#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:10:53 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179470 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/67/4336773.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_4336773
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+, 2(Re O4 1-), 2(C6 H5 Cl), C2 H3 N'
_chemical_formula_sum            'C46 H51 Cl2 Cr N5 O8 Re2 S12'
_chemical_formula_weight         1681.94
_chemical_name_common            '[CrCyclam(C2MeEDT-TTF)2][ReO4]2(PhCl)2(MeCN)'
_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                 103.4155(62)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   32.9055(71)
_cell_length_b                   12.1918(22)
_cell_length_c                   16.3414(35)
_cell_measurement_reflns_used    11078
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.5069
_cell_measurement_theta_min      2.1103
_cell_volume                     6377(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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
scan:
    Number of images: 360
               Slice: -80.0000 - 100.0000
         Image width: 0.5000
            Exp time: 12.0000
       Rotation axis: Phi
               Omega: 0.0000
                 Chi: 0.0000
                 Phi: 0.0000
                 XTD: 34.8737
              2theta: 9.9361
scan:
    Number of images: 98
               Slice: -29.5000 - 19.5000
         Image width: 0.5000
            Exp time: 12.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 0.0000
                 XTD: 34.8737
              2theta: 9.9361
scan:
    Number of images: 98
               Slice: -29.5000 - 19.5000
         Image width: 0.5000
            Exp time: 12.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 90.0000
                 XTD: 34.8737
              2theta: 9.9361
scan:
    Number of images: 98
               Slice: -29.5000 - 19.5000
         Image width: 0.5000
            Exp time: 12.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 180.0000
                 XTD: 34.8737
              2theta: 9.9361

;
_diffrn_measurement_device_type  'Rigaku AFC7R with CCD detector'
_diffrn_measurement_method       dtprofit.ref
_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  0.0619
_diffrn_reflns_av_sigmaI/netI    0.0504
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            31028
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         29.0
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    4.481
_exptl_absorpt_correction_T_max  0.7029
_exptl_absorpt_correction_T_min  0.4928
_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    1.752
_exptl_crystal_description       Block
_exptl_crystal_F_000             3304
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         3.237
_refine_diff_density_min         -1.486
_refine_diff_density_rms         0.201
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         8355
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1071
_refine_ls_R_factor_gt           0.0837
_refine_ls_shift/su_max          0.042
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1629P)²+0.4599P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2228
_refine_ls_wR_factor_ref         0.2589
_reflns_number_gt                4806
_reflns_number_total             8355
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402217c_si_001_5.cif
_cod_data_source_block           '[CrCyclam(C2MeEDT-TTF)2][ReO4]2(PhCl)2(MeCN)'
_cod_original_cell_volume        6376.9(2)
_cod_database_code               4336773
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
Cr1 Cr 0.7500 0.2500 0.5000 0.0551(4) Uani 1 2 d S
S1 S 0.92248(7) 0.3347(2) 0.50092(16) 0.0746(6) Uani 1 1 d .
S2 S 0.92489(6) 0.4369(2) 0.34038(14) 0.0741(6) Uani 1 1 d .
S3 S 1.02352(7) 0.3183(2) 0.54702(17) 0.0831(8) Uani 1 1 d .
S4 S 1.02510(7) 0.4202(3) 0.38541(15) 0.0878(8) Uani 1 1 d .
S5 S 1.11407(8) 0.2812(3) 0.59736(18) 0.0914(8) Uani 1 1 d .
S6 S 1.11485(8) 0.4033(3) 0.40302(19) 0.1007(9) Uani 1 1 d .
N1 N 0.7767(2) 0.0994(6) 0.5365(5) 0.0665(16) Uani 1 1 d .
H1 H 0.7581 0.0621 0.5593 0.080 Uiso 1 1 calc R
N2 N 0.7354(2) 0.1832(5) 0.3814(5) 0.0611(16) Uani 1 1 d .
H2 H 0.7553 0.2066 0.3550 0.073 Uiso 1 1 calc R
C1 C 0.8054(3) 0.2862(9) 0.6735(6) 0.079(2) Uani 1 1 d .
H1A H 0.8074 0.3163 0.7293 0.095 Uiso 1 1 calc R
H1B H 0.8276 0.3183 0.6513 0.095 Uiso 1 1 calc R
C2 C 0.8116(4) 0.1609(10) 0.6803(7) 0.090(3) Uani 1 1 d .
H2A H 0.8360 0.1459 0.7252 0.108 Uiso 1 1 calc R
H2B H 0.7877 0.1292 0.6967 0.108 Uiso 1 1 calc R
C3 C 0.8170(3) 0.1040(9) 0.6036(7) 0.082(3) Uani 1 1 d .
H3A H 0.8268 0.0299 0.6181 0.098 Uiso 1 1 calc R
H3B H 0.8381 0.1419 0.5815 0.098 Uiso 1 1 calc R
C4 C 0.7789(3) 0.0401(8) 0.4583(7) 0.077(2) Uani 1 1 d .
