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_7714809
_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         'C178.5 H255 N16 Ni24 O85, 12[C6H14], 0.5[H2O]'
_chemical_formula_sum            'C250.5 H424 N16 Ni24 O85.5'
_chemical_formula_weight         6437.07
_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             2023-12-07
_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                 90.278(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   33.427(5)
_cell_length_b                   26.526(4)
_cell_length_c                   35.933(5)
_cell_measurement_reflns_used    9923
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      23.473
_cell_measurement_theta_min      2.640
_cell_volume                     31861(8)
_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)'
_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  0.1589
_diffrn_reflns_av_unetI/netI     0.1325
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            347437
_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         2.288
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.455
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5568
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1005 before and 0.0872 after correction.
The Ratio of minimum to maximum transmission is 0.7469.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_description       block
_exptl_crystal_F_000             13580
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.353
_refine_diff_density_min         -0.757
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2848
_refine_ls_number_reflns         55965
_refine_ls_number_restraints     949
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.1883
_refine_ls_R_factor_gt           0.1080
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3204
_refine_ls_wR_factor_ref         0.3670
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25684
_reflns_number_total             55965
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03460g2.cif
_cod_data_source_block           (l6ni3)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        'C250.50 H424 N16 Ni24 O85.50'
_cod_database_code               7714809
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.905
_shelx_estimated_absorpt_t_min   0.669
_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
 C37-C34
 1.55 with sigma of 0.01
 C175-C174
 1.45 with sigma of 0.01
 N15-C175
 1.35 with sigma of 0.01
 C176-C175
 1.5 with sigma of 0.01
 H15G-H15F
 2.2 with sigma of 0.01
 H37B-H39B
 2.2 with sigma of 0.01
 H15E-H149
 2.2 with sigma of 0.01
 H15Q-H66
 2.2 with sigma of 0.01
 N13-C153
 1.45 with sigma of 0.01
 H15D-H15G
 2.2 with sigma of 0.01
 H87A-H36
 2.2 with sigma of 0.01
 H53-H56B
 2.2 with sigma of 0.01
 C31-C32
 1.5 with sigma of 0.01
 H57A-H56C
 2.2 with sigma of 0.01
 C57-N5
 1.45 with sigma of 0.01
 H57A-H56A
 2.2 with sigma of 0.01
 C5A-C6A
 2.2 with sigma of 0.01
 C181-N16 = N16-C183
 1.45 with sigma of 0.02
 C6A-N16 = N16-C4A
 1.45 with sigma of 0.02
 C181-C178 = C178-C179
 1.5 with sigma of 0.02
 C176-C175 = C175-N15
 1.4 with sigma of 0.02
 H46-H11D
 2.3 with sigma of 0.01
 H11H-H11D
 2.3 with sigma of 0.01
 H10K-H11G
 2.3 with sigma of 0.01
 H10I-H11G
 2.3 with sigma of 0.01
 C181-C183
 2.368 with sigma of 0.04
 C6A-C4A
 2.368 with sigma of 0.04
 C181-C179
 2.45 with sigma of 0.04
