#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/84/4318419.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_4318419
loop_
_publ_author_name
'Ho-Chol Chang'
'Katsunori Mochizuki'
'Susumu Kitagawa'
_publ_section_title
;
 Synthesis and Ligand-Based Mixed Valency of cis- and
 trans-CrIII(X4SQ)(X4Cat)(L)n (X = Cl and Br,n= 1 or 2) Complexes: Effects
 of Solvent Media on Intramolecular Charge Distribution and Ligand
 Dissociation of CrIII(X4SQ)3
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4444
_journal_page_last               4452
_journal_paper_doi               10.1021/ic025643p
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         'C28 H16 Cl8 Cr N2 O4 '
_chemical_formula_sum            'C28 H16 Cl8 Cr N2 O4'
_chemical_formula_weight         780.07
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_cell_angle_alpha                90
_cell_angle_beta                 102.944(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.128(7)
_cell_length_b                   26.148(5)
_cell_length_c                   8.5648(9)
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      22.5
_cell_volume                     3520.1(17)
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    SIR92
_diffrn_measured_fraction_theta_full 0.3549
_diffrn_measured_fraction_theta_max 0.3549
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.038
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            4755
_diffrn_reflns_theta_full        27.33
_diffrn_reflns_theta_max         27.33
_exptl_absorpt_coefficient_mu    0.966
_exptl_absorpt_correction_type   REQABA
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.36
_refine_diff_density_min         -0.35
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.405
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     195
_refine_ls_number_reflns         1344
_refine_ls_R_factor_gt           0.0742
_refine_ls_shift/su_max          0.0015
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[σ²(Fo) + 0.00181|Fo|²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0890
_reflns_number_gt                1344
_reflns_number_total             1415
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            ic025643p_3.cif
_cod_data_source_block           complex5
_cod_original_cell_volume        3520(1)
_cod_original_formula_sum        'C28 H16 Cl8 Cr N2 O4 '
_cod_database_code               4318419
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,y,1/2-z
-x,-y,-z
x,-y,1/2+z
1/2+x,1/2+y,z
1/2-x,1/2+y,1/2-z
1/2-x,1/2-y,-z
1/2+x,1/2-y,1/2+z
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cr(1) Cr 0.5000 0.14976(8) 0.2500 0.0640(8) Uani 1.00 d S . .
Cl(1) Cl 0.6178(2) 0.1865(1) 0.8137(3) 0.091(1) Uani 1.00 d . . .
Cl(2) Cl 0.6974(3) 0.2956(1) 0.8439(3) 0.102(1) Uani 1.00 d . . .
Cl(3) Cl 0.7039(3) 0.3585(1) 0.5393(4) 0.100(1) Uani 1.00 d . . .
Cl(4) Cl 0.6383(3) 0.3088(1) 0.1987(3) 0.097(1) Uani 1.00 d . . .
O(1) O 0.5594(5) 0.1533(2) 0.4718(7) 0.063(2) Uani 1.00 d . . .
O(2) O 0.5757(5) 0.2021(2) 0.2178(8) 0.069(2) Uani 1.00 d . . .
N(1) N 0.5705(7) 0.0887(3) 0.2001(10) 0.057(3) Uani 1.00 d . . .
C(1) C 0.5958(8) 0.1990(4) 0.498(1) 0.068(4) Uani 1.00 d . . .
C(2) C 0.6241(8) 0.2203(4) 0.645(1) 0.068(4) Uani 1.00 d . . .
C(3) C 0.6601(8) 0.2695(4) 0.658(1) 0.066(4) Uani 1.00 d . . .
C(4) C 0.6648(7) 0.2974(4) 0.521(1) 0.066(3) Uani 1.00 d . . .
C(5) C 0.6353(8) 0.2753(4) 0.370(1) 0.068(4) Uani 1.00 d . . .
C(6) C 0.6024(8) 0.2262(4) 0.358(1) 0.064(3) Uani 1.00 d . . .
C(7) C 0.6395(10) 0.0903(4) 0.148(1) 0.068(4) Uani 1.00 d . . .
C(8) C 0.6865(10) 0.0472(5) 0.113(1) 0.081(4) Uani 1.00 d . . .
C(9) C 0.6524(10) -0.0014(4) 0.135(1) 0.072(4) Uani 1.00 d . . .
C(10) C 0.5763(10) -0.0042(4) 0.192(1) 0.073(4) Uani 1.00 d . . .
C(11) C 0.5384(8) 0.0421(3) 0.221(1) 0.063(4) Uani 1.00 d . . .
C(12) C 0.768(1) 0.0546(5) 0.059(2) 0.102(5) Uani 1.00 d . . .
C(13) C 0.6966(10) -0.0488(5) 0.099(2) 0.096(5) Uani 1.00 d . . .
C(14) C 0.5349(9) -0.0502(4) 0.223(1) 0.080(5) Uani 1.00 d . . .
H(1) H 0.6619 0.1239 0.1297 0.0796 Uiso 1.00 calc . . .
H(2) H 0.7949 0.0223 0.0406 0.1217 Uiso 1.00 calc . . .
H(3) H 0.7620 0.0742 -0.0373 0.1217 Uiso 1.00 calc . . .
H(4) H 0.8114 0.0723 0.1402 0.1217 Uiso 1.00 calc . . .
H(5) H 0.6663 -0.0790 0.1185 0.1167 Uiso 1.00 calc . . .
H(6) H 0.7007 -0.0497 -0.0113 0.1167 Uiso 1.00 calc . . .
H(7) H 0.7532 -0.0511 0.1641 0.1167 Uiso 1.00 calc . . .