H4A H 0.8034 0.0637 0.4395 0.092 Uiso 1 1 calc R
H4B H 0.7814 -0.0381 0.4693 0.092 Uiso 1 1 calc R
C5 C 0.7409(3) 0.0625(7) 0.3921(6) 0.077(2) Uani 1 1 d .
H5A H 0.7167 0.0309 0.4078 0.093 Uiso 1 1 calc R
H5B H 0.7434 0.0294 0.3395 0.093 Uiso 1 1 calc R
C6 C 0.8066(2) 0.3088(6) 0.4783(6) 0.0601(19) Uani 1 1 d .
C7 C 0.8376(2) 0.3358(7) 0.4566(6) 0.0602(18) Uani 1 1 d .
C8 C 0.8395(3) 0.4414(9) 0.2894(7) 0.083(3) Uani 1 1 d .
H8A H 0.8346 0.3866 0.2460 0.125 Uiso 1 1 calc R
H8B H 0.8452 0.5104 0.2662 0.125 Uiso 1 1 calc R
H8C H 0.8151 0.4482 0.3120 0.125 Uiso 1 1 calc R
C9 C 0.8742(2) 0.3615(8) 0.4317(5) 0.0645(19) Uani 1 1 d .
C10 C 0.8759(2) 0.4085(6) 0.3576(5) 0.0597(17) Uani 1 1 d .
C11 C 0.9529(2) 0.3818(10) 0.4350(6) 0.079(3) Uani 1 1 d .
C12 C 0.9946(2) 0.3772(9) 0.4538(6) 0.073(2) Uani 1 1 d .
C13 C 1.0716(3) 0.3332(9) 0.5195(6) 0.074(2) Uani 1 1 d .
C14 C 1.0727(2) 0.3747(9) 0.4471(6) 0.071(2) Uani 1 1 d .
C15 C 1.1507(3) 0.2667(10) 0.5324(8) 0.090(3) Uani 1 1 d .
H15A H 1.1772 0.2419 0.5670 0.107 Uiso 1 1 calc R
H15B H 1.1407 0.2105 0.4905 0.107 Uiso 1 1 calc R
C16 C 1.1578(3) 0.3691(10) 0.4889(7) 0.084(3) Uani 1 1 d .
H16A H 1.1828 0.3610 0.4678 0.101 Uiso 1 1 calc R
H16B H 1.1624 0.4289 0.5292 0.101 Uiso 1 1 calc R
Re1 Re 0.772919(14) -0.18550(3) 0.66144(3) 0.0808(2) Uani 1 1 d .
O1 O 0.7409(2) -0.0774(6) 0.6242(7) 0.107(3) Uani 1 1 d .
O2 O 0.7920(4) -0.1730(10) 0.7650(6) 0.141(4) Uani 1 1 d .
O3 O 0.8158(4) -0.1794(10) 0.6216(8) 0.151(5) Uani 1 1 d .
O4 O 0.7476(5) -0.3028(11) 0.6421(15) 0.211(9) Uani 1 1 d .
C93 C 0.9214(8) 0.0513(17) 0.4181(16) 0.198(10) Uani 1 1 d G
C94 C 0.9615(6) 0.0824(19) 0.4132(15) 0.209(11) Uani 1 1 d G
H94 H 0.9838 0.0719 0.4591 0.250 Uiso 1 1 calc R
C95 C 0.9680(8) 0.1290(19) 0.340(2) 0.34(2) Uani 1 1 d G
H95 H 0.9948 0.1498 0.3365 0.404 Uiso 1 1 calc R
C96 C 0.9346(12) 0.145(2) 0.2711(15) 0.33(3) Uani 1 1 d G
H96 H 0.9389 0.1758 0.2220 0.394 Uiso 1 1 calc R
C97 C 0.8945(9) 0.114(2) 0.2760(17) 0.30(2) Uani 1 1 d G
H97 H 0.8722 0.1240 0.2301 0.362 Uiso 1 1 calc R
C98 C 0.8880(6) 0.067(2) 0.350(2) 0.271(17) Uani 1 1 d G
H98 H 0.8612 0.0461 0.3528 0.325 Uiso 1 1 calc R
Cl1 Cl 0.9142(5) -0.0006(12) 0.5092(13) 0.394(10) Uani 1 1 d .
C90 C 0.9247(6) 0.278(2) 0.7160(18) 0.110(7) Uiso 0.50 1 d PD
H90A H 0.9163 0.3006 0.7658 0.166 Uiso 0.50 1 calc PR
H90B H 0.9159 0.2038 0.7025 0.166 Uiso 0.50 1 calc PR
H90C H 0.9122 0.3252 0.6701 0.166 Uiso 0.50 1 calc PR
C91 C 0.9693(8) 0.284(3) 0.730(3) 0.161(14) Uiso 0.50 1 d PD
N92 N 1.0000 0.332(2) 0.7500 0.188(11) Uiso 1 2 d SD
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'
Re Re -1.0185 7.2310 '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
N2 Cr1 N2 179.998(2) . 7_656
N2 Cr1 N1 95.1(3) . 7_656
N2 Cr1 N1 84.9(3) 7_656 7_656
N2 Cr1 N1 84.9(3) . .
