The crystal structure of (dichromato-κ2 O,O′)bis(1,10-phenanthroline-κ2 N,N′)nickel(II), C12H16N4O7Cr2Ni
Wu-Hua, Chen; Gui-Xiang, Xie; Qin, Chen; Yan-Ming, Ruan; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 849–850; doi:10.1515/ncrs-2020-0053

data_8105306
_publ_section_title
;
 The crystal structure of (dichromato-\k2
 O,O&#x2032;)bis(1,10-phenanthroline-\k2 N,N&#x2032;)nickel(II),
 C12H16N4O7Cr2Ni
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur 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  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -42.00  61.00   1.00   18.22    --   15.88   0.00-180.00  103
  2  \w     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       '\w 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/[\s^2^(Fo^2^)+(0.0491P)^2^+0.8864P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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
_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)
;