Bimetallic nickel complexes containing imidazole-based phenolate ligands as efficient catalysts for the copolymerization of carbon dioxide with epoxides.
Hsu, Han-Fang; Liu, Guan-Lin; Su, Yu-Chia; Ko, Bao-Tsan; Dalton transactions (Cambridge, England : 2003) 53 (2023) 299–314; doi:10.1039/d3dt03084a

data_7714503
_publ_section_title
;
 Bimetallic nickel complexes containing imidazole-based phenolate ligands
 as efficient catalysts for the copolymerization of carbon dioxide with
 epoxides.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              299
_journal_page_last               314
_journal_paper_doi               10.1039/d3dt03084a
_journal_volume                  53
_journal_year                    2023
_chemical_formula_moiety         'C74 H60 N10 Ni2 O12'
_chemical_formula_sum            'C74 H60 N10 Ni2 O12'
_chemical_formula_weight         1398.74
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2023-08-18
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2023-09-06 deposited with the CCDC.	2023-11-17 downloaded from the CCDC.
;
_cell_angle_alpha                80.804(2)
_cell_angle_beta                 87.163(2)
_cell_angle_gamma                80.733(2)
_cell_formula_units_Z            2
_cell_length_a                   13.7649(7)
_cell_length_b                   13.7918(7)
_cell_length_c                   17.4684(9)
_cell_measurement_reflns_used    9790
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.36
_cell_measurement_theta_min      2.67
_cell_volume                     3229.9(3)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            50206
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.243
_diffrn_reflns_theta_max         26.412
_diffrn_reflns_theta_min         2.830
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.657
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6207
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0730 before and 0.0570 after correction.
The Ratio of minimum to maximum transmission is 0.8327.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_description       CUBE
_exptl_crystal_F_000             1452
_refine_diff_density_max         0.653
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     904
_refine_ls_number_reflns         13155
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0480
_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^)+(0.0093P)^2^+7.6131P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0975
_refine_ls_wR_factor_ref         0.1115
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10545
_reflns_number_total             13155
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03084a2.cif
_cod_data_source_block           pmi_dnp
_cod_depositor_comments
'Adding full bibliography for 7714500--7714509.cif.'
_cod_database_code               7714503
_shelx_shelxl_version_number     2018/3
_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
2. Uiso/Uaniso restraints and constraints
Uanis(O9A) \\sim Ueq, Uanis(N8A) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(N8)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C68) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C65A) \\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C66A) \\sim Ueq, Uanis(C66)
\\sim Ueq, Uanis(C67A) \\sim Ueq, Uanis(C67) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O9) = Uanis(O9A)
Uanis(N8) = Uanis(N8A)
Uanis(C65) = Uanis(C65A)
Uanis(C66) = Uanis(C66A)
Uanis(C67) = Uanis(C67A)
3. Others
 Sof(O9A)=Sof(N8A)=1-FVAR(1)
 Sof(O9)=Sof(N8)=FVAR(1)
 Sof(C65A)=Sof(H65A)=Sof(C66A)=Sof(C67A)=Sof(H67A)=Sof(H68A)=1-FVAR(2)
 Sof(C65)=Sof(H65)=Sof(C66)=Sof(C67)=Sof(H67)=Sof(H68)=FVAR(2)
4.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C14(H14), C16(H16), C19(H19), C20(H20), C21(H21), C22(H22),
 C23(H23), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C32(H32), C33(H33),
  C34(H34), C35(H35), C36(H36), C44(H44), C45(H45), C46(H46), C47(H47),
 C48(H48), C51(H51), C52(H52), C53(H53), C54(H54), C55(H55), C57(H57), C58(H58),
  C59(H59), C60(H60), C61(H61), C65(H65), C65A(H65A), C67(H67), C67A(H67A),
 C68(H68), C68(H68A), C71(H71), C73(H73), C74(H74)
4.c Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,
 H40C)
;
_shelx_res_checksum              84190
_shelx_fab_checksum              59511
_olex2_submission_special_instructions 'No special instructions were received'