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_7714807
_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
'C184 H280 Br8 N16 Ni24 O80, 0.5[H2O], 10[CH2Cl2], 9[C6H14]'
_chemical_formula_sum            'C248 H427 Br8 Cl20 N16 Ni24 O80.5'
_chemical_formula_weight         7678.35
_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             2023-12-04
_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                 90.081(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   33.816(4)
_cell_length_b                   26.775(4)
_cell_length_c                   36.089(5)
_cell_measurement_reflns_used    9757
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      25.28
_cell_measurement_theta_min      2.56
_cell_volume                     32676(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 0.996
_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  0.1287
_diffrn_reflns_av_unetI/netI     0.1290
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_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            295879
_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         2.426
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.562
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.4691
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1235 before and 0.0960 after correction.
The Ratio of minimum to maximum transmission is 0.6292.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_description       cube
_exptl_crystal_F_000             15852
_exptl_crystal_size_max          0.64
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.219
_refine_diff_density_min         -1.139
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2938
_refine_ls_number_reflns         57357
_refine_ls_number_restraints     2121
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1667
_refine_ls_R_factor_gt           0.0875
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1669P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2525
_refine_ls_wR_factor_ref         0.2980
_reflns_Friedel_coverage         0.000
_reflns_number_gt                26439
_reflns_number_total             57357
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03460g2.cif
_cod_data_source_block           (l5ni3)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        'C248 H427 Br8 Cl20 N16 Ni24 O80.50'
_cod_database_code               7714807
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.590
_shelx_estimated_absorpt_t_min   0.291
_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
 N12-C128 = C128-C125
 1.5 with sigma of 0.02
 C129-N12 = N12-C130
 1.47 with sigma of 0.02
 C130-N12 = N12-C128
 1.47 with sigma of 0.02
 H35A-H34C
 2.5 with sigma of 0.01
 C129-N12 = N12-C128
 1.47 with sigma of 0.02
 N16-C174 = C174-C171
 1.52 with sigma of 0.02
 C175-N16 = N16-C174
 1.47 with sigma of 0.02
 C130-N12 = N12-C1E
 1.46 with sigma of 0.02
 C1D-C125
 1.5 with sigma of 0.01
 H8A-H9B
 2.2 with sigma of 0.01
 H31A-H32A
 2.2 with sigma of 0.01
 H77C-H78A
 2.2 with sigma of 0.01
 H12Q-H13E
 2.2 with sigma of 0.01
 H83B-H84B
 2.2 with sigma of 0.01
 H10A-H10E
 2.2 with sigma of 0.01
 H82A-H83C
 2.2 with sigma of 0.01
 H36-H83A
 2.2 with sigma of 0.01
 H12Q-H56
 2.2 with sigma of 0.01
 H10B-H97
 2.2 with sigma of 0.01
 H12R-H13E
 2.2 with sigma of 0.01
 N12-C125
 2.45 with sigma of 0.04
 C129-C130
 2.401 with sigma of 0.04
 C130-C128
 2.401 with sigma of 0.04
 C129-C128
 2.401 with sigma of 0.04
 N16-C171
 2.483 with sigma of 0.04
