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_7160234
_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         'C43 H52 B N4 O3 P S, C H2 Cl2'
_chemical_formula_sum            'C44 H54 B Cl2 N4 O3 P S'
_chemical_formula_weight         831.65
_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     iterative
_audit_block_doi                 10.5517/ccdc.csd.cc2kv6j5
_audit_creation_date             2023-03-17
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-08-20 deposited with the CCDC.	2024-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.1494(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.24486(14)
_cell_length_b                   19.6073(3)
_cell_length_c                   24.3636(4)
_cell_measurement_reflns_used    17683
_cell_measurement_temperature    123.15
_cell_measurement_theta_max      76.7910
_cell_measurement_theta_min      3.6430
_cell_volume                     4409.64(12)
_computing_cell_refinement       'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/4 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      123.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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     77.00 156.00   0.50    1.00    --   96.50  32.00 173.00  158
  2  \w     55.00 122.00   0.50    0.20    --   43.05  32.00 173.00  134
  3  \w    114.00 140.00   0.50    1.00    --   96.50   0.00  90.00   52
  4  \w     71.00  97.00   0.50    1.00    --   96.50   0.00  90.00   52
  5  \w     24.00  64.00   0.50    1.00    --   96.50   0.00  90.00   80
  6  \w     22.00  49.00   0.50    1.00    --   96.50 -61.00 -90.00   54
  7  \w    -36.00   4.00   0.50    0.20    --   43.05 -19.00-150.00   80
  8  \w    -33.00  20.00   0.50    0.20    --   43.05 -37.00 -90.00  106
  9  \w    -34.00  -9.00   0.50    0.20    --   43.05 -32.00  14.00   50
 10  \w     22.00  49.00   0.50    1.00    --   96.50 -61.00 -60.00   54
 11  \w     77.00 106.00   0.50    1.00    --   96.50 -94.00 -90.00   58
 12  \w     36.00  66.00   0.50    1.00    --   96.50 -94.00 -90.00   60
 13  \w     74.00 100.00   0.50    1.00    --   96.50 -94.00  30.00   52
 14  \w     40.00  67.00   0.50    1.00    --   96.50 -94.00  30.00   54
 15  \w   -108.00 -36.00   0.50    0.20    --  -43.05 -32.00  14.00  144
 16  \w    -83.00 -38.00   0.50    1.00    -- -111.75  61.00 150.00   90
 17  \w   -124.00 -38.00   0.50    1.00    -- -111.75  77.00  30.00  172
 18  \w    -81.00 -37.00   0.50    1.00    -- -111.75  61.00  30.00   88
 19  \w    -79.00 -52.00   0.50    1.00    -- -111.75  61.00 -30.00   54
 20  \w    -72.00 -38.00   0.50    1.00    -- -111.75  45.00  30.00   68
 21  \w    -93.00 -40.00   0.50    1.00    -- -111.75  61.00 120.00  106
 22  \w    -72.00 -41.00   0.50    1.00    -- -111.75  45.00 120.00   62
 23  \w   -131.00 -88.00   0.50    1.00    -- -111.75 -32.00  14.00   86
 24  \w    -58.00  17.00   0.50    0.20    --  -43.05  32.00 173.00  150
 25  \w    -59.00 -32.00   0.50    1.00    -- -111.75  32.00 173.00   54
 26  \w    -66.00 -41.00   0.50    1.00    -- -111.75  45.00   0.00   50
 27  \w    -72.00 -37.00   0.50    1.00    -- -111.75  61.00 -60.00   70
 28  \w    -89.00 -38.00   0.50    1.00    -- -111.75  61.00-180.00  102
;
_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      0.0571786000
_diffrn_orient_matrix_UB_12      0.0022283000
_diffrn_orient_matrix_UB_13      -0.0581749000
_diffrn_orient_matrix_UB_21      -0.1418028000
_diffrn_orient_matrix_UB_22      -0.0327622000
_diffrn_orient_matrix_UB_23      -0.0233717000
_diffrn_orient_matrix_UB_31      -0.0667616000
_diffrn_orient_matrix_UB_32      0.0714201000
_diffrn_orient_matrix_UB_33      -0.0088805000
_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  0.0488
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            28396
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.251
_diffrn_reflns_theta_min         3.634
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.446
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61506
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.81a (Rigaku Oxford Diffraction, 2023)
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    1.253
_exptl_crystal_description       block
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.407
_refine_diff_density_min         -0.449
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     516
_refine_ls_number_reflns         8046
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0409
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1275
_refine_ls_wR_factor_ref         0.1318
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7360
_reflns_number_total             8046
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ob01565g2.cif
_cod_data_source_block           SN2024_compound_6a
_cod_depositor_comments
'Adding full bibliography for 7160230--7160235.cif.'
_cod_original_cell_volume        4409.64(11)
_cod_database_code               7160234
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C43 H52 B1 N4 O3 P1 S1'
_shelx_estimated_absorpt_t_max   0.792
_shelx_estimated_absorpt_t_min   0.527
_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:
 C20(H20), C17(H17)
2.b Secondary CH2 refined with riding coordinates:
 C55(H55A,H55B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C15(H15), C26(H26), C24(H24), C3(H3), C32(H32), C48(H48), C33(H33),
 C31(H31), C25(H25), C27(H27), C14(H14), C30(H30), C13(H13), C52(H52), C51(H51),
  C49(H49)
2.d Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C44(H44A,H44B,H44C), C46(H46A,H46B,H46C), C22(H22A,H22B,
 H22C), C21(H21A,H21B,H21C), C19(H19A,H19B,H19C), C18(H18A,H18B,H18C), C41(H41A,
 H41B,H41C), C53(H53A,H53B,H53C), C42(H42A,H42B,H42C), C45(H45A,H45B,H45C)
;
_shelx_res_checksum              56763
_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 1.562
_oxdiff_exptl_absorpt_empirical_full_min 0.627