Crystal structure of diammonium bis[tris(oxamide dioxime-κ^2^<i>N</i>,<i>N</i>')nickel(II)] bis[tris(oxalato-κ^2^<i>O</i>,<i>O</i>')chromate(III)] 6.76-hydrate
Mbiangué, Yves Alain; Bijvédé, Alfred; Kenfack Tsobnang, Patrice; Wenger, Emmanuel; Lecomte, Claude; Acta Crystallographica Section E 76 (2020) 1732–1736; doi:10.1107/S2056989020013390

data_2243622
_publ_section_title
;
 Crystal structure of diammonium bis[tris(oxamide
 dioxime-\k^2^<i>N</i>,<i>N</i>')nickel(II)]
 bis[tris(oxalato-\k^2^<i>O</i>,<i>O</i>')chromate(III)] 6.76-hydrate
;
_journal_coeditor_code           WM5586
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1732
_journal_page_last               1736
_journal_paper_doi               10.1107/S2056989020013390
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac
;
(N H4)2 [Ni (C2 H6 N4 O3)3] [Cr (C2 O4)3], 6.76H2 O
;
_chemical_formula_moiety
;
2(H4 N +), 2(C6 H18 N12 Ni O6 2+), 2(C6 Cr O12 3-), 6.76(H2 O)
;
_chemical_formula_sum            'C24 H57.53 Cr2 N26 Ni2 O42.76'
_chemical_formula_weight         1616.12
_chemical_name_systematic
;Diammonium bis[tris(oxamide
dioxime-\k^2^<i>N</i>,<i>N</i>')nickel(II)] bis[tris(oxalato-\k^2^<i>O</i><i>,O</i>')chromate(III)] 6.76-hydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 95.562(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.8065(3)
_cell_length_b                   16.6719(4)
_cell_length_c                   37.2296(9)
_cell_measurement_reflns_used    25623
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      76.0580
_cell_measurement_theta_min      3.5580
_cell_volume                     6058.1(3)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2015)
;
_computing_data_collection
;
CrysAlisPro (Rigaku OD, 2015)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku OD, 2015)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012) and DIAMOND (Brandenburg & Putz,
2018)
;
_computing_publication_material
;
WINGX (Farrugia, 2012) and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 10.4508
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Rigaku Supernova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0628
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            97200
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.051
_diffrn_reflns_theta_min         3.566
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    4.742
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.503
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2015)
;
_exptl_crystal_colour            'light violet'
_exptl_crystal_density_diffrn    1.772
_exptl_crystal_description       block
_exptl_crystal_F_000             3319
_exptl_crystal_size_max          0.221
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.046
_refine_diff_density_max         1.421
_refine_diff_density_min         -1.029
_refine_ls_extinction_coef       0.00017(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL-2018/3 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     903
_refine_ls_number_reflns         12706
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0596
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0870P)^2^+14.3935P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1715
_refine_ls_wR_factor_ref         0.1778
_reflns_number_gt                11294
_reflns_number_total             12706
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5586sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2243622
_shelx_hkl_checksum              63752
_shelx_res_checksum              47099
_cod_database_fobs_code 2243622