The significance of phosphoniocarbynes in halocarbyne cross-coupling reactions.
Burt, Liam K.; Cordiner, Richard L.; Hill, Anthony F.; Manzano, Richard A.; Wagler, Jörg; Chemical communications (Cambridge, England) 56 (2020) 5673–5676; doi:10.1039/d0cc02070b

data_7126401
_publ_section_title
;
 The significance of phosphoniocarbynes in halocarbyne cross-coupling
 reactions.
;
_journal_issue                   42
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5673
_journal_page_last               5676
_journal_paper_doi               10.1039/d0cc02070b
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C36 H37 B Br N6 O2 P Pd W, 3(C H Cl3)'
_chemical_formula_sum            'C39 H40 B Br Cl9 N6 O2 P Pd W'
_chemical_formula_weight         1355.76
_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_creation_date             2017-02-07
_audit_creation_method
;
Olex2 1.2
(compiled Dec 12 2016 15:38:10 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2020-03-06 deposited with the CCDC.	2020-04-08 downloaded from the CCDC.
;
_cell_angle_alpha                85.274(3)
_cell_angle_beta                 87.055(2)
_cell_angle_gamma                70.772(3)
_cell_formula_units_Z            2
_cell_length_a                   11.4100(4)
_cell_length_b                   13.4275(5)
_cell_length_c                   17.2454(5)
_cell_measurement_reflns_used    14107
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      27.3660
_cell_measurement_theta_min      2.7570
_cell_volume                     2485.43(15)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -20.00  54.00   1.00    8.34    --   15.42 -99.00 -90.00   74
  2  \w     -3.00  85.00   1.00    8.34    --   15.42  38.00  90.00   88
  3  \w     -1.00  83.00   1.00    8.34    --   15.42  57.00   0.00   84
  4  \w    -84.00  10.00   1.00    8.34    --  -16.36 -77.00 120.00   94
  5  \w     -1.00  83.00   1.00    8.34    --   15.42  57.00-120.00   84
  6  \w     35.00  88.00   1.00    8.34    --   15.42 178.00-120.00   53
  7  \w     35.00  88.00   1.00    8.34    --   15.42 178.00  60.00   53
  8  \w    -52.00  32.00   1.00    8.34    --   15.42 -57.00  90.00   84
  9  \w    -20.00  54.00   1.00    8.34    --   15.42 -99.00-180.00   74
 10  \w    -20.00  54.00   1.00    8.34    --   15.42 -99.00  60.00   74
 11  \w    -11.00  83.00   1.00    8.34    --   15.42  77.00 -30.00   94
 12  \w    -20.00  21.00   1.00    8.34    --   15.42 -99.00 -30.00   41
 13  \w    -52.00  32.00   1.00    8.34    --   15.42 -57.00 -30.00   84
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0403433000
_diffrn_orient_matrix_UB_12      -0.0047733000
_diffrn_orient_matrix_UB_13      0.0317249000
_diffrn_orient_matrix_UB_21      0.0174890000
_diffrn_orient_matrix_UB_22      -0.0551712000
_diffrn_orient_matrix_UB_23      -0.0040210000
_diffrn_orient_matrix_UB_31      0.0490307000
_diffrn_orient_matrix_UB_32      -0.0088535000
_diffrn_orient_matrix_UB_33      0.0261096000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0600
_diffrn_reflns_av_unetI/netI     0.0499
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            50588
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.932
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.034
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80779
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.812
_exptl_crystal_description       block
_exptl_crystal_F_000             1320
_exptl_crystal_preparation
'Vapor-vapor diffusion of hexane into chloroform solution'
_exptl_crystal_size_max          0.239
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.035
_refine_diff_density_max         1.541
_refine_diff_density_min         -1.387
_refine_diff_density_rms         0.136
_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     556
_refine_ls_number_reflns         10177
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0398
_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^)+(0.0320P)^2^+7.1610P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0842
_refine_ls_wR_factor_ref         0.0892
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8724
_reflns_number_total             10177
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc02070b3.cif
_cod_data_source_block           Compound_8
_cod_depositor_comments
'Adding full bibliography for 7126395--7126402.cif.'
_cod_database_code               7126401
_publcif_datablock.id            {ba2cac51-1f2a-4f6d-9fbf-86ef46b1b50c}
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         'C54 H52 B1 Br1 N6 O2 P2 Pd1 W'
_chemical_oxdiff_usercomment     'Orange plate from CH3Cl and pentane'
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C39(H39), B1(H1), C38(H38), C37(H37)
2.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C6(H6), C11(H11), C27(H27), C30(H30), C32(H32), C20(H20), C28(H28),
 C29(H29), C26(H26), C24(H24), C36(H36), C22(H22), C21(H21), C33(H33), C34(H34),
  C23(H23), C35(H35)
2.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C4(H4A,H4B,H4C),
 C18(H18A,H18B,H18C), C13(H13A,H13B,H13C)
;
_shelx_res_checksum              92862
_shelx_hkl_checksum              35648
_ins_header
;
TITL RAM-013_scale in P1 
REM P1 (#1 in standard setting)
CELL 0.71073  11.410034  13.427538  17.245449  85.2739  87.0550  70.7717
ZERR    2.00   0.000367   0.000471   0.000519   0.0027   0.0025   0.0030
LATT -1
SFAC C H B N O P Br Pd W
UNIT 108.00 104.00 2.00 12.00 4.00 4.00 2.00 2.00 2.00
TREF
HKLF 4
END
;
_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 1.432
_oxdiff_exptl_absorpt_empirical_full_min 0.792
_publcif_funding_html
;
;