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_7714509
_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         'C68 H66 N6 Ni2 O7'
_chemical_formula_sum            'C68 H66 N6 Ni2 O7'
_chemical_formula_weight         1196.68
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   38.1705(19)
_cell_length_b                   38.1705(19)
_cell_length_c                   22.8167(10)
_cell_measurement_reflns_used    9674
_cell_measurement_temperature    181(2)
_cell_measurement_theta_max      27.69
_cell_measurement_theta_min      2.62
_cell_volume                     28790(2)
_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      181.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_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  0.0939
_diffrn_reflns_av_unetI/netI     0.0371
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            155251
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.499
_diffrn_reflns_theta_min         2.394
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.644
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5155
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1416 before and 0.0993 after correction.
The Ratio of minimum to maximum transmission is 0.6915.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_description       CUBE
_exptl_crystal_F_000             11304
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.28
_refine_diff_density_max         1.365
_refine_diff_density_min         -0.727
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     764
_refine_ls_number_reflns         13242
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.1003
_refine_ls_R_factor_gt           0.0609
_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^)+(0.1099P)^2^+115.7863P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1631
_refine_ls_wR_factor_ref         0.1981
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9249
_reflns_number_total             13242
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03084a2.cif
_cod_data_source_block           et2cni_oac
_cod_depositor_comments
'Adding full bibliography for 7714500--7714509.cif.'
_cod_original_cell_volume        28790(3)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7714509
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.840
_shelx_estimated_absorpt_t_min   0.730
_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,H) groups
2. Restrained distances
 C42-C41 \\sim C42A-C41A
 with sigma of 0.02
 N6-C41A \\sim N6-C41
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C42) \\sim Ueq, Uanis(C42A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C41A) \\sim Ueq, Uanis(C41) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C41) = Uanis(C41A)
Uanis(C42) = Uanis(C42A)
4. Others
 Sof(C42A)=Sof(H42D)=Sof(H42E)=Sof(H42F)=1-FVAR(1)
 Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(H42C)=FVAR(1)
 Sof(C41A)=Sof(H41C)=Sof(H41D)=1-FVAR(2)
 Sof(C41)=Sof(H41A)=Sof(H41B)=FVAR(2)
5.a Rotating group:
 O5(H5A,H5B)
5.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C39(H39A,H39B),
 C41(H41A,H41B), C41A(H41C,H41D)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C14(H14), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20),
 C21(H21), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C32(H32), C33(H33),
  C34(H34), C35(H35), C36(H36), C47(H47), C48(H48), C49(H49), C50(H50),
 C51(H51), C54(H54), C55(H55), C56(H56), C57(H57), C58(H58), C60(H60), C61(H61),
  C62(H62), C63(H63), C64(H64)
5.d Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C42A(H42D,H42E,
 H42F), C43(H43A,H43B,H43C), C66(H66A,H66B,H66C), C68(H68A,H68B,H68C)
;
_shelx_res_checksum              91578
_shelx_fab_checksum              23799
_olex2_submission_special_instructions 'No special instructions were received'