 C175-C174
 2.401 with sigma of 0.04
 C130-C1E
 2.161 with sigma of 0.04
 C35A-C33 \\sim C35-C33
 with sigma of 0.02
 N4-C38 \\sim N4-C38A
 with sigma of 0.02
 N4-C37A \\sim N4-C37
 with sigma of 0.02
 N4-C36A \\sim N4-C36
 with sigma of 0.02
 C36A-C33 \\sim C36-C33
 with sigma of 0.02
 C1E-N12 \\sim N12-C128
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1 \\sim C1A \\sim C1AA \\sim C174 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6
\\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 C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30
\\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim C36 \\sim C36A \\sim C37 \\sim
C37A \\sim C38 \\sim C38A \\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 C73 \\sim C74 \\sim C75
\\sim C76 \\sim C77 \\sim C78 \\sim C79 \\sim C80 \\sim C81 \\sim C82 \\sim C83
\\sim C84 \\sim C85 \\sim C86 \\sim C87 \\sim C88 \\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 C112 \\sim C113
\\sim C114 \\sim C115 \\sim C116 \\sim C117 \\sim C118 \\sim C119 \\sim C120
\\sim C121 \\sim C122 \\sim C123 \\sim C124 \\sim C125 \\sim C126 \\sim C127
\\sim C1D \\sim C128 \\sim C1E \\sim C129 \\sim C130 \\sim C131 \\sim C132
\\sim C133 \\sim C134 \\sim C135 \\sim C136 \\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 C160
\\sim C161 \\sim C162 \\sim C163 \\sim C164 \\sim C165 \\sim C166 \\sim C167
\\sim C168 \\sim C169 \\sim C170 \\sim C171 \\sim C172 \\sim C173 \\sim C1B
\\sim C175 \\sim C176 \\sim C177 \\sim C178 \\sim C179 \\sim C180 \\sim C181
\\sim C182 \\sim C183 \\sim C184 \\sim C35 \\sim C35A: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C1) \\sim Ueq, Uanis(C1A) \\sim Ueq, Uanis(C1AA) \\sim Ueq, Uanis(C174)
\\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq,
Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim
Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq,
Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15)
\\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq,
Uanis(C19) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C22)
\\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C25) \\sim Ueq,
Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C29)
\\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C32) \\sim Ueq,
Uanis(C33) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C36A)
\\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C37A) \\sim Ueq, Uanis(C38) \\sim Ueq,
Uanis(C38A) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C41)
\\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C44) \\sim Ueq,
Uanis(C45) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C48)
\\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C51) \\sim Ueq,
Uanis(C52) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C55)
\\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C58) \\sim Ueq,
Uanis(C59) \\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C62)
\\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(C65) \\sim Ueq,
Uanis(C66) \\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(C69)
\\sim Ueq, Uanis(C70) \\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(C72) \\sim Ueq,
Uanis(C73) \\sim Ueq, Uanis(C74) \\sim Ueq, Uanis(C75) \\sim Ueq, Uanis(C76)
\\sim Ueq, Uanis(C77) \\sim Ueq, Uanis(C78) \\sim Ueq, Uanis(C79) \\sim Ueq,
Uanis(C80) \\sim Ueq, Uanis(C81) \\sim Ueq, Uanis(C82) \\sim Ueq, Uanis(C83)
\\sim Ueq, Uanis(C84) \\sim Ueq, Uanis(C85) \\sim Ueq, Uanis(C86) \\sim Ueq,
Uanis(C87) \\sim Ueq, Uanis(C88) \\sim Ueq, Uanis(C89) \\sim Ueq, Uanis(C90)
