Phosphaisonitrile umpolung - synthesis and reactivity of chloro aminophosphino carbynes.
Colebatch, Annie L.; Frogley, Benjamin J.; Hill, Anthony F.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 10628–10641; doi:10.1039/c9dt01838g

data_1551232
_publ_section_title
;
 Phosphaisonitrile umpolung - synthesis and reactivity of chloro
 aminophosphino carbynes.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10628
_journal_page_last               10641
_journal_paper_doi               10.1039/c9dt01838g
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C30 H41 B N7 O2 P W'
_chemical_formula_sum            'C30 H41 B N7 O2 P W'
_chemical_formula_weight         757.33
_space_group_crystal_system      trigonal
_space_group_IT_number           144
_space_group_name_Hall           'P 31'
_space_group_name_H-M_alt        'P 31'
_symmetry_space_group_name_Hall  'P 31'
_symmetry_space_group_name_H-M   'P 31'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-04-04 deposited with the CCDC.    2019-06-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   10.6921(2)
_cell_length_b                   10.6921(2)
_cell_length_c                   25.0214(2)
_cell_measurement_reflns_used    42135
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      73.3590
_cell_measurement_theta_min      4.7410
_cell_volume                     2477.24(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.0(1)
_diffrn_detector_area_resol_mean 8.1297
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_unetI/netI     0.0189
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            59289
_diffrn_reflns_point_group_measured_fraction_full 0.901
_diffrn_reflns_point_group_measured_fraction_max 0.892
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.772
_diffrn_reflns_theta_min         4.776
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    7.238
_exptl_absorpt_correction_T_max  0.775
_exptl_absorpt_correction_T_min  0.591
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
                        a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_description       trapezoid
_exptl_crystal_F_000             1140
_exptl_crystal_size_max          0.136
_exptl_crystal_size_mid          0.071
_exptl_crystal_size_min          0.061
_refine_diff_density_max         1.241
_refine_diff_density_min         -0.730
_refine_diff_density_rms         0.111
_refine_ls_abs_structure_details
;
 Flack x determined using 2562 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.026(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         5942
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0353
_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^)+(0.0713P)^2^+1.8690P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0906
_refine_ls_wR_factor_ref         0.0906
_reflns_Friedel_coverage         0.787
_reflns_Friedel_fraction_full    0.801
_reflns_Friedel_fraction_max     0.786
_reflns_number_gt                5930
_reflns_number_total             5942
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01838g2.cif
_cod_data_source_block           Compound_5c
_cod_depositor_comments
'Adding full bibliography for 1551229--1551233.cif.'
_cod_original_cell_volume        2477.24(9)
_cod_database_code               1551232
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              39421