Redetermination of the crystal structure of bis[N,N′-ethylenebis(acetylacetoniminato)nickel(II)] sodium perchlorate, C24H36ClN4NaNi2O8
Dey, Lucky; Rabi, Saswata; Begum, Zinnat A.; Takase, Tsugiko; Rahman, Ismail M.M.; Tiekink, Edward R.T.; Roy, Tapashi Ghosh; Zeitschrift für Kristallographie - New Crystal Structures 236 (2021) 1147–1150; doi:10.1515/ncrs-2021-0254

data_8104551
_publ_section_title
;
 Redetermination of the crystal structure of
 bis[N,N&#x2032;-ethylenebis(acetylacetoniminato)nickel(II)] sodium
 perchlorate, C24H36ClN4NaNi2O8
;
_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1147
_journal_page_last               1150
_journal_paper_doi               10.1515/ncrs-2021-0254
_journal_volume                  236
_journal_year                    2021
_chemical_formula_moiety         'C24 H36 Cl N4 Na Ni2 O8'
_chemical_formula_sum            'C24 H36 Cl N4 Na Ni2 O8'
_chemical_formula_weight         684.43
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 112.0320(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.5909(11)
_cell_length_b                   10.8023(6)
_cell_length_c                   14.5722(8)
_cell_measurement_reflns_used    13693
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      27.59
_cell_measurement_theta_min      3.14
_cell_volume                     2858.7(3)
_computing_cell_refinement       'CrystalClear [2]'
_computing_data_collection       'CrystalClear [2]'
_computing_data_reduction        'CrystalClear [2]'
_computing_molecular_graphics    'ORTEP-3 for Windows [5]'
_computing_publication_material  'SHELXL-2018/3 [4]'
_computing_structure_refinement  'SHELXL-2018/3 [4]'
_computing_structure_solution    'SHELXS [3]'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14344
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.476
_diffrn_reflns_theta_min         3.373
_exptl_absorpt_coefficient_mu    1.479
_exptl_absorpt_correction_T_max  0.732
_exptl_absorpt_correction_T_min  0.550
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB [1]'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_description       block
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.783
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         3261
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0260
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0409P)^2^+2.3767P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0695
_refine_ls_wR_factor_ref         0.0701
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3129
_reflns_number_total             3261
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2021-0254_suppl.cif
_cod_data_source_block           shelx
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               8104551
_shelx_estimated_absorpt_t_min   0.756
_shelx_estimated_absorpt_t_max   0.756
_shelx_res_checksum              20025
_shelx_hkl_checksum              68666