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#$Date: 2022-05-19 12:14:45 +0300 (Thu, 19 May 2022) $
#$Revision: 275547 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/53/8105306.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_8105306
loop_
_publ_author_name
'Wu-Hua, Chen'
'Gui-Xiang, Xie'
'Qin, Chen'
'Yan-Ming, Ruan'
_publ_section_title
;
 The crystal structure of (dichromato-κ2
 O,O′)bis(1,10-phenanthroline-κ2 N,N′)nickel(II),
 C12H16N4O7Cr2Ni
;
_journal_issue                   4
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              849
_journal_page_last               850
_journal_paper_doi               10.1515/ncrs-2020-0053
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         'C24 H16 Cr2 N4 Ni O7'
_chemical_formula_sum            'C24 H16 Cr2 N4 Ni O7'
_chemical_formula_weight         635.12
_chemical_name_systematic
;
tris(₂-Oxo)-bis(1'10-phenanthroline)-tetraoxo-di-chromium(VI)-
nike(II)
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.7804(5)
_cell_length_b                   10.3110(5)
_cell_length_c                   16.4118(6)
_cell_measurement_reflns_used    2613
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.6950
_cell_measurement_theta_min      3.7520
_cell_volume                     2331.95(16)
_computing_cell_refinement
'CrysAlisPro 1.171.38.41k (Rigaku OD, 2015)[1]'
_computing_data_collection
'CrysAlisPro 1.171.38.41k (Rigaku OD, 2015)[1]'
_computing_data_reduction
'CrysAlisPro 1.171.38.41k (Rigaku OD, 2015)[1]'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)[2]'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)[2]'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)[3]'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)[4]'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.1151
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.871
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω    -42.00  61.00   1.00   18.22    --   15.88   0.00-180.00  103
  2  ω     12.00  55.00   1.00   18.22    --   15.88 -99.00 150.00   43
;
_diffrn_measurement_device_type  'Rigaku R-axis Spider'
_diffrn_measurement_method       'ω oscillation'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_unetI/netI     0.0436
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.871
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            6978
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.871
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.179
_diffrn_reflns_theta_min         3.501
_exptl_absorpt_coefficient_mu    1.771
_exptl_absorpt_correction_T_max  0.767
_exptl_absorpt_correction_T_min  0.734
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41k (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'translucent dark red'
_exptl_crystal_density_diffrn    1.809
_exptl_crystal_description       block
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.429
_refine_diff_density_min         -0.591
_refine_diff_density_rms         0.128
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         2753
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0438
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0491P)²+0.8864P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1021
_refine_ls_wR_factor_ref         0.1111
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2186
_reflns_number_total             2753
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_ncrs-2020-0053_suppl.cif
_cod_data_source_block           lgh1230-g3(red)
_cod_original_cell_volume        2331.96(17)
_cod_database_code               8105306
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10)
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.5000 0.61861(5) 0.7500 0.02363(16) Uani 1 2 d S T P . .
Cr1 Cr 0.56435(4) 0.92105(5) 0.83073(3) 0.02935(16) Uani 1 1 d . . . . .
O1 O 0.67825(19) 0.9422(3) 0.81649(19) 0.0662(8) Uani 1 1 d . . . . .
O2 O 0.5351(2) 0.9850(3) 0.91573(14) 0.0626(8) Uani 1 1 d . . . . .
O3 O 0.5000 0.9966(3) 0.7500 0.0443(9) Uani 1 2 d S T P . .
O4 O 0.53769(16) 0.7658(2) 0.83101(10) 0.0321(5) Uani 1 1 d . . . . .
N1 N 0.63929(17) 0.6104(2) 0.70156(14) 0.0262(5) Uani 1 1 d . . . . .
N2 N 0.48005(17) 0.4791(3) 0.65990(14) 0.0272(6) Uani 1 1 d . . . . .
C1 C 0.7190(2) 0.6742(3) 0.72425(19) 0.0356(7) Uani 1 1 d . . . . .
H1 H 0.7158 0.7274 0.7699 0.043 Uiso 1 1 calc R . . . .
C2 C 0.8069(2) 0.6648(4) 0.6828(2) 0.0415(8) Uani 1 1 d . . . . .
H2 H 0.8609 0.7105 0.7009 0.050 Uiso 1 1 calc R . . . .
C3 C 0.8130(2) 0.5877(4) 0.6150(2) 0.0417(9) Uani 1 1 d . . . . .
H3 H 0.8710 0.5820 0.5862 0.050 Uiso 1 1 calc R . . . .
C4 C 0.7313(2) 0.5172(3) 0.58913(17) 0.0341(7) Uani 1 1 d . . . . .
C5 C 0.7308(3) 0.4336(4) 0.5201(2) 0.0440(9) Uani 1 1 d . . . . .
H5 H 0.7862 0.4270 0.4879 0.053 Uiso 1 1 calc R . . . .
C6 C 0.6513(3) 0.3637(4) 0.5006(2) 0.0443(9) Uani 1 1 d . . . . .
H6 H 0.6534 0.3084 0.4559 0.053 Uiso 1 1 calc R . . . .
C7 C 0.5634(2) 0.3727(3) 0.54727(18) 0.0344(7) Uani 1 1 d . . . . .
C8 C 0.4794(3) 0.3007(4) 0.5316(2) 0.0436(9) Uani 1 1 d . . . . .