N2 Cr1 N1 95.1(3) 7_656 .
N1 Cr1 N1 179.999(1) 7_656 .
N2 Cr1 C6 89.9(3) . .
N2 Cr1 C6 90.1(3) 7_656 .
N1 Cr1 C6 89.0(3) 7_656 .
N1 Cr1 C6 91.0(3) . .
N2 Cr1 C6 90.1(3) . 7_656
N2 Cr1 C6 89.9(3) 7_656 7_656
N1 Cr1 C6 91.0(3) 7_656 7_656
N1 Cr1 C6 89.0(3) . 7_656
C6 Cr1 C6 180.0(4) . 7_656
C11 S1 C9 96.0(4) . .
C10 S2 C11 95.7(4) . .
C13 S3 C12 94.4(4) . .
C12 S4 C14 96.2(4) . .
C13 S5 C15 97.9(5) . .
C14 S6 C16 100.9(5) . .
C4 N1 C3 115.7(7) . .
C4 N1 Cr1 106.7(5) . .
C3 N1 Cr1 114.8(6) . .
C1 N2 C5 112.9(7) 7_656 .
C1 N2 Cr1 116.9(6) 7_656 .
C5 N2 Cr1 106.6(5) . .
N2 C1 C2 112.3(7) 7_656 .
C3 C2 C1 116.3(9) . .
C2 C3 N1 112.1(8) . .
C5 C4 N1 109.8(7) . .
C4 C5 N2 109.1(7) . .
C7 C6 Cr1 172.0(8) . .
C6 C7 C9 177.1(9) . .
C10 C9 C7 125.1(7) . .
C10 C9 S1 115.9(6) . .
C7 C9 S1 119.0(7) . .
C9 C10 C8 126.2(7) . .
C9 C10 S2 117.5(6) . .
C8 C10 S2 116.2(6) . .
C12 C11 S1 123.6(7) . .
C12 C11 S2 121.7(7) . .
S1 C11 S2 114.7(4) . .
C11 C12 S4 123.5(7) . .
C11 C12 S3 122.7(7) . .
S4 C12 S3 113.6(4) . .
C14 C13 S3 119.5(7) . .
C14 C13 S5 127.6(8) . .
S3 C13 S5 112.8(6) . .
C13 C14 S6 130.5(7) . .
C13 C14 S4 116.2(7) . .
S6 C14 S4 113.1(5) . .
C16 C15 S5 113.7(8) . .
C15 C16 S6 112.9(8) . .
O4 Re1 O2 109.1(9) . .
O4 Re1 O3 113.3(9) . .
O2 Re1 O3 103.6(7) . .
O4 Re1 O1 111.0(6) . .
O2 Re1 O1 110.3(5) . .
O3 Re1 O1 109.3(5) . .
C94 C93 C98 120.0 . .
C94 C93 Cl1 119(2) . .
C98 C93 Cl1 121(2) . .
C93 C94 C95 120.0 . .
C96 C95 C94 120.0 . .
C95 C96 C97 120.0 . .
C98 C97 C96 120.0 . .
C97 C98 C93 120.0 . .
N92 C91 C90 151(4) . .
N92 C91 C91 30(3) . 2_756
C90 C91 C91 170(5) . 2_756
C91 N92 C91 119(5) 2_756 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cr1 N2 2.054(7) .
Cr1 N2 2.054(7) 7_656
Cr1 N1 2.063(7) 7_656
Cr1 N1 2.063(7) .
Cr1 C6 2.102(8) .
Cr1 C6 2.102(8) 7_656
S1 C11 1.731(9) .
S1 C9 1.755(8) .
S2 C10 1.736(7) .
S2 C11 1.740(9) .
S3 C13 1.751(10) .
S3 C12 1.753(9) .
S4 C12 1.747(9) .
S4 C14 1.744(9) .
S5 C13 1.774(9) .
S5 C15 1.791(11) .
S6 C14 1.741(9) .
S6 C16 1.794(11) .
N1 C4 1.485(12) .
N1 C3 1.512(11) .
N2 C1 1.481(12) 7_656
N2 C5 1.488(11) .
C1 N2 1.481(12) 7_656
C1 C2 1.543(15) .
C2 C3 1.478(17) .
C4 C5 1.477(14) .
C6 C7 1.201(11) .
C7 C9 1.391(11) .
C8 C10 1.489(12) .
C9 C10 1.353(12) .
C11 C12 1.334(11) .
C13 C14 1.295(14) .
C15 C16 1.481(17) .
Re1 O4 1.648(14) .
Re1 O2 1.670(11) .
Re1 O3 1.689(12) .
Re1 O1 1.709(7) .
C93 C94 1.393(13) .
C93 C98 1.384(12) .
C93 Cl1 1.684(30) .
C94 C95 1.385(13) .
C95 C96 1.393(14) .
C96 C97 1.393(13) .
C97 C98 1.399(12) .
C90 C91 1.434(18) .
C91 N92 1.141(17) .
C91 C91 1.97(5) 2_756
N92 C91 1.141(17) 2_756
