A comparative study on <i>nido</i>- and <i>closo</i>-carborane supported zinc-salen catalysts for the ROCOP of epoxides and anhydrides.
Xue, Jin-Bian; Wang, Jia-Ni; Chen, Ke-Cheng; Cheng, Qian; Zhang, Jia-Ying; Xiao, Xu-Qiong; Dalton transactions (Cambridge, England : 2003) 54 (2025) 8400–8404; doi:10.1039/d5dt00946d

data_7718736
_publ_section_title
;
 A comparative study on <i>nido</i>- and <i>closo</i>-carborane supported
 zinc-salen catalysts for the ROCOP of epoxides and anhydrides.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8400
_journal_page_last               8404
_journal_paper_doi               10.1039/d5dt00946d
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety
'C32 H48 B18 N4 O8 Zn3, 4(C4 H8 O), 2(H2 O), 0.5[], 0.5[]'
_chemical_formula_sum            'C48 H84 B18 N4 O14 Zn3'
_chemical_formula_weight         1331.88
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_update_record
;
2025-04-17 deposited with the CCDC.	2025-05-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 128.651(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.280(3)
_cell_length_b                   13.2146(11)
_cell_length_c                   22.686(4)
_cell_measurement_reflns_used    3384
_cell_measurement_temperature    106.55
_cell_measurement_theta_max      23.77
_cell_measurement_theta_min      2.36
_cell_volume                     7323.4(16)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      106.55
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0810
_diffrn_reflns_av_unetI/netI     0.0950
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            29602
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.332
_diffrn_reflns_theta_min         1.667
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.029
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8710
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0642 before and 0.0556 after correction.
The Ratio of minimum to maximum transmission is 0.8710.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.208
_exptl_crystal_description       block
_exptl_crystal_F_000             2768
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.617
_refine_diff_density_min         -0.556
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         9077
_refine_ls_number_restraints     475
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.0974
_refine_ls_R_factor_gt           0.0501
_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^)+(0.0544P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1088
_refine_ls_wR_factor_ref         0.1264
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5741
_reflns_number_total             9077
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00946d2.cif
_cod_data_source_block           complex2a
_cod_depositor_comments
'Adding full bibliography for 7718736--7718738.cif.'
_cod_original_cell_volume        7323.3(14)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7718736
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.869
_shelx_estimated_absorpt_t_min   0.861
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 B9-H7B
 1.2 with sigma of 0.02
 B7-H7B
 1.2 with sigma of 0.02
 C18-C19 \\sim C18-C19A
 with sigma of 0.02
 C19-C20 \\sim C19A-C20
 with sigma of 0.02
 C22-C23 \\sim C22-C23A
 with sigma of 0.02
 C23-C24 \\sim C23A-C24
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(H18C)=Sof(H18D)=Sof(C19A)=Sof(H19C)=Sof(H19D)=1-FVAR(1)
 Sof(H18A)=Sof(H18B)=Sof(C19)=Sof(H19A)=Sof(H19B)=FVAR(1)
 Sof(H22C)=Sof(H22D)=Sof(H24C)=Sof(H24D)=Sof(C23A)=Sof(H23C)=Sof(H23D)=1-FVAR(2)
 Sof(H22A)=Sof(H22B)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H24A)=Sof(H24B)=FVAR(2)
5.a Free rotating group:
 O8(H8B,H8C)
5.b Rotating group:
 O3(H3A,H3B), O4(H4A,H4B)
5.c Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C18(H18A,H18B), C18(H18C,H18D), C19(H19A,H19B), C19A(H19C,
 H19D), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C22(H22C,H22D),
 C23(H23A,H23B), C24(H24A,H24B), C24(H24C,H24D), C23A(H23C,H23D)
5.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C12(H12), C13(H13),
 C14(H14), C15(H15)
5.e Boron cage BH refined with riding coordinates:
 B1(H1), B2(H2), B3(H3C), B4(H4), B5(H5A), B6(H6A), B7(H7A), B8(H8A), B9(H9)
;
_shelx_res_checksum              44441
_shelx_hkl_checksum              95278
_shelx_fab_checksum              31216
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'