Binuclear Nickel Complexes of a New Di(hydroxyphenyl)imidazolate
Nikovskiy, Igor A.; Karnaukh, Kseniia M.; Aleshin, Dmitry Yu.; Spiridonov, Kirill A.; Danshina, Anastasia A.; Nelyubina, Yulia V.; Polezhaev, Alexander V.; Novikov, Valentin V.; Magnetochemistry 8 (2022) 132–; doi:10.3390/magnetochemistry8100132

data_1567908
_publ_section_title
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 Binuclear Nickel Complexes of a New Di(hydroxyphenyl)imidazolate
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_journal_issue                   10
_journal_name_full               Magnetochemistry
_journal_page_first              132
_journal_paper_doi               10.3390/magnetochemistry8100132
_journal_volume                  8
_journal_year                    2022
_chemical_formula_moiety
'C59 H49 N10 Ni2 O2, Cl, 2(C H4 O), 0.75(C4 H10 O)'
_chemical_formula_sum            'C64 H64.5 Cl N10 Ni2 O4.75'
_chemical_formula_weight         1202.62
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-09-13
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_cell_angle_alpha                77.732(3)
_cell_angle_beta                 70.231(3)
_cell_angle_gamma                81.830(3)
_cell_formula_units_Z            2
_cell_length_a                   13.555(2)
_cell_length_b                   15.389(3)
_cell_length_c                   17.007(3)
_cell_measurement_reflns_used    4139
_cell_measurement_temperature    120
_cell_measurement_theta_max      30.53
_cell_measurement_theta_min      2.18
_cell_volume                     3252.8(10)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II DUO CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1590
_diffrn_reflns_av_unetI/netI     0.1795
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            45304
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.998
_diffrn_reflns_theta_min         1.702
_exptl_absorpt_coefficient_mu    0.673
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5714
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0932 before and 0.0690 after correction.
The Ratio of minimum to maximum transmission is 0.7658.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_description       plate
_exptl_crystal_F_000             1259
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.955
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.955
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     756
_refine_ls_number_reflns         14150
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.955
_refine_ls_R_factor_all          0.1660
_refine_ls_R_factor_gt           0.0794
_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^)+(0.1038P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1799
_refine_ls_wR_factor_ref         0.2188
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6921
_reflns_number_total             14150
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            '[(bipy)4Ni2(L)](Cl).cif'
_cod_data_source_block           nil2cl
_cod_original_cell_volume        3253.0(9)
_cod_original_formula_sum        'C64 H64.50 Cl N10 Ni2 O4.75'
_cod_database_code               1567908
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.987
_shelx_estimated_absorpt_t_min   0.936
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Others
 Fixed Sof: O3S(0.75) C3S(0.75) H3SA(0.75) H3SB(0.75) C4S(0.75) H4SA(0.75)
 H4SB(0.75) H4SC(0.75) C5S(0.75) H5SA(0.75) H5SB(0.75) C6S(0.75) H6SA(0.75)
 H6SB(0.75) H6SC(0.75)
3.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C18(H18A,H18B), C3S(H3SA,H3SB), C5S(H5SA,H5SB)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C5(H5), C7(H7), C8(H8), C13(H13), C15(H15), C16(H16), C20(H20),
 C21(H21), C22(H22), C23(H23), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30),
  C31(H31), C32(H32), C33(H33), C36(H36), C37(H37), C38(H38), C39(H39),
 C40(H40), C41(H41), C42(H42), C43(H43), C46(H46), C47(H47), C48(H48), C49(H49),
  C50(H50), C51(H51), C52(H52), C53(H53), C56(H56), C57(H57), C58(H58), C59(H59)
3.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C19(H19A,H19B,H19C), C1S(H1SA,H1SB,H1SC), C2S(H2SA,H2SB,
 H2SC), C4S(H4SA,H4SB,H4SC), C6S(H6SA,H6SB,H6SC)
3.d Idealised tetrahedral OH refined as rotating group:
 O1S(H1S), O2S(H2S)
;
_olex2_submission_special_instructions 'No special instructions were received'