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_7718738
_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         'C24 H36 B9 Cl N2 O2 Zn, C H Cl3, 2(C6 H16 N)'
_chemical_formula_sum            'C37 H69 B9 Cl4 N4 O2 Zn'
_chemical_formula_weight         906.42
_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
_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                103.925(12)
_cell_angle_beta                 99.199(12)
_cell_angle_gamma                97.975(12)
_cell_formula_units_Z            2
_cell_length_a                   10.390(6)
_cell_length_b                   12.226(7)
_cell_length_c                   22.240(13)
_cell_measurement_reflns_used    3782
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      20.581
_cell_measurement_theta_min      2.225
_cell_volume                     2660(3)
_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  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.893
_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  0.0744
_diffrn_reflns_av_unetI/netI     0.1264
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.893
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            34030
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.893
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.505
_diffrn_reflns_theta_min         1.746
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.695
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5891
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1267 before and 0.0588 after correction.
The Ratio of minimum to maximum transmission is 0.7896.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.132
_exptl_crystal_description       block
_exptl_crystal_F_000             956
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.434
_refine_diff_density_min         -0.547
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.960
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         14512
_refine_ls_number_restraints     524
_refine_ls_restrained_S_all      0.947
_refine_ls_R_factor_all          0.1441
_refine_ls_R_factor_gt           0.0642
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0673P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1417
_refine_ls_wR_factor_ref         0.1737
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7136
_reflns_number_total             14512
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00946d2.cif
_cod_data_source_block           complex3b
_cod_depositor_comments
'Adding full bibliography for 7718736--7718738.cif.'
_cod_database_code               7718738
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.921
_shelx_estimated_absorpt_t_min   0.903
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N3-H3B
 1 with sigma of 0.02
 B8-H8A
 1.2 with sigma of 0.02
 B9-H8A
 1.2 with sigma of 0.02
 N4-H4A
 1 with sigma of 0.02
3. Rigid bond restraints
 C25, C26
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C25 \\sim C26: within 2A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 2A
5. 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
6.a Ternary CH refined with riding coordinates:
 C37(H37)
6.b Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C27(H27A,H27B), C29(H29A,H29B), C31(H31A,H31B), C33(H33A,
 H33B), C35(H35A,H35B)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C7(H7), C14(H14), C16(H16), C17(H17), C18(H18)
6.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C28(H28A,
 H28B,H28C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C),
 C36(H36A,H36B,H36C)
6.e Boron cage BH refined with riding coordinates:
 B1(H1), B2(H2), B3(H3A), B4(H4), B5(H5A), B6(H6A)
;
_shelx_res_checksum              89636
_shelx_hkl_checksum              93435
_shelx_fab_checksum              49115
_olex2_submission_special_instructions 'No special instructions were received'