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_7160232
_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         'C42 H50 B N4 O P, 1.5[H2O]'
_chemical_formula_sum            'C42 H50 B N4 O P'
_chemical_formula_weight         668.64
_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_block_doi                 10.5517/ccdc.csd.cc2kv6l7
_audit_creation_date             2022-09-21
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-08-20 deposited with the CCDC.	2024-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                102.478(3)
_cell_angle_beta                 94.349(3)
_cell_angle_gamma                100.379(3)
_cell_formula_units_Z            2
_cell_length_a                   9.9881(3)
_cell_length_b                   13.2977(5)
_cell_length_c                   15.5488(6)
_cell_measurement_reflns_used    5911
_cell_measurement_temperature    193.15
_cell_measurement_theta_max      72.6020
_cell_measurement_theta_min      3.4810
_cell_volume                     1969.19(13)
_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 1.5 (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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      193.15
_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 0.998
_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     -6.00  34.00   0.50    5.00    --  -42.93  39.00  84.00   80
  2  \w     67.00 120.00   0.50    5.00    --   42.93  39.00  84.00  106
  3  \w     80.00 105.00   0.50   10.00    --   76.50  39.00  84.00   50
  4  \w     67.00  97.00   0.50   10.00    --   76.50 -39.00 -69.00   60
  5  \w     51.00  94.00   0.50   10.00    --   76.50 -99.00 -90.00   86
  6  \w     21.00  60.00   0.50    5.00    --   42.93  39.00  84.00   78
  7  \w    -34.00  46.00   0.50    5.00    --   42.93 -39.00 -69.00  160
  8  \w    110.00 149.00   0.50   10.00    --   76.50 125.00 -90.00   78
  9  \w    -60.00 -32.00   0.50   10.00    -- -106.00 125.00  30.00   56
 10  \w    -94.00 -17.00   0.50    5.00    --  -42.93 125.00 150.00  154
 11  \w    -99.00 -64.00   0.50   10.00    -- -106.00  77.00   0.00   70
 12  \w   -106.00 -80.00   0.50   10.00    -- -106.00 125.00  30.00   52
 13  \w   -112.00 -36.00   0.50   10.00    -- -106.00 125.00  60.00  152
 14  \w   -106.00 -35.00   0.50   10.00    -- -106.00  57.00  90.00  142
 15  \w   -114.00 -32.00   0.50   10.00    -- -106.00 125.00 -60.00  164
 16  \w   -114.00 -68.00   0.50   10.00    -- -106.00 125.00  90.00   92
 17  \w   -124.00 -29.00   0.50   10.00    -- -106.00  39.00  84.00  190
 18  \w   -108.00 -83.00   0.50   10.00    -- -106.00 -37.00  60.00   50
 19  \w   -123.00 -97.00   0.50   10.00    -- -106.00 -37.00   0.00   52
 20  \w   -134.00 -25.00   0.50   10.00    -- -106.00  19.00 -60.00  218
 21  \w   -107.00 -65.00   0.50   10.00    -- -106.00  77.00 -90.00   84
 22  \w   -117.00 -41.00   0.50   10.00    -- -106.00 125.00-120.00  152
 23  \w   -124.00 -33.00   0.50   10.00    -- -106.00  57.00 -90.00  182
 24  \w   -119.00 -23.00   0.50    5.00    --  -42.93 -39.00 -69.00  192
 25  \w   -115.00 -84.00   0.50    5.00    --  -42.93-125.00  90.00   62
 26  \w   -142.00 -85.00   0.50   10.00    -- -106.00 -57.00 120.00  114
 27  \w   -150.00-123.00   0.50   10.00    -- -106.00 -37.00  60.00   54
 28  \w   -174.00-149.00   0.50   10.00    -- -106.00 -57.00 120.00   50
 29  \w   -175.00 -86.00   0.50   10.00    -- -106.00 -99.00 150.00  178
 30  \w   -174.00-134.00   0.50   10.00    -- -106.00 -37.00   0.00   80
 31  \w   -163.00 -84.00   0.50   10.00    -- -106.00 -39.00 -69.00  158
 32  \w   -127.00 -34.00   0.50   10.00    -- -106.00  37.00 -90.00  186
 33  \w   -116.00 -72.00   0.50    5.00    --  -42.93-125.00 -90.00   88
;
_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      -0.1336442000
_diffrn_orient_matrix_UB_12      -0.0720355000
_diffrn_orient_matrix_UB_13      -0.0506388000
_diffrn_orient_matrix_UB_21      0.0680474000
_diffrn_orient_matrix_UB_22      -0.0961338000
_diffrn_orient_matrix_UB_23      -0.0066744000
_diffrn_orient_matrix_UB_31      -0.0495269000
_diffrn_orient_matrix_UB_32      -0.0156916000
_diffrn_orient_matrix_UB_33      0.0885308000
_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  0.0496
_diffrn_reflns_av_unetI/netI     0.0499
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22010
_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         68.248
_diffrn_reflns_theta_min         3.476
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.886
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88568
_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    1.128
_exptl_crystal_description       block
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.306
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         7179
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0500
_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^)+(0.0543P)^2^+0.6522P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1160
_refine_ls_wR_factor_ref         0.1236
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5767
_reflns_number_total             7179
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ob01565g2.cif
_cod_data_source_block           SN2024_compound_8b
_cod_depositor_comments
'Adding full bibliography for 7160230--7160235.cif.'
_cod_database_code               7160232
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C88 H108 B2 N6 O2 P2 '
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C33(H33), C36(H36)
2.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C18(H18), C10(H10), C29(H29), C7(H7), C31(H31), C13(H13), C4(H4),
 C30(H30), C11(H11), C5(H5), C12(H12), C6(H6), C24(H24), C26(H26), C22(H22),
 C25(H25), C23(H23)
2.c Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C), C34(H34A,H34B,H34C), C38(H38A,H38B,H38C), C37(H37A,H37B,
 H37C), C47(H47A,H47B,H47C), C46(H46A,H46B,H46C), C42(H42A,H42B,H42C), C45(H45A,
 H45B,H45C), C48(H48A,H48B,H48C), C44(H44A,H44B,H44C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 28 electrons were 
found in a volume of 177\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1.5[H2O] per Asymmetric Unit 
which account for 30 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              960
_shelx_fab_checksum              24578
_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 2.002
_oxdiff_exptl_absorpt_empirical_full_min 0.668