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_7714502
_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         'C66 H54 F6 N6 Ni2 O6'
_chemical_formula_sum            'C66 H54 F6 N6 Ni2 O6'
_chemical_formula_weight         1258.57
_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                87.747(4)
_cell_angle_beta                 74.480(4)
_cell_angle_gamma                72.929(4)
_cell_formula_units_Z            2
_cell_length_a                   12.6449(17)
_cell_length_b                   13.4163(19)
_cell_length_c                   22.200(3)
_cell_measurement_reflns_used    9968
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.85
_cell_measurement_theta_min      2.69
_cell_volume                     3465.8(8)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.1011
_diffrn_reflns_av_unetI/netI     0.0974
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            40229
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         2.925
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.609
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.3784
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1292 before and 0.0880 after correction.
The Ratio of minimum to maximum transmission is 0.5077.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_description       cube
_exptl_crystal_F_000             1300
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.909
_refine_diff_density_min         -0.826
_refine_diff_density_rms         0.119
_refine_ls_extinction_coef       0.0125(12)
_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   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     781
_refine_ls_number_reflns         12114
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1437
_refine_ls_R_factor_gt           0.0951
_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^)+(0.1003P)^2^+22.7644P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2434
_refine_ls_wR_factor_ref         0.2708
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7880
_reflns_number_total             12114
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03084a2.cif
_cod_data_source_block           hpmi_tfa
_cod_depositor_comments
'Adding full bibliography for 7714500--7714509.cif.'
_cod_database_code               7714502
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.925
_shelx_estimated_absorpt_t_min   0.843
_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(F5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C31) \\sim Ueq, Uanis(C31A) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C32A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C32) = Uanis(C32A)
Uanis(C33) = Uanis(C33A)
Uanis(C34) = Uanis(C34A)
Uanis(C35) = Uanis(C35A)
Uanis(C36) = Uanis(C36A)
Uanis(C31) = Uanis(C31A)
Uanis(F5) = Uanis(F5A)
3. Others
 Sof(C33A)=Sof(H33A)=Sof(C32A)=Sof(H32A)=1-FVAR(1)
 Sof(C33)=Sof(H33)=Sof(C32)=Sof(H32)=FVAR(1)
 Sof(C34A)=Sof(H34A)=1-FVAR(2)
 Sof(C34)=Sof(H34)=FVAR(2)
 Sof(C31A)=Sof(C36A)=Sof(H36A)=Sof(C35A)=Sof(H35A)=1-FVAR(3)
 Sof(C31)=Sof(C36)=Sof(H36)=Sof(C35)=Sof(H35)=FVAR(3)
 Sof(F5A)=1-FVAR(4)
 Sof(F5)=FVAR(4)
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), C36(H36), C35(H35),
  C34(H34), C33(H33), C32(H32), C36A(H36A), C35A(H35A), C34A(H34A), C33A(H33A),
 C32A(H32A), 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)
4.c Fitted hexagon refined as free rotating group:
 C31(C36,C35,C34,C33,C32), C31A(C36A,C35A,C34A,C33A,C32A)
4.d Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,
 H41C)
;
_shelx_res_checksum              26666
_shelx_fab_checksum              88062
_olex2_submission_special_instructions 'No special instructions were received'