Bifunctional organoboron–phosphonium catalysts for coupling reactions of CO2 and epoxides
Sengoden, Mani; Bhat, Gulzar A.; Darensbourg, Donald J.; RSC Advances 12 (2022) 32440–32447; doi:10.1039/D2RA06358A

data_7245827
_publ_section_title
;
 Bifunctional organoboron--phosphonium catalysts for coupling reactions of
 CO2 and epoxides
;
_journal_issue                   50
_journal_name_full               'RSC Advances'
_journal_page_first              32440
_journal_page_last               32447
_journal_paper_doi               10.1039/D2RA06358A
_journal_volume                  12
_journal_year                    2022
_chemical_formula_moiety         'C29 H35 B Cl P'
_chemical_formula_sum            'C29 H35 B Cl P'
_chemical_formula_weight         460.80
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-04-18
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-07-18 deposited with the CCDC.	2022-10-28 downloaded from the CCDC.
;
_cell_angle_alpha                87.7740(10)
_cell_angle_beta                 85.4210(10)
_cell_angle_gamma                89.4850(10)
_cell_formula_units_Z            4
_cell_length_a                   12.0911(3)
_cell_length_b                   13.1217(3)
_cell_length_c                   15.7545(4)
_cell_measurement_reflns_used    4812
_cell_measurement_temperature    110.00
_cell_measurement_theta_max      70.199
_cell_measurement_theta_min      4.444
_cell_volume                     2489.64(11)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      110.00
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Bruker Venture (PHOTON III)'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16280
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.193
_diffrn_reflns_theta_min         2.816
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.055
_exptl_absorpt_correction_T_max  0.384
_exptl_absorpt_correction_T_min  0.279
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0842 before and 0.0403 after correction.
 
For component 2:
 wR2(int) was 0.0850 before and 0.0413 after correction.
 The Ratio of minimum to maximum transmission is 0.73.

Final HKLF 4 output contains 66971 reflections, Rint = 0.0345
 (51792 with I > 3sig(I), Rint = 0.0334)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_description       block
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.102
_exptl_crystal_size_mid          0.067
_exptl_crystal_size_min          0.043
_refine_diff_density_max         0.482
_refine_diff_density_min         -0.266
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     578
_refine_ls_number_reflns         16280
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0331
_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^)+(0.0504P)^2^+0.5136P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0887
_refine_ls_wR_factor_ref         0.0910
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15035
_reflns_number_total             16280
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ra06358a3.cif
_cod_data_source_block           1
_cod_database_code               7245827
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.917
_shelx_estimated_absorpt_t_min   0.818
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5334(9)
 0.4666(9)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3.a Ternary CH refined with riding coordinates:
 C1(H1), C5(H5), C1B(H1B), C5B(H5B)
3.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B),
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C2B(H2BA,H2BB), C3B(H3BA,H3BB),
 C4B(H4BA,H4BB), C6B(H6BA,H6BB), C7B(H7BA,H7BB), C8B(H8BA,H8BB), C9B(H9BA,H9BB),
  C10B(H10C,H10D), C11B(H11C,H11D)
3.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C19(H19), C20(H20),
 C21(H21), C22(H22), C23(H23), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29),
  C13B(H13B), C14B(H14B), C15B(H15B), C16B(H16B), C17B(H17B), C19B(H19B),
 C20B(H20B), C21B(H21B), C22B(H22B), C23B(H23B), C25B(H25B), C26B(H26B),
 C27B(H27B), C28B(H28B), C29B(H29B)
;
_shelx_res_checksum              13558
_olex2_submission_special_instructions 'No special instructions were received'