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_7126399
_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         'C72 H74 B2 Br2 Mo2 N12 O4 P2 Pd2'
_chemical_formula_sum            'C82 H92 B2 Br2 Mo2 N12 O7 P2 Pd2'
_chemical_formula_weight         2005.73
_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
_audit_creation_date             2019-06-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 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                 104.9650(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.0575(4)
_cell_length_b                   11.7128(2)
_cell_length_c                   29.6534(3)
_cell_measurement_reflns_used    13212
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      73.6570
_cell_measurement_theta_min      3.9460
_cell_volume                     9079.0(2)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(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 0.976
_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    -44.00  20.00   1.00    8.11    --  -37.21  57.00  85.00   64
  2  \w     -2.00  66.00   1.00    8.11    --   37.21 -19.00 -90.00   68
  3  \w    -30.00  -3.00   1.00    8.11    --   37.21 -19.00 -90.00   27
  4  \w    -16.00  63.00   1.00    8.11    --   37.21 -77.00-150.00   79
  5  \w     41.00  91.00   1.00    8.11    --   37.21-125.00  90.00   50
  6  \w     27.00 102.00   1.00    8.11    --   37.21  57.00 120.00   75
  7  \w    105.00 175.00   1.00   32.44    --  111.00 111.00 150.00   70
  8  \w     92.00 175.00   1.00   32.44    --  111.00  64.00 -30.00   83
  9  \w     43.00 106.00   1.00   32.44    --  111.00 -92.00-150.00   63
 10  \w     44.00 128.00   1.00   32.44    --  111.00 -50.00-180.00   84
 11  \w     51.00 106.00   1.00   32.44    --  111.00 -92.00  60.00   55
 12  \w     65.00 109.00   1.00   32.44    --  111.00-111.00   0.00   44
 13  \w    104.00 177.00   1.00   32.44    --  111.00  77.00-120.00   73
 14  \w     97.00 178.00   1.00   32.44    --  111.00  64.00 -60.00   81
;
_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      -0.0514103000
_diffrn_orient_matrix_UB_12      0.0242090000
_diffrn_orient_matrix_UB_13      -0.0356348000
_diffrn_orient_matrix_UB_21      -0.0075070000
_diffrn_orient_matrix_UB_22      -0.1289243000
_diffrn_orient_matrix_UB_23      -0.0096031000
_diffrn_orient_matrix_UB_31      -0.0278606000
_diffrn_orient_matrix_UB_32      -0.0096407000
_diffrn_orient_matrix_UB_33      0.0390705000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0567
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            37379
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.842
_diffrn_reflns_theta_min         3.382
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.167
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65591
_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    1.467
_exptl_crystal_description       block
_exptl_crystal_F_000             4040
_exptl_crystal_size_max          0.246
_exptl_crystal_size_mid          0.108
_exptl_crystal_size_min          0.046
_refine_diff_density_max         1.699
_refine_diff_density_min         -0.942
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     895
_refine_ls_number_reflns         17953
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0707
_refine_ls_R_factor_gt           0.0565
_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^)+(0.0452P)^2^+37.9025P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1312
_refine_ls_wR_factor_ref         0.1374
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14248
_reflns_number_total             17953
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc02070b3.cif
_cod_data_source_block           5a_Et2O
_cod_depositor_comments
'Adding full bibliography for 7126395--7126402.cif.'
_cod_database_code               7126399
_publcif_datablock.id            {04c6bbd9-ded0-48ba-a2e4-9959bdc8849a}
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C104 H104 B2 N12 O4 P2 Br2 Mo2 Pd2'
_chemical_oxdiff_usercomment     'Liq diff n-hex into THF, 0 degC'
_reflns_odcompleteness_completeness 98.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_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), B2(H2)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C17(H17), C22(H22), C27(H27), C32(H32), C37(H37), C41(H41),
 C42(H42), C43(H43), C44(H44), C45(H45), C51(H51), C52(H52), C53(H53), C54(H54),
  C55(H55), C61(H61), C62(H62), C63(H63), C64(H64), C65(H65), C71(H71),
 C72(H72), C73(H73), C74(H74), C75(H75), C81(H81), C82(H82), C83(H83), C84(H84),
  C85(H85), C91(H91), C92(H92), C93(H93), C94(H94), C95(H95)
2.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C29(H29A,
 H29B,H29C), C30(H30A,H30B,H30C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C),
 C39(H39A,H39B,H39C)
;
_shelx_res_checksum              14584
_shelx_hkl_checksum              97197
_shelx_fab_checksum              18111
_ins_header
;
TITL LB012_scale in P2(1)/n 
REM P2(1)/n (#14 in standard setting)
CELL 1.54184  27.057466  11.712830  29.653386  90.0000 104.9648  90.0000
ZERR    4.00   0.000407   0.000151   0.000343   0.0000   0.0013   0.0000
LATT  1
SYMM -x+1/2, y+1/2,-z+1/2 
SFAC C H B N O P Br Mo Pd
UNIT 416.00 416.00 8.00 48.00 16.00 8.00 8.00 8.00 8.00
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 1.581
_oxdiff_exptl_absorpt_empirical_full_min 0.803
_publcif_funding_html
;
;