Transformation of CO<sub>2</sub> and isocyanates mediated by <i>N</i>-borane-substituted cyclic phosphine imides (BCPIs) <i>via</i> λ<sup>5</sup>-oxazaphosphetanes.
Nagai, Shun; Ogoshi, Sensuke; Hoshimoto, Yoichi; Organic & biomolecular chemistry 23 (2024) 202–206; doi:10.1039/d4ob01565g

data_7160233
_publ_section_title
;
 Transformation of CO<sub>2</sub> and isocyanates mediated by
 <i>N</i>-borane-substituted cyclic phosphine imides (BCPIs) <i>via</i>
 &#x3bb;<sup>5</sup>-oxazaphosphetanes.
;
_journal_issue                   1
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              202
_journal_page_last               206
_journal_paper_doi               10.1039/d4ob01565g
_journal_volume                  23
_journal_year                    2024
_chemical_formula_moiety         'C36 H45 B N3 O2 P, C H2 Cl2'
_chemical_formula_sum            'C37 H47 B Cl2 N3 O2 P'
_chemical_formula_weight         678.45
_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
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2f6qt6
_audit_creation_date             2021-12-17
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-02-09 deposited with the CCDC.	2024-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.512(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.6693(3)
_cell_length_b                   19.5252(3)
_cell_length_c                   16.0002(4)
_cell_measurement_reflns_used    9489
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      75.8490
_cell_measurement_theta_min      3.6860
_cell_volume                     3774.54(15)
_computing_cell_refinement       'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     56.00 123.00   0.50    2.96    --   49.96  31.00-140.00  134
  2  \w     74.00  99.00   0.50    2.96    --   66.50  31.00-140.00   50
  3  \w     77.00 121.00   0.50    2.96    --   49.96 125.00-120.00   88
  4  \w      5.00  45.00   0.50    2.96    --   66.50 -31.00  59.00   80
  5  \w     -5.00  79.00   0.50    2.96    --   66.50 -57.00   0.00  168
  6  \w    -19.00  11.00   0.50    2.96    --   49.96 -31.00  59.00   60
  7  \w    -21.00  58.00   0.50    2.96    --   49.96 -37.00 -60.00  158
  8  \w    -45.00  20.00   0.50    2.96    --  -53.21  31.00-140.00  130
  9  \w    -89.00 -51.00   0.50    2.96    --  -53.21 -31.00  59.00   76
 10  \w    -98.00 -53.00   0.50    2.96    -- -105.75  37.00  30.00   90
 11  \w   -111.00 -52.00   0.50    2.96    -- -105.75  77.00  60.00  118
 12  \w   -112.00 -53.00   0.50    2.96    -- -105.75  19.00 -30.00  118
 13  \w   -110.00 -72.00   0.50    2.96    -- -105.75  31.00-140.00   76
 14  \w   -109.00 -32.00   0.50    2.96    -- -105.75  19.00-120.00  154
 15  \w   -112.00 -33.00   0.50    2.96    -- -105.75  19.00  30.00  158
 16  \w   -112.00 -34.00   0.50    2.96    -- -105.75  57.00  60.00  156
 17  \w   -161.00-136.00   0.50    2.96    -- -105.75 -31.00  59.00   50
 18  \w   -167.00-110.00   0.50    2.96    -- -105.75 -19.00   0.00  114
 19  \w   -175.00-122.00   0.50    2.96    -- -105.75 -19.00  90.00  106
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0186268000
_diffrn_orient_matrix_UB_12      -0.0242063000
_diffrn_orient_matrix_UB_13      -0.0861562000
_diffrn_orient_matrix_UB_21      0.1226971000
_diffrn_orient_matrix_UB_22      0.0209788000
_diffrn_orient_matrix_UB_23      0.0352584000
_diffrn_orient_matrix_UB_31      0.0294245000
_diffrn_orient_matrix_UB_32      -0.0720750000
_diffrn_orient_matrix_UB_33      0.0390802000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_unetI/netI     0.0441
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            28175
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.246
_diffrn_reflns_theta_min         3.676
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.213
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57179
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.43a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.194
_exptl_crystal_description       plate
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.014
_refine_diff_density_min         -0.669
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         6898
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_gt           0.0716
_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^)+(0.1048P)^2^+3.9052P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1888
_refine_ls_wR_factor_ref         0.1998
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5733
_reflns_number_total             6898
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ob01565g2.cif
_cod_data_source_block           compound_6a
_cod_depositor_comments
'Adding full bibliography for 7160230--7160235.cif.'
_cod_database_code               7160233
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C38 H50 B1 N3 O2 P1 Cl4'
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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 C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C38(H38), C41(H41)
2.b Secondary CH2 refined with riding coordinates:
 C44(H44A,H44B)
2.c Aromatic/amide H refined with riding coordinates:
 C19(H19), C18(H18), C7(H7), C13(H13), C4(H4), C6(H6), C34(H34), C36(H36),
 C12(H12), C10(H10), C11(H11), C5(H5), C35(H35)
2.d Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C24(H24A,H24B,H24C), C39(H39A,H39B,H39C), C26(H26A,H26B,
 H26C), C43(H43A,H43B,H43C), C25(H25A,H25B,H25C), C28(H28A,H28B,H28C), C29(H29A,
 H29B,H29C), C42(H42A,H42B,H42C), C30(H30A,H30B,H30C)
;
_shelx_res_checksum              33868
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.145
_oxdiff_exptl_absorpt_empirical_full_min 0.358