H8 H 0.4780 0.2409 0.4892 0.052 Uiso 1 1 calc R . . . .
C9 C 0.3997(3) 0.3194(4) 0.5794(2) 0.0457(9) Uani 1 1 d . . . . .
H9 H 0.3436 0.2717 0.5698 0.055 Uiso 1 1 calc R . . . .
C10 C 0.4019(2) 0.4101(3) 0.6428(2) 0.0373(8) Uani 1 1 d . . . . .
H10 H 0.3463 0.4223 0.6740 0.045 Uiso 1 1 calc R . . . .
C11 C 0.5608(2) 0.4600(3) 0.61338(16) 0.0267(6) Uani 1 1 d . . . . .
C12 C 0.6457(2) 0.5320(3) 0.63496(16) 0.0259(6) Uani 1 1 d . . . . .
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'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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
O4 Ni1 O4 86.47(12) 3_656 .
N1 Ni1 O4 92.49(9) 3_656 3_656
N1 Ni1 O4 90.91(9) 3_656 .
N1 Ni1 O4 92.49(9) . .
N1 Ni1 O4 90.91(9) . 3_656
N1 Ni1 N1 175.33(14) 3_656 .
N1 Ni1 N2 96.98(9) 3_656 .
N1 Ni1 N2 79.76(9) . .
N1 Ni1 N2 96.98(9) . 3_656
N1 Ni1 N2 79.76(9) 3_656 3_656
N2 Ni1 O4 171.82(9) . .
N2 Ni1 O4 171.82(9) 3_656 3_656
N2 Ni1 O4 91.00(9) . 3_656
N2 Ni1 O4 91.00(9) 3_656 .
N2 Ni1 N2 92.54(14) . 3_656
O1 Cr1 O3 108.73(12) . .
O1 Cr1 O4 110.63(14) . .
O2 Cr1 O1 108.61(17) . .
O2 Cr1 O3 110.18(13) . .
O2 Cr1 O4 110.12(13) . .
O4 Cr1 O3 108.55(13) . .
Cr1 O3 Cr1 127.9(2) 3_656 .
Cr1 O4 Ni1 139.82(11) . .
C1 N1 Ni1 129.3(2) . .
C1 N1 C12 117.6(3) . .
C12 N1 Ni1 112.99(18) . .
C10 N2 Ni1 129.1(2) . .
C10 N2 C11 117.9(3) . .
C11 N2 Ni1 112.95(19) . .
N1 C1 H1 118.5 . .
N1 C1 C2 123.1(3) . .
C2 C1 H1 118.5 . .
C1 C2 H2 120.3 . .
C3 C2 C1 119.4(3) . .
C3 C2 H2 120.3 . .
C2 C3 H3 120.1 . .
C2 C3 C4 119.8(3) . .
C4 C3 H3 120.1 . .
C3 C4 C5 123.9(3) . .
C3 C4 C12 117.0(3) . .
C12 C4 C5 119.1(3) . .
C4 C5 H5 119.5 . .
C6 C5 C4 121.0(3) . .
C6 C5 H5 119.5 . .
C5 C6 H6 119.2 . .
C5 C6 C7 121.7(3) . .
C7 C6 H6 119.2 . .
C8 C7 C6 124.5(3) . .
C8 C7 C11 117.3(3) . .
C11 C7 C6 118.3(3) . .
C7 C8 H8 120.4 . .
C9 C8 C7 119.1(3) . .
C9 C8 H8 120.4 . .
C8 C9 H9 119.8 . .
C8 C9 C10 120.3(3) . .
C10 C9 H9 119.8 . .
N2 C10 C9 122.4(3) . .
N2 C10 H10 118.8 . .
C9 C10 H10 118.8 . .
N2 C11 C7 123.0(3) . .
N2 C11 C12 117.0(3) . .
C7 C11 C12 120.0(3) . .
N1 C12 C4 123.2(3) . .
N1 C12 C11 117.0(2) . .
C4 C12 C11 119.8(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O4 2.084(2) .
Ni1 O4 2.084(2) 3_656
Ni1 N1 2.079(2) .
Ni1 N1 2.079(2) 3_656
Ni1 N2 2.081(2) .
Ni1 N2 2.081(2) 3_656
Cr1 O1 1.602(3) .
Cr1 O2 1.595(2) .
Cr1 O3 1.7744(16) .
Cr1 O4 1.642(2) .
O3 Cr1 1.7744(16) 3_656
N1 C1 1.334(4) .
N1 C12 1.362(4) .
N2 C10 1.321(4) .
N2 C11 1.363(3) .
C1 H1 0.9300 .
C1 C2 1.392(4) .
C2 H2 0.9300 .
C2 C3 1.370(5) .
C3 H3 0.9300 .
C3 C4 1.406(5) .
C4 C5 1.424(4) .
C4 C12 1.408(4) .
C5 H5 0.9300 .
C5 C6 1.350(5) .
C6 H6 0.9300 .
C6 C7 1.435(5) .
C7 C8 1.399(5) .
C7 C11 1.410(4) .
C8 H8 0.9300 .
C8 C9 1.363(5) .
C9 H9 0.9300 .
C9 C10 1.399(5) .
C10 H10 0.9300 .
C11 C12 1.430(4) .
