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_7714505
_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         'C78 H70 N6 Ni2 O9'
_chemical_formula_sum            'C78 H70 N6 Ni2 O9'
_chemical_formula_weight         1352.82
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2023-07-28
_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                90
_cell_angle_beta                 112.230(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.0623(12)
_cell_length_b                   47.324(4)
_cell_length_c                   11.6909(8)
_cell_measurement_reflns_used    9883
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.36
_cell_measurement_theta_min      2.82
_cell_volume                     7714.0(10)
_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      150.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71076
_diffrn_reflns_av_R_equivalents  0.0746
_diffrn_reflns_av_unetI/netI     0.0560
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       56
_diffrn_reflns_limit_k_min       -56
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            73662
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.551
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.544
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6009
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0877 before and 0.0672 after correction.
The Ratio of minimum to maximum transmission is 0.8061.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_description       cube
_exptl_crystal_F_000             2832
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.29
_refine_diff_density_max         1.030
_refine_diff_density_min         -1.212
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       0.0014(2)
_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 2018)'
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     969
_refine_ls_number_reflns         13515
_refine_ls_number_restraints     186
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0922
_refine_ls_R_factor_gt           0.0798
_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^)+52.9260P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1760
_refine_ls_wR_factor_ref         0.1814
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11609
_reflns_number_total             13515
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03084a2.cif
_cod_data_source_block           hmpi_niomeba
_cod_depositor_comments
'Adding full bibliography for 7714500--7714509.cif.'
_cod_database_code               7714505
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9923(4)
 0.0077(4)
2. 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,H) groups
3. Uiso/Uaniso restraints and constraints
C25 \\sim C25A \\sim C26 \\sim C26A \\sim C27 \\sim C27A \\sim C28 \\sim C28A
\\sim C29 \\sim C29A \\sim C30 \\sim C30A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Others
 Sof(C25A)=Sof(C26A)=Sof(H26A)=Sof(C27A)=Sof(H27A)=Sof(C28A)=Sof(H28A)=
 Sof(C29A)=Sof(H29A)=Sof(C30A)=Sof(H30A)=1-FVAR(1)
 Sof(C25)=Sof(C26)=Sof(H26)=Sof(C27)=Sof(H27)=Sof(C28)=Sof(H28)=Sof(C29)=
 Sof(H29)=Sof(C30)=Sof(H30)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C10(H10A,H10B)
5.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), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C45(H45), C46(H46),
  C47(H47), C48(H48), C49(H49), C52(H52), C53(H53), C54(H54), C55(H55),
 C56(H56), C58(H58), C59(H59), C60(H60), C61(H61), C62(H62), C65(H65), C66(H66),
  C68(H68), C69(H69), C73(H73), C74(H74), C76(H76), C77(H77)
5.c Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C70(H70A,H70B,
 H70C), C78(H78A,H78B,H78C)
;
_shelx_res_checksum              75008
_shelx_fab_checksum              38582
_olex2_submission_special_instructions 'No special instructions were received'