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_7714805
_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
'C32 H48 F2 N4 Ni2 O7, C1.59 H3.20 O1.60, C0.41 H0.81 O0.40'
_chemical_formula_sum            'C34 H52 F2 N4 Ni2 O9'
_chemical_formula_weight         816.21
_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
_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                 92.829(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.7730(5)
_cell_length_b                   12.7347(5)
_cell_length_c                   20.8529(8)
_cell_measurement_reflns_used    9871
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      27.849
_cell_measurement_theta_min      3.304
_cell_volume                     3918.3(3)
_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 0.997
_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  0.0486
_diffrn_reflns_av_unetI/netI     0.0275
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_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            61192
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.243
_diffrn_reflns_theta_max         26.500
_diffrn_reflns_theta_min         2.925
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.025
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6319
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0718 before and 0.0599 after correction.
The Ratio of minimum to maximum transmission is 0.8475.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_description       cube
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.335
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         8099
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0283
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0311P)^2^+2.1374P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0699
_refine_ls_wR_factor_ref         0.0740
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6975
_reflns_number_total             8099
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03460g2.cif
_cod_data_source_block           (l1ni)2
_cod_depositor_comments
'Adding full bibliography for 7714805--7714810.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7714805
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.980
_shelx_estimated_absorpt_t_min   0.679
_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) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C33) = Uanis(C33A)
Uanis(C34) = Uanis(C34A)
Uanis(O8) = Uanis(O8A)
Uanis(O9) = Uanis(O9A)
3. Others
 Sof(O8A)=Sof(C33A)=Sof(C34A)=Sof(H34D)=Sof(H34E)=Sof(H34F)=1-FVAR(1)
 Sof(O8)=Sof(C33)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=FVAR(1)
 Sof(O9A)=Sof(H9A)=1-FVAR(2)
 Sof(O9)=Sof(H9)=FVAR(2)
4.a Free rotating group:
 O5(H5A,H5B)
4.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C12(H12A,H12B), C22(H22A,H22B), C26(H26A,H26B)
4.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C7(H7), C16(H16), C17(H17), C19(H19), C21(H21)
4.d Tetrahedral OH refined with riding coordinates:
 O9(H9), O9A(H9A)
4.e Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C28(H28A,
 H28B,H28C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C),
 C34A(H34D,H34E,H34F)
;
_shelx_res_checksum              30866
_olex2_submission_special_instructions 'No special instructions were received'