\\sim Ueq, Uanis(C91) \\sim Ueq, Uanis(C92) \\sim Ueq, Uanis(C93) \\sim Ueq,
Uanis(C94) \\sim Ueq, Uanis(C95) \\sim Ueq, Uanis(C96) \\sim Ueq, Uanis(C97)
\\sim Ueq, Uanis(C98) \\sim Ueq, Uanis(C99) \\sim Ueq, Uanis(C100) \\sim Ueq,
Uanis(C101) \\sim Ueq, Uanis(C102) \\sim Ueq, Uanis(C103) \\sim Ueq,
Uanis(C104) \\sim Ueq, Uanis(C105) \\sim Ueq, Uanis(C106) \\sim Ueq,
Uanis(C107) \\sim Ueq, Uanis(C108) \\sim Ueq, Uanis(C109) \\sim Ueq,
Uanis(C110) \\sim Ueq, Uanis(C111) \\sim Ueq, Uanis(C112) \\sim Ueq,
Uanis(C113) \\sim Ueq, Uanis(C114) \\sim Ueq, Uanis(C115) \\sim Ueq,
Uanis(C116) \\sim Ueq, Uanis(C117) \\sim Ueq, Uanis(C118) \\sim Ueq,
Uanis(C119) \\sim Ueq, Uanis(C120) \\sim Ueq, Uanis(C121) \\sim Ueq,
Uanis(C122) \\sim Ueq, Uanis(C123) \\sim Ueq, Uanis(C124) \\sim Ueq,
Uanis(C125) \\sim Ueq, Uanis(C126) \\sim Ueq, Uanis(C127) \\sim Ueq, Uanis(C1D)
\\sim Ueq, Uanis(C128) \\sim Ueq, Uanis(C1E) \\sim Ueq, Uanis(C129) \\sim Ueq,
Uanis(C130) \\sim Ueq, Uanis(C131) \\sim Ueq, Uanis(C132) \\sim Ueq,
Uanis(C133) \\sim Ueq, Uanis(C134) \\sim Ueq, Uanis(C135) \\sim Ueq,
Uanis(C136) \\sim Ueq, Uanis(C137) \\sim Ueq, Uanis(C138) \\sim Ueq,
Uanis(C139) \\sim Ueq, Uanis(C140) \\sim Ueq, Uanis(C141) \\sim Ueq,
Uanis(C142) \\sim Ueq, Uanis(C143) \\sim Ueq, Uanis(C144) \\sim Ueq,
Uanis(C145) \\sim Ueq, Uanis(C146) \\sim Ueq, Uanis(C147) \\sim Ueq,
Uanis(C148) \\sim Ueq, Uanis(C149) \\sim Ueq, Uanis(C150) \\sim Ueq,
Uanis(C151) \\sim Ueq, Uanis(C152) \\sim Ueq, Uanis(C153) \\sim Ueq,
Uanis(C154) \\sim Ueq, Uanis(C155) \\sim Ueq, Uanis(C156) \\sim Ueq,
Uanis(C157) \\sim Ueq, Uanis(C158) \\sim Ueq, Uanis(C159) \\sim Ueq,
Uanis(C160) \\sim Ueq, Uanis(C161) \\sim Ueq, Uanis(C162) \\sim Ueq,
Uanis(C163) \\sim Ueq, Uanis(C164) \\sim Ueq, Uanis(C165) \\sim Ueq,
Uanis(C166) \\sim Ueq, Uanis(C167) \\sim Ueq, Uanis(C168) \\sim Ueq,
Uanis(C169) \\sim Ueq, Uanis(C170) \\sim Ueq, Uanis(C171) \\sim Ueq,
Uanis(C172) \\sim Ueq, Uanis(C173) \\sim Ueq, Uanis(C1B) \\sim Ueq, Uanis(C175)
\\sim Ueq, Uanis(C176) \\sim Ueq, Uanis(C177) \\sim Ueq, Uanis(C178) \\sim Ueq,
Uanis(C179) \\sim Ueq, Uanis(C180) \\sim Ueq, Uanis(C181) \\sim Ueq,
Uanis(C182) \\sim Ueq, Uanis(C183) \\sim Ueq, Uanis(C184) \\sim Ueq, Uanis(C35)
\\sim Ueq, Uanis(C35A) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.01
Uanis(C35) \\sim Ueq, Uanis(C35A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C36) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C34)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C128) \\sim Ueq, Uanis(C125) \\sim Ueq, Uanis(C127) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
Uanis(C175) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(Br2) \\sim Ueq, Uanis(Br1) \\sim Ueq, Uanis(Br2A) \\sim Ueq, Uanis(Br1A)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C128) \\sim Ueq, Uanis(C1E) \\sim Ueq, Uanis(C127) \\sim Ueq, Uanis(C1D)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C35) = Uanis(C35A)
Uanis(C38) = Uanis(C38A)
Uanis(C37) = Uanis(C37A)
Uanis(C36) = Uanis(C36A)
Uanis(C176) = Uanis(C1A)
Uanis(C175) = Uanis(C1AA)
Uanis(C174) = Uanis(C174)
Uanis(Br1) = Uanis(Br1A)
Uanis(Br2) = Uanis(Br2A)
Uanis(C128) = Uanis(C1E)
4. Others
 Sof(C36A)=Sof(H36C)=Sof(H36D)=Sof(C37A)=Sof(H37D)=Sof(H37E)=Sof(H37F)=
 Sof(C38A)=Sof(H38D)=Sof(H38E)=Sof(H38F)=1-FVAR(1)
 Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(H37C)=Sof(C38)=
 Sof(H38A)=Sof(H38B)=Sof(H38C)=FVAR(1)
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C1AA)=Sof(H1AD)=Sof(H1AE)=
