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_7714808
_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
'C160 H232 F8 N16 Ni24 O80, 10[C6H14], 3[CH2Cl2], 0.5[H2O]'
_chemical_formula_sum            'C223 H379 Cl6 F8 N16 Ni24 O80.5'
_chemical_formula_weight         6346.14
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-11-10
_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                 93.397(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.8794(10)
_cell_length_b                   26.4236(10)
_cell_length_c                   43.2603(17)
_cell_measurement_reflns_used    9403
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      26.301
_cell_measurement_theta_min      2.686
_cell_volume                     28389.5(19)
_computing_cell_refinement       '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 0.997
_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  0.0607
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            342711
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.403
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.689
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5976
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0842 before and 0.0705 after correction.
The Ratio of minimum to maximum transmission is 0.8017.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_description       cube
_exptl_crystal_F_000             13276
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.28
_refine_diff_density_max         1.755
_refine_diff_density_min         -1.024
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2641
_refine_ls_number_reflns         49878
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.1216
_refine_ls_R_factor_gt           0.0832
_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^)+(0.0951P)^2^+342.2578P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2130
_refine_ls_wR_factor_ref         0.2430
_reflns_Friedel_coverage         0.000
_reflns_number_gt                34738
_reflns_number_total             49878
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03460g2.cif
_cod_data_source_block           (l2ni3)8_sq
_cod_depositor_comments
'Adding full bibliography for 7714805--7714810.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C223 H379 Cl6 F8 N16 Ni24 O80.50'
_cod_database_code               7714808
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.649
_shelx_estimated_absorpt_t_min   0.574
_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.a Ternary CH refined with riding coordinates:
 O6(H6), O16(H16), O26(H26), O36(H36), O46(H46), O56(H56), O66(H66), O76(H76)
2.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C28(H28A,H28B), C29(H29A,H29B),
 C30(H30A,H30B), C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B), C68(H68A,H68B),
  C69(H69A,H69B), C70(H70A,H70B), C88(H88A,H88B), C89(H89A,H89B), C90(H90A,
 H90B), C108(H10F,H10G), C109(H10H,H10I), C110(H11D,H11E), C128(H12G,H12H),
 C129(H12I,H12J), C130(H13A,H13B), C148(H14G,H14H), C149(H14I,H14J), C150(H15A,
 H15B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C7(H7), C22(H22), C23(H23), C25(H25), C27(H27),
 C42(H42), C43(H43), C45(H45), C47(H47), C62(H62), C63(H63), C65(H65), C67(H67),
  C82(H82), C83(H83), C85(H85), C87(H87), C102(H102), C103(H103), C105(H105),
 C107(H107), C122(H122), C123(H123), C125(H125), C127(H127), C142(H142),
 C143(H143), C145(H145), C147(H147)
2.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C16(H16A,H16B,
 H16C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C38(H38A,H38B,H38C),
 C40(H40A,H40B,H40C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C54(H54A,H54B,
 H54C), C56(H56A,H56B,H56C), C58(H58A,H58B,H58C), C60(H60A,H60B,H60C), C71(H71A,
 H71B,H71C), C72(H72A,H72B,H72C), C74(H74A,H74B,H74C), C76(H76A,H76B,H76C),
 C78(H78A,H78B,H78C), C80(H80A,H80B,H80C), C91(H91A,H91B,H91C), C92(H92A,H92B,
 H92C), C94(H94A,H94B,H94C), C96(H96A,H96B,H96C), C98(H98A,H98B,H98C),
 C100(H10C,H10D,H10E), C111(H11F,H11G,H11H), C112(H11I,H11J,H11K), C114(H11L,
 H11M,H11N), C116(H11O,H11P,H11Q), C118(H11R,H11S,H11T), C120(H12D,H12E,H12F),
 C131(H13C,H13D,H13E), C132(H13F,H13G,H13H), C134(H13I,H13J,H13K), C136(H13L,
 H13M,H13N), C138(H13O,H13P,H13Q), C140(H14D,H14E,H14F), C151(H15C,H15D,H15E),
 C152(H15F,H15G,H15H), C154(H15I,H15J,H15K), C156(H15L,H15M,H15N), C158(H15O,
 H15P,H15Q), C160(H16D,H16E,H16F)
;
_shelx_res_checksum              3060
_shelx_fab_checksum              97389
_platon_squeeze_special_details
;
A solvent mask was calculated and 2535 electrons were 
found in a volume of 12384\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
10[C6H14], 3[CH2Cl2], 0.5[H2O] per Asymmetric Unit 
which account for 2524 electrons 
per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'