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#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/84/4318417.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_4318417
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         'C16 H6 Cl8 Cr N2 O4 '
_chemical_formula_sum            'C16 H6 Cl8 Cr N2 O4'
_chemical_formula_weight         625.85
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                109.517(5)
_cell_angle_beta                 99.967(3)
_cell_angle_gamma                92.822(2)
_cell_formula_units_Z            1
_cell_length_a                   5.9174(8)
_cell_length_b                   9.4798(8)
_cell_length_c                   10.672(2)
_cell_measurement_temperature    296.2
_cell_volume                     552.03(14)
_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 0.9355
_diffrn_measured_fraction_theta_max 0.9355
_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  0.015
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3999
_diffrn_reflns_theta_full        27.26
_diffrn_reflns_theta_max         27.26
_exptl_absorpt_coefficient_mu    1.513
_exptl_absorpt_correction_type   REQABA
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.882
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platet
_exptl_crystal_size_max          0.225
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.38
_refine_diff_density_min         -0.26
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.678
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     154
_refine_ls_number_reflns         2991
_refine_ls_R_factor_gt           0.0420
_refine_ls_shift/su_max          0.0004
_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         0.0840
_reflns_number_gt                2991
_reflns_number_total             2306
_reflns_threshold_expression     F²>3.0σ(F²)
_cod_data_source_file            ic025643p_1.cif
_cod_data_source_block           complex1
_cod_original_cell_volume        552.0(2)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C16 H6 Cl8 Cr N2 O4 '
_cod_database_code               4318417
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-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 1.0000 0.0000 1.0000 0.0396(2) Uani 1.00 d S . .
Cl(1) Cl 0.6353(2) -0.0015(1) 1.3775(1) 0.0538(3) Uani 1.00 d . . .
Cl(2) Cl 0.8085(2) -0.2497(1) 1.4945(1) 0.0591(3) Uani 1.00 d . . .
Cl(3) Cl 1.1706(2) -0.4510(1) 1.3674(1) 0.0594(3) Uani 1.00 d . . .
Cl(4) Cl 1.3372(2) -0.4165(1) 1.1128(1) 0.0637(4) Uani 1.00 d . . .
O(1) O 0.8632(4) 0.0127(3) 1.1548(2) 0.0429(7) Uani 1.00 d . . .
O(2) O 1.1402(5) -0.1649(3) 1.0381(3) 0.0450(7) Uani 1.00 d . . .
N(1) N 0.7203(7) -0.1465(4) 0.8799(3) 0.0498(10) Uani 1.00 d . . .
C(1) C 0.9191(6) -0.0932(4) 1.2035(4) 0.0388(9) Uani 1.00 d . . .
C(2) C 0.8341(6) -0.1143(4) 1.3109(4) 0.0397(9) Uani 1.00 d . . .
C(3) C 0.9105(6) -0.2270(4) 1.3590(4) 0.043(1) Uani 1.00 d . . .
C(4) C 1.0703(6) -0.3181(4) 1.3016(4) 0.044(1) Uani 1.00 d . . .
C(5) C 1.1485(6) -0.3023(4) 1.1907(4) 0.0408(10) Uani 1.00 d . . .
C(6) C 1.0750(6) -0.1903(4) 1.1409(4) 0.0385(9) Uani 1.00 d . . .
C(7) C 0.5537(8) -0.2250(5) 0.8259(4) 0.050(1) Uani 1.00 d . . .
C(8) C 0.3434(9) -0.3230(6) 0.7579(6) 0.063(1) Uani 1.00 d . . .
H(1) H 0.25(1) -0.275(9) 0.721(8) 0.14(2) Uiso 1.00 calc . . .
H(2) H 0.25(2) -0.34(1) 0.830(10) 0.17(2) Uiso 1.00 calc . . .
H(3) H 0.36(1) -0.413(7) 0.702(6) 0.10(2) 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
Cr Cr 0.321 0.624
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
N N 0.006 0.003
;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)
;
O O 0.011 0.006
;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)
;
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) 180.0 . . 2_757 yes
O(1) Cr(1) O(2) 83.68(10) . . . yes
O(1) Cr(1) O(2) 96.32(10) . . 2_757 yes
O(1) Cr(1) N(1) 88.2(1) . . . yes
O(1) Cr(1) N(1) 91.8(1) . . 2_757 yes
O(1) Cr(1) O(2) 96.32(10) 2_757 . . yes
O(1) Cr(1) O(2) 83.68(10) 2_757 . 2_757 yes
O(1) Cr(1) N(1) 91.8(1) 2_757 . . yes
O(1) Cr(1) N(1) 88.2(1) 2_757 . 2_757 yes
O(2) Cr(1) O(2) 180.0 . . 2_757 yes
O(2) Cr(1) N(1) 89.6(1) . . . yes
O(2) Cr(1) N(1) 90.4(1) . . 2_757 yes
O(2) Cr(1) N(1) 90.4(1) 2_757 . . yes
O(2) Cr(1) N(1) 89.6(1) 2_757 . 2_757 yes
N(1) Cr(1) N(1) 180.0000(1) . . 2_757 yes
Cr(1) O(1) C(1) 111.8(2) . . . yes
Cr(1) O(2) C(6) 112.2(2) . . . yes
Cr(1) N(1) C(7) 172.2(3) . . . yes
O(1) C(1) C(2) 123.5(3) . . . yes
O(1) C(1) C(6) 116.6(3) . . . yes
C(2) C(1) C(6) 119.9(3) . . . yes
Cl(1) C(2) C(1) 118.4(3) . . . yes
Cl(1) C(2) C(3) 122.3(3) . . . yes
C(1) C(2) C(3) 119.2(3) . . . yes
Cl(2) C(3) C(2) 118.9(3) . . . yes
Cl(2) C(3) C(4) 120.2(3) . . . yes
C(2) C(3) C(4) 121.0(3) . . . yes
Cl(3) C(4) C(3) 120.0(3) . . . yes
Cl(3) C(4) C(5) 119.8(3) . . . yes
C(3) C(4) C(5) 120.2(3) . . . yes
Cl(4) C(5) C(4) 121.9(3) . . . yes
Cl(4) C(5) C(6) 118.2(3) . . . yes
C(4) C(5) C(6) 119.9(3) . . . yes
O(2) C(6) C(1) 115.6(3) . . . yes
O(2) C(6) C(5) 124.7(3) . . . yes
C(1) C(6) C(5) 119.7(3) . . . yes
N(1) C(7) C(8) 179.7(4) . . . 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) 1.934(3) . . yes
Cr(1) O(1) 1.934(3) . 2_757 yes
Cr(1) O(2) 1.933(2) . . yes
Cr(1) O(2) 1.933(2) . 2_757 yes
Cr(1) N(1) 2.040(4) . . yes
Cr(1) N(1) 2.040(4) . 2_757 yes
Cl(1) C(2) 1.714(3) . . yes
Cl(2) C(3) 1.732(4) . . yes
Cl(3) C(4) 1.718(4) . . yes
Cl(4) C(5) 1.718(3) . . yes
O(1) C(1) 1.308(4) . . yes
O(2) C(6) 1.313(4) . . yes
N(1) C(7) 1.141(6) . . yes
C(1) C(2) 1.397(5) . . yes
C(1) C(6) 1.425(5) . . yes
C(2) C(3) 1.393(5) . . yes
C(3) C(4) 1.394(5) . . yes
C(4) C(5) 1.392(5) . . yes
C(5) C(6) 1.393(5) . . yes
C(7) C(8) 1.436(7) . . yes
