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_7714507
_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 H58 N12 Ni2 O16'
_chemical_formula_sum            'C74 H58 N12 Ni2 O16'
_chemical_formula_weight         1488.74
_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                75.096(3)
_cell_angle_beta                 84.014(3)
_cell_angle_gamma                75.408(3)
_cell_formula_units_Z            2
_cell_length_a                   14.0031(12)
_cell_length_b                   16.2239(15)
_cell_length_c                   17.5740(16)
_cell_measurement_reflns_used    9987
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.38
_cell_measurement_theta_min      2.70
_cell_volume                     3730.5(6)
_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 0.996
_diffrn_measured_fraction_theta_max 0.988
_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  0.0781
_diffrn_reflns_av_unetI/netI     0.0653
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            58827
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.243
_diffrn_reflns_theta_max         26.515
_diffrn_reflns_theta_min         2.655
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.578
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5425
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0934 before and 0.0744 after correction.
The Ratio of minimum to maximum transmission is 0.7278.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_description       CUBE
_exptl_crystal_F_000             1540
_refine_diff_density_max         1.069
_refine_diff_density_min         -0.936
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1009
_refine_ls_number_reflns         15307
_refine_ls_number_restraints     308
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0870
_refine_ls_R_factor_gt           0.0580
_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^)+(0.1030P)^2^+2.8220P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1538
_refine_ls_wR_factor_ref         0.1799
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10828
_reflns_number_total             15307
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03084a2.cif
_cod_data_source_block           pmi_tnp
_cod_depositor_comments
'Adding full bibliography for 7714500--7714509.cif.'
_cod_database_code               7714507
_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. Restrained distances
 N8A-C66A \\sim N8-C66
 with sigma of 0.02
 O3A-C63A \\sim O3-C63
 with sigma of 0.02
 O4A-N7A \\sim O4-N7
 with sigma of 0.02
 O5-N7 \\sim O5A-N7A
 with sigma of 0.02
 N9A-C68A \\sim N9-C68
 with sigma of 0.02
 O12-N9 \\sim O12A-N9A
 with sigma of 0.02
 O11A-N9A \\sim O11-N9
 with sigma of 0.02
 O12-O11 \\sim O11A-O12A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C36) \\sim Ueq, Uanis(C36A) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C35A)
\\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C34A) \\sim Ueq, Uanis(C33A) \\sim Ueq,
Uanis(C32) \\sim Ueq, Uanis(C32A) \\sim Ueq, Uanis(C33) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(O13) \\sim Ueq, Uanis(O13A) \\sim Ueq, Uanis(N11) \\sim Ueq, Uanis(N11A)
\\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(O14A) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C31) \\sim Ueq, Uanis(C31A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O3) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(N7) \\sim
Ueq, Uanis(C63) \\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(C65) \\sim Ueq,
Uanis(O10) \\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(C67)
\\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(N8) \\sim Ueq, Uanis(O4A) \\sim Ueq,
Uanis(N7A) \\sim Ueq, Uanis(O5A) \\sim Ueq, Uanis(C64A) \\sim Ueq, Uanis(C65A)
\\sim Ueq, Uanis(C63A) \\sim Ueq, Uanis(O3A) \\sim Ueq, Uanis(C68A) \\sim Ueq,
Uanis(C67A) \\sim Ueq, Uanis(C66A) \\sim Ueq, Uanis(N8A) \\sim Ueq, Uanis(O10A)
\\sim Ueq, Uanis(O9A) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(O12A) \\sim Ueq, Uanis(N9A) \\sim Ueq, Uanis(O11A) \\sim Ueq, Uanis(N9)
\\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(O11) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C36) = Uanis(C36A)
Uanis(C35) = Uanis(C35A)
Uanis(C34) = Uanis(C34A)
Uanis(C32) = Uanis(C32A)
Uanis(C33) = Uanis(C33A)
Uanis(O13) = Uanis(O13A)
Uanis(N11) = Uanis(N11A)
Uanis(O14) = Uanis(O14A)
Uanis(C31) = Uanis(C31A)
Uanis(O4) = Uanis(O4A)
Uanis(N7) = Uanis(N7A)
Uanis(O5) = Uanis(O5A)
Uanis(C64) = Uanis(C64A)
Uanis(C65) = Uanis(C65A)
Uanis(C63) = Uanis(C63A)
Uanis(O3) = Uanis(O3A)
Uanis(C68) = Uanis(C68A)
Uanis(C67) = Uanis(C67A)
Uanis(C66) = Uanis(C66A)
Uanis(N8) = Uanis(N8A)
Uanis(O9) = Uanis(O9A)
Uanis(O10) = Uanis(O10A)
Uanis(N9) = Uanis(N9A)
Uanis(O12) = Uanis(O12A)
Uanis(O11) = Uanis(O11A)
4. Others
 Sof(C32A)=Sof(H32A)=Sof(C33A)=Sof(H33A)=Sof(C34A)=Sof(H34A)=Sof(C35A)=
 Sof(H35A)=Sof(C36A)=Sof(H36A)=1-FVAR(1)
 Sof(C32)=Sof(H32)=Sof(C33)=Sof(H33)=Sof(C34)=Sof(H34)=Sof(C35)=Sof(H35)=
 Sof(C36)=Sof(H36)=FVAR(1)
 Sof(O13A)=Sof(O14A)=Sof(N11A)=1-FVAR(2)
 Sof(O13)=Sof(O14)=Sof(N11)=FVAR(2)
 Sof(C31A)=1-FVAR(3)
 Sof(C31)=FVAR(3)
 Sof(O3A)=Sof(O4A)=Sof(O5A)=Sof(O9A)=Sof(O10A)=Sof(N7A)=Sof(N8A)=Sof(C64A)=
 Sof(C65A)=Sof(H65A)=Sof(C66A)=Sof(C67A)=Sof(H67A)=Sof(C68A)=Sof(C63A)=1-FVAR(4)
 Sof(O3)=Sof(O4)=Sof(O5)=Sof(O9)=Sof(O10)=Sof(N7)=Sof(N8)=Sof(C63)=Sof(C64)=
 Sof(C65)=Sof(H65)=Sof(C66)=Sof(C67)=Sof(H67)=Sof(C68)=FVAR(4)
 Sof(O11A)=Sof(O12A)=Sof(N9A)=1-FVAR(5)
 Sof(O11)=Sof(O12)=Sof(N9)=FVAR(5)
5.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B)
5.b 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), C45(H45), C46(H46), C47(H47), C48(H48),
 C49(H49), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C58(H58),
 C32A(H32A), C59(H59), C33A(H33A), C60(H60), C34A(H34A), C61(H61), C35A(H35A),
 C62(H62), C36A(H36A), C65A(H65A), C67A(H67A), C65(H65), C67(H67), C71(H71),
 C73(H73)
5.c Fitted hexagon refined as free rotating group:
 C64A(C65A,C66A,C67A,C68A,C63A)
5.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              69109
_shelx_fab_checksum              91340
_olex2_submission_special_instructions 'No special instructions were received'