Tetracosanuclear nickel complexes as effective catalysts for cycloaddition of carbon dioxide with epoxides.
Liu, Guan-Lin; Wu, En-Hsu; Hung, Yu-Ching; Chou, Wei-Chi; Hung, Chia-Hsin; Lin, Chu-Chieh; Ko, Bao-Tsan; Dalton transactions (Cambridge, England : 2003) 53 (2024) 1425–1429; doi:10.1039/d3dt03460g

data_7714810
_publ_section_title
;
 Tetracosanuclear nickel complexes as effective catalysts for
 cycloaddition of carbon dioxide with epoxides.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1425
_journal_page_last               1429
_journal_paper_doi               10.1039/d3dt03460g
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C176 H272 N16 Ni24 O88, [14.5 CH2Cl2 ]'
_chemical_formula_sum            'C234 H388 Cl116 N16 Ni24 O88'
_chemical_formula_weight         10354.82
_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_Hall           '-I 4'
_space_group_name_H-M_alt        'I 4/m'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-12-05
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-12-10 deposited with the CCDC.	2023-12-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.8850(12)
_cell_length_b                   24.8850(12)
_cell_length_c                   73.876(6)
_cell_measurement_reflns_used    9615
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      27.03
_cell_measurement_theta_min      2.59
_cell_volume                     45749(5)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.00
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_av_unetI/netI     0.0198
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       87
_diffrn_reflns_limit_l_min       -87
_diffrn_reflns_number            318236
_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         2.471
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.700
_exptl_absorpt_correction_T_max  0.9281
_exptl_absorpt_correction_T_min  0.8192
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0633 before and 0.0526 after correction.
The Ratio of minimum to maximum transmission is 0.8827.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_description       cube
_exptl_crystal_F_000             21008
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.815
_refine_diff_density_min         -1.005
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     701
_refine_ls_number_reflns         20267
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0963
_refine_ls_R_factor_gt           0.0846
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0724P)^2^+1162.9983P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2303
_refine_ls_wR_factor_ref         0.2375
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17396
_reflns_number_total             20267
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03460g2.cif
_cod_data_source_block           (l4ni3)8_sq
_cod_depositor_comments
'Adding full bibliography for 7714805--7714810.cif.'
_cod_original_cell_volume        45749(6)
_cod_database_code               7714810
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.727
_shelx_estimated_absorpt_t_min   0.542
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H31A-H30B
 2.2 with sigma of 0.01
 H9B-H8A
 2.2 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C30) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C8) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4.a Ternary CH refined with riding coordinates:
 O6(H6), O16(H16)
4.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C31(H31A,H31B), C32(H32A,H32B),
 C33(H33A,H33B)
4.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C24(H24), C25(H25), C27(H27)
4.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C22(H22A,
 H22B,H22C), C30(H30A,H30B,H30C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C),
 C36(H36A,H36B,H36C), C38(H38A,H38B,H38C), C40(H40A,H40B,H40C), C42(H42A,H42B,
 H42C), C44(H44A,H44B,H44C)
;
_shelx_res_checksum              7888
_shelx_fab_checksum              80528
_platon_squeeze_special_details
;
A solvent mask was calculated and 9710 electrons were 
found in a volume of 28336\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
[14.5 CH2Cl2] per Asymmetric Unit 
which account for 9744 electrons 
per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'