H(8) H 0.5606 -0.0827 0.2040 0.0945 Uiso 1.00 calc . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
N N 0.006 0.003
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
O O 0.011 0.006
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
Cl Cl 0.148 0.159
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
C C 0.003 0.002
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
H H 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
Cr Cr 0.321 0.624
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O(1) Cr(1) O(1) 174.5(4) . . 2_655 yes
O(1) Cr(1) O(2) 85.1(3) . . . yes
O(1) Cr(1) O(2) 90.9(3) . . 2_655 yes
O(1) Cr(1) N(1) 93.8(3) . . . yes
O(1) Cr(1) N(1) 90.5(3) . . 2_655 yes
O(1) Cr(1) O(2) 90.9(3) 2_655 . . yes
O(1) Cr(1) O(2) 85.1(3) 2_655 . 2_655 yes
O(1) Cr(1) N(1) 90.5(3) 2_655 . . yes
O(1) Cr(1) N(1) 93.8(3) 2_655 . 2_655 yes
O(2) Cr(1) O(2) 87.4(5) . . 2_655 yes
O(2) Cr(1) N(1) 97.3(3) . . . yes
O(2) Cr(1) N(1) 173.6(4) . . 2_655 yes
O(2) Cr(1) N(1) 173.6(4) 2_655 . . yes
O(2) Cr(1) N(1) 97.3(3) 2_655 . 2_655 yes
N(1) Cr(1) N(1) 78.3(5) . . 2_655 yes
Cr(1) O(1) C(1) 108.3(6) . . . yes
Cr(1) O(2) C(6) 107.4(6) . . . yes
Cr(1) N(1) C(7) 127.3(7) . . . yes
Cr(1) N(1) C(11) 115.2(8) . . . yes
C(7) N(1) C(11) 117.4(9) . . . yes
O(1) C(1) C(2) 124.7(9) . . . yes
O(1) C(1) C(6) 114.8(8) . . . yes
C(2) C(1) C(6) 120.4(10) . . . yes
Cl(1) C(2) C(1) 119.8(8) . . . yes
Cl(1) C(2) C(3) 120.5(8) . . . yes
C(1) C(2) C(3) 119.7(9) . . . yes
Cl(2) C(3) C(2) 119.5(8) . . . yes
Cl(2) C(3) C(4) 119.8(8) . . . yes
C(2) C(3) C(4) 120.7(9) . . . yes
Cl(3) C(4) C(3) 119.9(8) . . . yes
Cl(3) C(4) C(5) 120.9(7) . . . yes
C(3) C(4) C(5) 119.1(9) . . . yes
Cl(4) C(5) C(4) 120.6(8) . . . yes
Cl(4) C(5) C(6) 119.3(8) . . . yes
C(4) C(5) C(6) 120.1(9) . . . yes
O(2) C(6) C(1) 117.0(9) . . . yes
O(2) C(6) C(5) 123.2(9) . . . yes
C(1) C(6) C(5) 119.9(9) . . . yes
N(1) C(7) C(8) 125(1) . . . yes
C(7) C(8) C(9) 116(1) . . . yes
C(7) C(8) C(12) 120(1) . . . yes
C(9) C(8) C(12) 123(1) . . . yes
C(8) C(9) C(10) 118(1) . . . yes
C(8) C(9) C(13) 119(1) . . . yes
C(10) C(9) C(13) 121(1) . . . yes
C(9) C(10) C(11) 117(1) . . . yes
C(9) C(10) C(14) 125(1) . . . yes
C(11) C(10) C(14) 117(1) . . . yes
N(1) C(11) C(10) 124(1) . . . yes
N(1) C(11) C(11) 115.6(6) . . 2_655 yes
C(10) C(11) C(11) 120.2(8) . . 2_655 yes
C(10) C(14) C(14) 122.6(7) . . 2_655 yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cr(1) O(1) 1.929(6) . . yes
Cr(1) O(1) 1.929(6) . 2_655 yes
Cr(1) O(2) 1.895(7) . . yes
Cr(1) O(2) 1.895(7) . 2_655 yes
Cr(1) N(1) 2.060(9) . . yes
Cr(1) N(1) 2.060(9) . 2_655 yes
Cl(1) C(2) 1.715(10) . . yes
Cl(2) C(3) 1.71(1) . . yes
Cl(3) C(4) 1.711(10) . . yes
Cl(4) C(5) 1.722(9) . . yes
O(1) C(1) 1.33(1) . . yes
O(2) C(6) 1.34(1) . . yes
N(1) C(7) 1.29(1) . . yes
N(1) C(11) 1.35(1) . . yes
C(1) C(2) 1.36(1) . . yes
C(1) C(6) 1.42(1) . . yes
C(2) C(3) 1.40(1) . . yes
C(3) C(4) 1.40(1) . . yes
C(4) C(5) 1.40(1) . . yes
C(5) C(6) 1.38(1) . . yes
C(7) C(8) 1.43(2) . . yes
C(8) C(9) 1.41(2) . . yes
C(8) C(12) 1.50(2) . . yes
C(9) C(10) 1.42(2) . . yes
C(9) C(13) 1.50(2) . . yes
C(10) C(11) 1.40(1) . . yes
C(10) C(14) 1.43(2) . . yes
C(11) C(11) 1.44(2) . 2_655 yes
C(14) C(14) 1.31(2) . 2_655 yes
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
Cl(2) Cl(4) 3.400(5) . 1_556 ?
Cl(3) C(13) 3.27(1) . 6_655 ?
Cl(3) C(7) 3.51(1) . 7_656 ?
O(1) C(14) 3.52(1) . 4_555 ?
O(1) C(13) 3.53(2) . 4_555 ?
C(3) C(5) 3.56(2) . 7_656 ?
