413(7) .
Cl1 O3 1.416(7) .
Cl1 O1 1.430(7) .
Cl1 O2 1.431(7) .
I1 C98 2.089(13) .
C93 C94 1.31(2) .
C93 C98 1.406(15) .
C94 C95 1.36(2) .
C95 C96 1.42(2) .
C96 C97 1.35(2) .
C97 C98 1.410(15) .
I2 C100 2.084(11) .
C100 C104 1.362(15) .
C100 C102 1.378(14) .
C102 C103 1.387(16) .
C103 C105 1.361(18) .
C104 C101 1.426(17) .
C105 C101 1.439(18) .
