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_1567909
_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         'C67 H49 N10 Ni2 O2, Cl, 3(C H4 O)'
_chemical_formula_sum            'C70 H61 Cl N10 Ni2 O5'
_chemical_formula_weight         1275.15
_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   mixed
_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                72.9350(10)
_cell_angle_beta                 77.2100(10)
_cell_angle_gamma                89.9820(10)
_cell_formula_units_Z            2
_cell_length_a                   12.2327(3)
_cell_length_b                   13.0491(3)
_cell_length_c                   20.7742(5)
_cell_measurement_reflns_used    9990
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.67
_cell_measurement_theta_min      2.25
_cell_volume                     3084.00(13)
_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      100.00
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Quest D8'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1989
_diffrn_reflns_av_unetI/netI     0.2337
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            41247
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.108
_exptl_absorpt_coefficient_mu    0.715
_exptl_absorpt_correction_T_max  0.2657
_exptl_absorpt_correction_T_min  0.2088
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1355 before and 0.0459 after correction.
The Ratio of minimum to maximum transmission is 0.8322.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_description       prism
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.109
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     811
_refine_ls_number_reflns         10859
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.2209
_refine_ls_R_factor_gt           0.0811
_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^)+(0.1576P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2341
_refine_ls_wR_factor_ref         0.2702
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5967
_reflns_number_total             10859
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            '[(phen)4Ni2(L)](Cl).cif'
_cod_data_source_block           niphen
_cod_database_code               1567909
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.870
_shelx_estimated_absorpt_t_min   0.836
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C19-C18' \\sim C19'-C18
 with sigma of 0.02
 C18'-C16 \\sim C18-C16
 with sigma of 0.02
 C11'-C10 \\sim C11-C10
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C18) = Uanis(C18')
Uanis(C19) = Uanis(C19')
Uanis(C11') = Uanis(C11)
4. Others
 Sof(C18')=Sof(H18C)=Sof(H18D)=Sof(C19')=Sof(H19D)=Sof(H19E)=Sof(H19F)=1-FVAR(1)
 Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=FVAR(1)
 Sof(H10C)=Sof(H10D)=Sof(C11')=Sof(H11D)=Sof(H11E)=Sof(H11F)=1-FVAR(2)
 Sof(H10A)=Sof(H10B)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=FVAR(2)
5.a Riding coordinates:
 O1S(H1S), O2S(H2S), O3S(H3S)
5.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C10(H10C,H10D), C18(H18A,H18B), C18'(H18C,H18D)
5.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C6(H6), C7(H7), C9(H9), C14(H14), C15(H15), C17(H17), C20(H20),
 C21(H21), C22(H22), C24(H24), C25(H25), C27(H27), C28(H28), C29(H29), C32(H32),
  C33(H33), C34(H34), C36(H36), C37(H37), C39(H39), C40(H40), C41(H41),
 C44(H44), C45(H45), C46(H46), C48(H48), C49(H49), C51(H51), C52(H52), C53(H53),
  C56(H56), C57(H57), C58(H58), C60(H60), C61(H61), C63(H63), C64(H64), C65(H65)
5.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C19(H19A,H19B,H19C), C11'(H11D,H11E,H11F), C19'(H19D,
 H19E,H19F), C1S(H1SA,H1SB,H1SC), C2S(H2SA,H2SB,H2SC), C3S(H3SA,H3SB,H3SC)
;
_olex2_submission_special_instructions 'No special instructions were received'