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_7126397
_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         'C54 H52 B Br N6 O2 P2 Pt W'
_chemical_formula_sum            'C54 H52 B Br N6 O2 P2 Pt W'
_chemical_formula_weight         1348.61
_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     dual
_audit_creation_date             2019-03-21
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-03-06 deposited with the CCDC.	2020-04-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.6360(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.59230(10)
_cell_length_b                   22.6404(4)
_cell_length_c                   23.4154(3)
_cell_measurement_reflns_used    8021
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.5750
_cell_measurement_theta_min      4.7470
_cell_volume                     5027.55(12)
_computing_cell_refinement       'CrysAlisPro 1.171.40.36a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.36a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.36a (Rigaku OD, 2018)'
_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 0.995
_diffrn_measured_fraction_theta_max 0.973
_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     21.00 106.00   1.00    4.00    --   37.20  38.00 120.00   85
  2  \w    -11.00  54.00   1.00    4.00    --   37.20 -57.00-120.00   65
  3  \w    -24.00  65.00   1.00    4.00    --   37.20 -19.00  90.00   89
  4  \w      7.00  76.00   1.00    4.00    --   37.20 -99.00   0.00   69
  5  \w     58.00 131.00   1.00   12.00    --  111.00 -25.00   0.00   73
  6  \w     59.00 109.00   1.00   12.00    --  111.00-111.00  30.00   50
  7  \w     63.00 117.00   1.00   12.00    --  111.00 -38.00 -60.00   54
  8  \w     52.00 106.00   1.00   12.00    --  111.00 -92.00 -90.00   54
  9  \w     41.00  84.00   1.00   12.00    --  111.00-111.00  90.00   43
 10  \w    124.00 175.00   1.00   12.00    --  111.00  77.00  30.00   51
 11  \w     41.00 133.00   1.00   12.00    --  111.00 -25.00  90.00   92
 12  \w     45.00 128.00   1.00   12.00    --  111.00 -50.00-120.00   83
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0492435000
_diffrn_orient_matrix_UB_12      -0.0638859000
_diffrn_orient_matrix_UB_13      -0.0076447000
_diffrn_orient_matrix_UB_21      0.1077450000
_diffrn_orient_matrix_UB_22      0.0224288000
_diffrn_orient_matrix_UB_23      -0.0375603000
_diffrn_orient_matrix_UB_31      0.1111834000
_diffrn_orient_matrix_UB_32      0.0065154000
_diffrn_orient_matrix_UB_33      0.0544205000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18731
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.753
_diffrn_reflns_theta_min         3.819
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.205
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84689
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.36a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_density_diffrn    1.782
_exptl_crystal_description       plate
_exptl_crystal_F_000             2624
_exptl_crystal_size_max          0.135
_exptl_crystal_size_mid          0.054
_exptl_crystal_size_min          0.035
_refine_diff_density_max         1.854
_refine_diff_density_min         -2.477
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     619
_refine_ls_number_reflns         9886
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0371
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0527P)^2^+13.7141P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0925
_refine_ls_wR_factor_ref         0.0979
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8545
_reflns_number_total             9886
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc02070b3.cif
_cod_data_source_block           2b
_cod_depositor_comments
'Adding full bibliography for 7126395--7126402.cif.'
_cod_database_code               7126397
_publcif_datablock.id            {3da3ee68-6444-4c9d-8da2-df66d939449c}
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C52 H52 B1 N6 P2 Br W1 Pt1'
_chemical_oxdiff_usercomment     'True evap. Ether/n-pent'
_reflns_odcompleteness_completeness 99.25
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_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:
 B1(H1)
2.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C23(H23), C33(H33), C42(H42), C43(H43), C44(H44), C45(H45),
 C46(H46), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C62(H62), C63(H63),
  C64(H64), C65(H65), C66(H66), C72(H72), C73(H73), C74(H74), C75(H75),
 C76(H76), C82(H82), C83(H83), C84(H84), C85(H85), C86(H86), C92(H92), C93(H93),
  C94(H94), C95(H95), C96(H96)
2.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C15(H15A,H15B,H15C), C21(H21A,H21B,H21C), C25(H25A,H25B,
 H25C), C31(H31A,H31B,H31C), C35(H35A,H35B,H35C)
;
_shelx_res_checksum              5213
_shelx_hkl_checksum              91643
_ins_header
;
TITL LB003_scale in P2(1)/n 
REM P2(1)/n (#14 in standard setting)
CELL 1.54184   9.592335  22.640353  23.415446  90.0000  98.6362  90.0000
ZERR    4.00   0.000113   0.000357   0.000295   0.0000   0.0011   0.0000
LATT  1
SYMM -x+1/2, y+1/2,-z+1/2 
SFAC C H B N P Br W Pt
UNIT 208.00 208.00 4.00 24.00 8.00 4.00 4.00 4.00
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 1.267
_oxdiff_exptl_absorpt_empirical_full_min 0.865
_publcif_funding_html
;
;