Crystal structure of bis(N,2-bis(4-ethoxybenzylidene)hydrazine-1-carbohydrazonothioato-κ2 N,S)nickel(II) — N,N-dimethylformamide (1/2), C44H56N10S2O6Ni
Li, Zhuang-Yu; Liu, E.; Liu, Xiao-Jing; Jian, Fang-Fang; Liang, Tong-ling; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 811–813; doi:10.1515/ncrs-2020-0025

data_8105295
_publ_section_title
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 Crystal structure of
 bis(N,2-bis(4-ethoxybenzylidene)hydrazine-1-carbohydrazonothioato-\k2
 N,S)nickel(II) --- N,N-dimethylformamide (1/2), C44H56N10S2O6Ni
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_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              811
_journal_page_last               813
_journal_paper_doi               10.1515/ncrs-2020-0025
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         'C38 H42 N8 Ni O4 S2, 2(C3 H7 N O)'
_chemical_formula_sum            'C44 H56 N10 Ni O6 S2'
_chemical_formula_weight         943.82
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_atom_sites_solution_primary     direct
_cell_angle_alpha                70.889(3)
_cell_angle_beta                 75.532(2)
_cell_angle_gamma                87.544(3)
_cell_formula_units_Z            1
_cell_length_a                   9.3077(14)
_cell_length_b                   9.9624(14)
_cell_length_c                   14.0449(19)
_cell_measurement_reflns_used    3256
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.37
_cell_volume                     1190.5(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      293.0
_diffrn_measured_fraction_theta_full 0.9931
_diffrn_measured_fraction_theta_max 0.9931
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4 diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_av_unetI/netI     0.0928
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7848
_diffrn_reflns_theta_full        25.0092
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    0.551
_exptl_absorpt_correction_T_max  0.9247
_exptl_absorpt_correction_T_min  0.9014
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.3164
_exptl_crystal_description       block
_exptl_crystal_F_000             498.7864
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.4661
_refine_diff_density_min         -0.3951
_refine_diff_density_rms         0.0965
_refine_ls_d_res_high            0.8406
_refine_ls_d_res_low             9.4048
_refine_ls_goodness_of_fit_ref   1.0052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    46
_refine_ls_number_parameters     286
_refine_ls_number_reflns         4160
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.0021
_refine_ls_R_factor_all          0.1053
_refine_ls_R_factor_gt           0.0528
_refine_ls_shift/su_max          0.0005
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0469P)^2^+0.1456P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1037
_refine_ls_wR_factor_ref         0.1279
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              -10
_reflns_limit_k_max              11
_reflns_limit_k_min              -11
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                2365
_reflns_number_total             4160
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            suppl_ncrs-2020-0025_suppl.cif
_cod_data_source_block           QJ0832
_cod_database_code               8105295
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C18 \\sim O2 \\sim H18a \\sim H18b \\sim C19: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C2(H2a,H2b), C18(H18a,H18b)
3.b Me refined with riding coordinates:
 C1(H1a,H1b,H1c), C19(H19a,H19b,H19c), C22(H22a,H22b,H22c)
3.c Aromatic/amide H refined with riding coordinates:
 N3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C11(H11), C13(H13), C14(H14),
 C16(H16), C17(H17), C20(H20)
3.d Idealised Me refined as rotating group:
 C21(H21a,H21b,H21c)
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_olex2_submission_special_instructions 'No special instructions were received'