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_7245828
_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         '0.5(Br), C29 H37 B O P'
_chemical_formula_sum            'C29 H37 B Br0.5 O P'
_chemical_formula_weight         483.32
_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_creation_date             2022-04-08
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-07-18 deposited with the CCDC.	2022-10-28 downloaded from the CCDC.
;
_cell_angle_alpha                69.3050(10)
_cell_angle_beta                 66.3040(10)
_cell_angle_gamma                73.1480(10)
_cell_formula_units_Z            2
_cell_length_a                   10.0310(3)
_cell_length_b                   12.2645(4)
_cell_length_c                   12.4476(4)
_cell_measurement_reflns_used    9804
_cell_measurement_temperature    110.00
_cell_measurement_theta_max      30.530
_cell_measurement_theta_min      2.210
_cell_volume                     1292.08(7)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      110.00
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Quest (PHOTON III)'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            65447
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.566
_diffrn_reflns_theta_min         1.802
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.899
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6849
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1335 before and 0.0659 after correction.
The Ratio of minimum to maximum transmission is 0.9180.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_description       plate
_exptl_crystal_F_000             513
_exptl_crystal_size_max          0.207
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.027
_refine_diff_density_max         0.465
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         7896
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0349
_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^)+(0.0662P)^2^+0.1626P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1011
_refine_ls_wR_factor_ref         0.1055
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6607
_reflns_number_total             7896
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ra06358a3.cif
_cod_data_source_block           2
_cod_original_formula_sum        'C29 H37 B Br0.50 O P'
_cod_database_code               7245828
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.976
_shelx_estimated_absorpt_t_min   0.836
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: Br1(0.5)
3.a Riding coordinates:
 O1(H1A,H1B)
3.b Ternary CH refined with riding coordinates:
 C1(H1), C5(H5)
3.c 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)
3.d 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)
;
_shelx_res_checksum              25488
_olex2_submission_special_instructions 'No special instructions were received'