Two approaches to phosphaniminocarbyne complexes.
Foglia, Lucas G.; Kirk, Ryan M.; Hill, Anthony F.; Dalton transactions (Cambridge, England : 2003) 55 (2026) 4057–4061; doi:10.1039/d6dt00303f

data_7720141
_publ_section_title
;
 Two approaches to phosphaniminocarbyne complexes.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4057
_journal_page_last               4061
_journal_paper_doi               10.1039/d6dt00303f
_journal_volume                  55
_journal_year                    2026
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C36 H37 B N7 O2 P W, C H2 Cl2'
_chemical_formula_sum            'C37 H39 B Cl2 N7 O2 P W'
_chemical_formula_weight         910.313
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Photo-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_symmetry_Int_Tables_number      7
_audit_block_doi                 10.5517/ccdc.csd.cc2q26vw
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2026-01-11 deposited with the CCDC.	2026-02-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.853(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.0998(2)
_cell_length_b                   16.9706(4)
_cell_length_c                   11.3101(3)
_cell_measurement_reflns_used    6357
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      78.5450
_cell_measurement_theta_min      2.5590
_cell_volume                     1928.44(8)
_computing_cell_refinement       'CrysAlisPro 1.171.44.119a (Rigaku OD, 2025)'
_computing_data_collection
'CrysAlisPro system (CCD 44.119a 64-bit (release 12-08-2025))'
_computing_data_reduction        'CrysAlisPro 1.171.44.119a (Rigaku OD, 2025)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9986
_diffrn_measured_fraction_theta_max 0.9570
_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   -113.00 -76.00   0.50    0.50    --  -45.79-142.00-164.00   74
  2  \w    -89.00 -45.00   0.50    0.50    --  -45.79 128.00  80.00   88
  3  \w   -118.00 -75.00   0.50    0.50    --  -45.79-128.00   6.00   86
  4  \w     48.00  79.00   0.50    0.50    --   45.79-128.00   6.00   62
  5  \w     49.00  74.00   0.50    0.50    --   45.79-142.00-164.00   50
  6  \w     93.00 135.00   0.50    3.00    --  110.00 128.00  80.00   84
  7  \w     88.00 135.00   0.50    3.00    --  110.00 142.00-108.00   94
  8  \w     83.00 125.00   0.50    3.00    --  110.00-142.00-164.00   84
  9  \w     75.00 109.00   0.50    3.00    --  110.00-128.00   6.00   68
 10  \w     -6.00  30.00   0.50    0.50    --  -45.79  19.00-180.00   72
 11  \w    -21.00  29.00   0.50    0.50    --  -45.79  38.00  30.00  100
 12  \w     -2.00  31.00   0.50    0.50    --  -45.79  19.00  90.00   66
 13  \w     -2.00  25.00   0.50    0.50    --  -45.79  19.00-120.00   54
 14  \w     37.00 106.00   0.50    3.00    --  110.00 -95.00   0.00  138
 15  \w     50.00  93.00   0.50    3.00    --  110.00 -61.00 150.00   86
 16  \w     81.00 106.00   0.50    3.00    --  110.00 -95.00  30.00   50
 17  \w     37.00  62.00   0.50    3.00    --  110.00 -95.00-150.00   50
 18  \w     37.00  72.00   0.50    3.00    --  110.00 -95.00  30.00   70
 19  \w     92.00 166.00   0.50    3.00    --  110.00  61.00 -30.00  148
 20  \w    102.00 171.00   0.50    3.00    --  110.00  45.00   0.00  138
 21  \w     43.00  73.00   0.50    3.00    --  110.00 -45.00  60.00   60
 22  \w     43.00  72.00   0.50    3.00    --  110.00 -45.00-180.00   58
 23  \w     41.00  73.00   0.50    3.00    --  110.00 -45.00 150.00   64
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0570119000
_diffrn_orient_matrix_UB_12      0.0660092000
_diffrn_orient_matrix_UB_13      0.0733570000
_diffrn_orient_matrix_UB_21      0.0529064000
_diffrn_orient_matrix_UB_22      0.0622039000
_diffrn_orient_matrix_UB_23      -0.0826046000
_diffrn_orient_matrix_UB_31      -0.1321685000
_diffrn_orient_matrix_UB_32      -0.0036197000
_diffrn_orient_matrix_UB_33      -0.0808701000
_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  0.0687
_diffrn_reflns_av_unetI/netI     0.0796
_diffrn_reflns_Laue_measured_fraction_full 0.9986
_diffrn_reflns_Laue_measured_fraction_max 0.9570
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11468
_diffrn_reflns_point_group_measured_fraction_full 0.6057
_diffrn_reflns_point_group_measured_fraction_max 0.5764
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         78.61
_diffrn_reflns_theta_min         2.60
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.557
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78953
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.44.119a (Rigaku Oxford Diffraction, 2025)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_description       irregular
_exptl_crystal_F_000             902.724
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.5300
_refine_diff_density_min         -0.7882
_refine_diff_density_rms         0.1260
_refine_ls_abs_structure_details
'Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.'
_refine_ls_abs_structure_Flack   -0.06(3)
_refine_ls_d_res_high            0.7864
_refine_ls_d_res_low             16.9706
_refine_ls_goodness_of_fit_ref   1.0420
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    65
_refine_ls_number_parameters     466
_refine_ls_number_reflns         4789
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.0420
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0595
_refine_ls_shift/su_max          -0.0068
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1053P)^2^+0.4464P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1483
_refine_ls_wR_factor_ref         0.1579
_reflns_Friedel_coverage         0.194
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              20
_reflns_limit_k_min              -20
_reflns_limit_l_max              14
_reflns_limit_l_min              -14
_reflns_number_gt                4226
_reflns_number_total             4789
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d6dt00303f2.cif
_cod_data_source_block           Compound_1
_cod_depositor_comments          'Adding full bibliography for 7720141.cif.'
_cod_original_cell_volume        1928.42(8)
_cod_database_code               7720141
_chemical_oxdiff_formula         C37H39BCl2N7O2PW
_cell_oxdiff_angle_alpha         89.997(2)
_cell_oxdiff_angle_beta          95.889(2)
_cell_oxdiff_angle_gamma         90.002(2)
_cell_oxdiff_length_a            10.1044(3)
_cell_oxdiff_length_b            16.9852(5)
_cell_oxdiff_length_c            11.3236(3)
_cell_oxdiff_measurement_reflns_used 6320
_cell_oxdiff_volume              1933.16(10)
_diffrn_oxdiff_digest_hkl
;
43da34b702afb3abb3d211511775cfbc8366a0
;
_diffrn_oxdiff_measurement_exp_name LGF-31-fk1.par
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, 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:
 B1(H1)
2.b Secondary CH2 refined with riding coordinates:
 C50(H50a,H50b)
2.c Aromatic/amide H refined with riding coordinates:
 C44(H44), C45(H45), C43(H43), C32(H32), C33(H33), C34(H34), C42(H42), C6(H6),
 C21(H21), C25(H25), C31(H31), C15(H15), C35(H35), C24(H24), C10(H10), C22(H22),
  C41(H41), C23(H23)
2.d Idealised Me refined as rotating group:
 C9(H9a,H9b,H9c), C12(H12a,H12b,H12c), C17(H17a,H17b,H17c), C13(H13a,H13b,
 H13c), C8(H8a,H8b,H8c), C4(H4a,H4b,H4c)
;
_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 1.299
_oxdiff_exptl_absorpt_empirical_full_min 0.809