 Sof(H1AF)=Sof(C174)=Sof(H17A)=Sof(H17B)=1-FVAR(2)
 Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(C175)=Sof(H17N)=Sof(H17O)=Sof(H17P)=
 Sof(C176)=Sof(H17Q)=Sof(H17R)=Sof(H17S)=FVAR(2)
 Sof(Br1A)=Sof(Br2A)=1-FVAR(3)
 Sof(Br1)=Sof(Br2)=FVAR(3)
 Sof(C1D)=Sof(H1DA)=Sof(H1DB)=Sof(H1DC)=1-FVAR(4)
 Sof(C127)=Sof(H12L)=Sof(H12M)=Sof(H12N)=FVAR(4)
 Sof(C1E)=Sof(H1EA)=Sof(H1EB)=1-FVAR(5)
 Sof(C128)=Sof(H12O)=Sof(H12P)=FVAR(5)
 Sof(C35A)=Sof(H35D)=Sof(H35E)=Sof(H35F)=1-FVAR(6)
 Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=FVAR(6)
5.a Ternary CH refined with riding coordinates:
 O6(H6), O16(H16), O26(H26), O36(H36), O46(H46), O56(H56), O66(H66), O76(H76)
5.b Secondary CH2 refined with riding coordinates:
 C174(H17A,H17B), C9(H9A,H9B), C13(H13A,H13B), C32(H32A,H32B), C36(H36A,H36B),
 C36A(H36C,H36D), C55(H55A,H55B), C59(H59A,H59B), C78(H78A,H78B), C82(H82A,
 H82B), C101(H10D,H10E), C105(H10L,H10M), C124(H12G,H12H), C128(H12O,H12P),
 C1E(H1EA,H1EB), C147(H14G,H14H), C151(H15G,H15H), C170(H17F,H17G), C1B(H1BA,
 H1BB)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C25(H25), C26(H26A), C28(H28), C48(H48), C49(H49),
 C51(H51), C71(H71), C72(H72), C74(H74), C94(H94), C95(H95), C97(H97),
 C117(H117), C118(H118), C120(H120), C140(H140), C141(H141), C143(H143),
 C163(H163), C164(H164), C166(H166)
5.d Idealised Me refined as rotating group:
 C1A(H1AA,H1AB,H1AC), C1AA(H1AD,H1AE,H1AF), C8(H8A,H8B,H8C), C11(H11A,H11B,
 H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17C,
 H17D,H17E), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C),
 C31(H31A,H31B,H31C), C34(H34A,H34B,H34C), C37(H37A,H37B,H37C), C37A(H37D,H37E,
 H37F), C38(H38A,H38B,H38C), C38A(H38D,H38E,H38F), C40(H40A,H40B,H40C),
 C42(H42A,H42B,H42C), C44(H44A,H44B,H44C), C46(H46A,H46B,H46C), C54(H54A,H54B,
 H54C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C), C60(H60A,H60B,H60C), C61(H61A,
 H61B,H61C), C63(H63A,H63B,H63C), C65(H65A,H65B,H65C), C67(H67A,H67B,H67C),
 C69(H69A,H69B,H69C), C77(H77A,H77B,H77C), C80(H80A,H80B,H80C), C81(H81A,H81B,
 H81C), C83(H83A,H83B,H83C), C84(H84A,H84B,H84C), C86(H86A,H86B,H86C), C88(H88A,
 H88B,H88C), C90(H90A,H90B,H90C), C92(H92A,H92B,H92C), C100(H10A,H10B,H10C),
 C103(H10F,H10G,H10H), C104(H10I,H10J,H10K), C106(H10N,H10O,H10P), C107(H10Q,
 H10R,H10S), C109(H10T,H10U,H10V), C111(H11D,H11E,H11F), C113(H11G,H11H,H11I),
 C115(H11J,H11K,H11L), C123(H12D,H12E,H12F), C126(H12I,H12J,H12K), C127(H12L,
 H12M,H12N), C1D(H1DA,H1DB,H1DC), C129(H12Q,H12R,H12S), C130(H13C,H13D,H13E),
 C132(H13F,H13G,H13H), C134(H13I,H13J,H13K), C136(H13L,H13M,H13N), C138(H13O,
 H13P,H13Q), C146(H14D,H14E,H14F), C149(H14I,H14J,H14K), C150(H15D,H15E,H15F),
 C152(H15I,H15J,H15K), C153(H15L,H15M,H15N), C155(H15O,H15P,H15Q), C157(H15R,
 H15S,H15T), C159(H15U,H15V,H15W), C161(H16A,H16B,H16C), C169(H16D,H16E,H16F),
 C172(H17H,H17I,H17J), C173(H17K,H17L,H17M), C175(H17N,H17O,H17P), C176(H17Q,
 H17R,H17S), C178(H17T,H17U,H17V), C180(H18A,H18B,H18C), C182(H18D,H18E,H18F),
 C184(H18G,H18H,H18I), C35(H35A,H35B,H35C), C35A(H35D,H35E,H35F)
;
_shelx_res_checksum              30820
_shelx_fab_checksum              83719
_platon_squeeze_special_details
;
A solvent mask was calculated and 3481 electrons were 
found in a volume of 13905\%A^3^ in 4 voids per unit cell. 
This is consistent with the presence of 
0.1[H2O], 10[CH2Cl2],9[C6H14], 0.3[H2O], 0.1[H2O] per Asymmetric Unit 
which account for 3380 electrons 
per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'