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_7714806
_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
'C28 H40 F2 N4 Ni2 O7, 0.25[C6H14], 0.5[CH2Cl2], 0.25[H2O]'
_chemical_formula_sum            'C30 H45 Cl F2 N4 Ni2 O7.25'
_chemical_formula_weight         768.57
_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   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                107.870(2)
_cell_angle_beta                 107.105(3)
_cell_angle_gamma                99.032(2)
_cell_formula_units_Z            4
_cell_length_a                   12.1743(8)
_cell_length_b                   17.2045(12)
_cell_length_c                   18.9504(13)
_cell_measurement_reflns_used    9817
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.90
_cell_measurement_theta_min      3.11
_cell_volume                     3474.7(4)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_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)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.992
_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  0.0445
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            71803
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.243
_diffrn_reflns_theta_max         27.925
_diffrn_reflns_theta_min         3.106
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.221
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.630
_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    1.469
_exptl_crystal_description       cube
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.619
_refine_diff_density_min         -0.585
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     793
_refine_ls_number_reflns         16506
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0398
_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^)+(0.0565P)^2^+4.1748P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1071
_refine_ls_wR_factor_ref         0.1200
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13114
_reflns_number_total             16506
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03460g2.cif
_cod_data_source_block           (l2ni)2_sq
_cod_depositor_comments
'Adding full bibliography for 7714805--7714810.cif.'
_cod_database_code               7714806
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.877
_shelx_estimated_absorpt_t_min   0.482
_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.a Free rotating group:
 O5(H5A,H5B), O12(H12D,H12E)
2.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C20(H20A,H20B), C21(H21A,H21B),
 C22(H22A,H22B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C48(H48A,H48B),
  C49(H49A,H49B), C50(H50A,H50B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C7(H7), C14(H14), C15(H15), C17(H17), C19(H19),
 C30(H30), C31(H31), C33(H33), C35(H35), C42(H42), C43(H43), C45(H45), C47(H47)
2.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C39(H39A,H39B,H39C), C40(H40A,
 H40B,H40C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C54(H54A,H54B,H54C),
 C56(H56A,H56B,H56C)
;
_shelx_res_checksum              23557
_shelx_fab_checksum              67785
_platon_squeeze_special_details
;
A solvent mask was calculated and 145 electrons were 
found in a volume of 652\%A^3^ in 4 voids per unit cell. 
This is consistent with the presence of 
0.25[C6H14], 0.5[CH2Cl2], 0.25[H2O] per Asymmetric Unit 
which account for 144 electrons 
per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'