 C176-N15
 2.425 with sigma of 0.04
 N12-C2A \\sim N12-C134
 with sigma of 0.02
 N12-C133 \\sim N12-C1A
 with sigma of 0.02
 N12-C135 \\sim N12-C3A
 with sigma of 0.02
 C133-C130 \\sim C1A-C130
 with sigma of 0.02
 C1A-C132 \\sim C133-C131
 with sigma of 0.02
 N16-C5A \\sim N16-C182
 with sigma of 0.02
 N16-C183 \\sim N16-C6A
 with sigma of 0.02
 N16-C181 \\sim N16-C4A
 with sigma of 0.02
 C181-C178 \\sim C4A-C178
 with sigma of 0.02
 C181-C180 \\sim C4A-C179
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1 \\sim C1A \\sim C2 \\sim C2A \\sim C3 \\sim C3A \\sim C4 \\sim C4A \\sim C5
\\sim C5A \\sim C6 \\sim C6A \\sim C7 \\sim C8 \\sim C9 \\sim C10 \\sim C11
\\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim C19
\\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C27 \\sim C26 \\sim C25
\\sim C30 \\sim C29 \\sim C28 \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35
\\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41 \\sim C42 \\sim C43 \\sim C44
\\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49 \\sim C50 \\sim C51 \\sim C52
\\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57 \\sim C58 \\sim C59 \\sim C60
\\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65 \\sim C66 \\sim C67 \\sim C68
\\sim C69 \\sim C70 \\sim C71 \\sim C72 \\sim C74 \\sim C73 \\sim C78 \\sim C77
\\sim C76 \\sim C75 \\sim C79 \\sim C80 \\sim C81 \\sim C82 \\sim C85 \\sim C86
\\sim C87 \\sim C89 \\sim C90 \\sim C91 \\sim C92 \\sim C93 \\sim C94 \\sim C95
\\sim C96 \\sim C97 \\sim C98 \\sim C99 \\sim C100 \\sim C101 \\sim C102 \\sim
C103 \\sim C104 \\sim C105 \\sim C106 \\sim C107 \\sim C108 \\sim C109 \\sim
C110 \\sim C111 \\sim C113 \\sim C114 \\sim C115 \\sim C116 \\sim C117 \\sim
C118 \\sim C119 \\sim C120 \\sim C126 \\sim C121 \\sim C122 \\sim C123 \\sim
C124 \\sim C125 \\sim C127 \\sim C128 \\sim C129 \\sim C130 \\sim C131 \\sim
C132 \\sim C133 \\sim C134 \\sim C135 \\sim C137 \\sim C138 \\sim C139 \\sim
C140 \\sim C141 \\sim C142 \\sim C143 \\sim C144 \\sim C145 \\sim C146 \\sim
C147 \\sim C148 \\sim C149 \\sim C150 \\sim C151 \\sim C152 \\sim C153 \\sim
C154 \\sim C155 \\sim C156 \\sim C157 \\sim C158 \\sim C159 \\sim C161 \\sim
C162 \\sim C163 \\sim C164 \\sim C165 \\sim C166 \\sim C167 \\sim C168 \\sim
C174 \\sim C169 \\sim C170 \\sim C171 \\sim C172 \\sim C173 \\sim C175 \\sim
C176 \\sim C177 \\sim C178 \\sim C179 \\sim C180 \\sim C181 \\sim C182 \\sim
C183 \\sim C185 \\sim C186 \\sim C187 \\sim C188 \\sim C189 \\sim C190 \\sim
C191 \\sim C192: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(C181) \\sim Ueq, Uanis(C4A) \\sim Ueq, Uanis(C5A) \\sim Ueq, Uanis(C182)
\\sim Ueq, Uanis(C6A) \\sim Ueq, Uanis(C183) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O82) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O86) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C39) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C158) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O84) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C176) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C133) = Uanis(C1A)
Uanis(C135) = Uanis(C3A)
Uanis(C134) = Uanis(C2A)
Uanis(C182) = Uanis(C5A)
Uanis(C183) = Uanis(C6A)
Uanis(C181) = Uanis(C4A)
4. Others
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(C2A)=Sof(C3A)=1-FVAR(1)
 Sof(C133)=Sof(H13I)=Sof(H13J)=Sof(C134)=Sof(C135)=FVAR(1)
 Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(C5A)=Sof(C6A)=1-FVAR(2)
 Sof(C181)=Sof(H18G)=Sof(H18H)=Sof(C182)=Sof(C183)=FVAR(2)
 Fixed Sof: O82(0.5) O83(0.5) O84(0.5) O86(0.5) O87(0.5) O88(0.5) C33(0.5)
 H33A(0.5) H33B(0.5) C34(0.5) H34(0.5) C35(0.5) H35A(0.5) H35B(0.5) H35C(0.5)
 C37(0.5) H37A(0.5) H37B(0.5) C38(0.5) H38A(0.5) H38B(0.5) H38C(0.5) C39(0.5)
 H39A(0.5) H39B(0.5) H39C(0.5) C40(0.5) H40A(0.5) H40B(0.5) H40C(0.5) C64(0.5)
 H64A(0.5) H64B(0.5) H64C(0.5) C86(0.5) H86A(0.5) H86B(0.5) H86C(0.5) C87(0.5)
 H87A(0.5) H87B(0.5) H87C(0.5) C176(0.5)
5.a Ternary CH refined with riding coordinates:
 O6(H6), O16(H16), O26(H26), O36(H36), O46(H46), O56(H56), O66(H66), O76(H76),
 C34(H34)
5.b Secondary CH2 refined with riding coordinates:
 C1A(H1AA,H1AB), C4A(H4AA,H4AB), C9(H9A,H9B), C13(H13A,H13B), C33(H33A,H33B),
 C37(H37A,H37B), C57(H57A,H57B), C61(H61A,H61B), C81(H81A,H81B), C82(H82A,H82B),
  C85(H85A,H85B), C105(H10D,H10E), C109(H10L,H10M), C129(H12J,H12K), C133(H13I,
 H13J), C153(H15G,H15H), C157(H15O,H15P), C177(H17A,H17B), C181(H18G,H18H)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C27(H27), C26(H26A), C29(H29), C50(H50), C51(H51),
 C53(H53), C74(H74), C77(H77), C75(H75), C98(H98), C99(H99), C101(H101),
 C122(H122), C123(H123), C125(H125), C146(H146), C147(H147), C149(H149),
 C170(H170), C171(H171), C173(H173)
5.d Fitted hexagon refined as free rotating group:
 C27(C26,C25,C30,C29,C28), C74(C73,C78,C77,C76,C75), C126(C121,C122,C123,C124,
 C125), C174(C169,C170,C171,C172,C173)
5.e Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,
 H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C20(H20A,
 H20B,H20C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C32(H32A,H32B,H32C),
 C35(H35A,H35B,H35C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,
 H40C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C), C46(H46A,H46B,H46C), C48(H48A,
 H48B,H48C), C56(H56A,H56B,H56C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C),
 C62(H62A,H62B,H62C), C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C66(H66A,H66B,
 H66C), C68(H68A,H68B,H68C), C70(H70A,H70B,H70C), C72(H72A,H72B,H72C), C80(H80A,
 H80B,H80C), C86(H86A,H86B,H86C), C87(H87A,H87B,H87C), C90(H90A,H90B,H90C),
 C92(H92A,H92B,H92C), C94(H94A,H94B,H94C), C96(H96A,H96B,H96C), C104(H10A,H10B,
 H10C), C107(H10F,H10G,H10H), C108(H10I,H10J,H10K), C110(H11D,H11E,H11F),
 C111(H11G,H11H,H11I), C114(H11J,H11K,H11L), C116(H11M,H11N,H11O), C118(H11P,
 H11Q,H11R), C120(H12D,H12E,H12F), C128(H12G,H12H,H12I), C131(H13C,H13D,H13E),
 C132(H13F,H13G,H13H), C138(H13K,H13L,H13M), C140(H14D,H14E,H14F), C142(H14G,
 H14H,H14I), C144(H14J,H14K,H14L), C152(H15D,H15E,H15F), C155(H15I,H15J,H15K),
 C156(H15L,H15M,H15N), C158(H15Q,H15R,H15S), C159(H15T,H15U,H15V), C162(H16D,
 H16E,H16F), C164(H16G,H16H,H16I), C166(H16J,H16K,H16L), C168(H16M,H16N,H16O),
 C179(H17C,H17D,H17E), C180(H18D,H18E,H18F), C186(H18I,H18J,H18K), C188(H18L,
 H18M,H18N), C190(H19A,H19B,H19C), C192(H19D,H19E,H19F)
;
_shelx_res_checksum              93755
_shelx_fab_checksum              63793
_platon_squeeze_special_details
;
A solvent mask was calculated and 2381 electrons were 
found in a volume of 13509\%A^3^ in 3 voids per unit cell. 
This is consistent with the presence of 
12[C6H14], 0.5[H2O] per Asymmetric Unit 
which account for 2420 electrons 
per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'