High oxidation state bromocarbyne complexes.
Hill, Anthony F.; Kong, Richard Y.; Chemical communications (Cambridge, England) 53 (2017) 759–762; doi:10.1039/c6cc08946a

data_7119333
_publ_section_title
;
 High oxidation state bromocarbyne complexes.
;
_journal_issue                   4
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              759
_journal_page_last               762
_journal_paper_doi               10.1039/c6cc08946a
_journal_volume                  53
_journal_year                    2017
_chemical_formula_moiety         'C35 H53 Br O2 P2 W'
_chemical_formula_sum            'C35 H53 Br O2 P2 W'
_chemical_formula_weight         831.47
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-09-28
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2016-11-08 deposited with the CCDC.
2016-12-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.0542(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.41025(11)
_cell_length_b                   13.66762(12)
_cell_length_c                   23.3661(3)
_cell_measurement_reflns_used    37403
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      73.7430
_cell_measurement_theta_min      3.7230
_cell_volume                     3588.01(7)
_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    'olex2.solve (Bourhis et al., 2015)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.989
_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   -108.00  -8.00   1.00    1.00    --  -36.95 -19.00 150.00  100
  2  \w      1.00  76.00   1.00    1.00    --   36.95 -99.00 -30.00   75
  3  \w     20.00 104.00   1.00    1.00    --   36.95  57.00 150.00   84
  4  \w     20.00 104.00   1.00    1.00    --   36.95  57.00-120.00   84
  5  \w     20.00 104.00   1.00    1.00    --   36.95  57.00-180.00   84
  6  \w     23.00  90.00   1.00    1.00    --   36.95-125.00  60.00   67
  7  \w    -32.00  56.00   1.00    1.00    --   36.95 -38.00 -90.00   88
  8  \w    -34.00  66.00   1.00    1.00    --   36.95 -19.00   0.00  100
  9  \w     23.00  90.00   1.00    1.00    --   36.95-125.00  90.00   67
 10  \w     24.00  51.00   1.00    1.00    --   36.95 -57.00   0.00   27
 11  \w    -29.00  14.00   1.00    1.00    --   36.95 -57.00   0.00   43
 12  \w    -31.00  55.00   1.00    1.00    --   36.95 -38.00  60.00   86
 13  \w     23.00  86.00   1.00    1.00    --   36.95-125.00-120.00   63
 14  \w     32.00  65.00   1.00    1.00    --   36.95-125.00 -30.00   33
 15  \w     39.00  65.00   1.00    1.00    --   36.95 -99.00 150.00   26
 16  \w     42.00  67.00   1.00    1.00    --  111.00-111.00  30.00   25
 17  \w     95.00 139.00   1.00    1.00    --  111.00  38.00-120.00   44
 18  \w     44.00  69.00   1.00    1.00    --  111.00 -50.00  90.00   25
 19  \w     80.00 113.00   1.00    1.00    --  111.00-111.00-120.00   33
 20  \w     57.00 113.00   1.00    1.00    --  111.00-111.00-180.00   56
 21  \w     73.00 106.00   1.00    1.00    --  111.00 -38.00  60.00   33
 22  \w    152.00 177.00   1.00    1.00    --  111.00  38.00   0.00   25
 23  \w     61.00 132.00   1.00    1.00    --  111.00 -25.00  60.00   71
 24  \w    100.00 126.00   1.00    1.00    --  111.00 -64.00   0.00   26
 25  \w     72.00 126.00   1.00    1.00    --  111.00 -50.00 150.00   54
 26  \w     42.00  68.00   1.00    1.00    --  111.00 -92.00 -90.00   26
 27  \w     91.00 150.00   1.00    1.00    --  111.00  25.00 120.00   59
 28  \w     53.00 101.00   1.00    1.00    --  111.00 -64.00  90.00   48
 29  \w     69.00 115.00   1.00    1.00    --  111.00 -25.00-150.00   46
 30  \w    153.00 178.00   1.00    1.00    --  111.00  12.00  90.00   25
 31  \w     65.00 127.00   1.00    1.00    --  111.00  12.00  90.00   62
 32  \w     43.00 103.00   1.00    1.00    --  111.00 -50.00-150.00   60
 33  \w     76.00 102.00   1.00    1.00    --  111.00 -64.00 -60.00   26
 34  \w     92.00 119.00   1.00    1.00    --  111.00  25.00 -30.00   27
 35  \w    105.00 130.00   1.00    1.00    --  111.00 -38.00 -30.00   25
 36  \w     95.00 132.00   1.00    1.00    --  111.00  38.00   0.00   37
 37  \w     45.00 104.00   1.00    1.00    --  111.00 -92.00   0.00   59
 38  \w     43.00 113.00   1.00    1.00    --  111.00-111.00-150.00   70
 39  \w    102.00 176.00   1.00    1.00    --  111.00  77.00-120.00   74
 40  \w     43.00  93.00   1.00    1.00    --  111.00-111.00  90.00   50
 41  \w    131.00 177.00   1.00    1.00    --  111.00  12.00-150.00   46
 42  \w    104.00 130.00   1.00    1.00    --  111.00 -64.00 -60.00   26
 43  \w     70.00 104.00   1.00    1.00    --  111.00 -38.00 120.00   34
 44  \w     73.00 120.00   1.00    1.00    --  111.00 -92.00 -30.00   47
 45  \w     52.00 114.00   1.00    1.00    --  111.00-111.00 120.00   62
 46  \w     47.00  72.00   1.00    1.00    --  111.00 -92.00  90.00   25
 47  \w     90.00 116.00   1.00    1.00    --  111.00 -92.00  90.00   26
 48  \w    104.00 177.00   1.00    1.00    --  111.00  50.00  60.00   73
 49  \w    101.00 149.00   1.00    1.00    --  111.00 178.00  60.00   48
 50  \w     68.00  93.00   1.00    1.00    --  111.00 -77.00   0.00   25
 51  \w    104.00 134.00   1.00    1.00    --  111.00 -77.00   0.00   30
 52  \w     91.00 117.00   1.00    1.00    --  111.00  12.00-150.00   26
 53  \w    129.00 155.00   1.00    1.00    --  111.00  50.00  30.00   26
 54  \w     42.00  86.00   1.00    1.00    --  111.00 -38.00 -30.00   44
 55  \w    106.00 132.00   1.00    1.00    --  111.00 -25.00   0.00   26
 56  \w     47.00 125.00   1.00    1.00    --  111.00 -64.00 150.00   78
 57  \w     98.00 130.00   1.00    1.00    --  111.00 -77.00-150.00   32
 58  \w     59.00  85.00   1.00    1.00    --  111.00 -25.00   0.00   26
 59  \w     43.00 131.00   1.00    1.00    --  111.00   5.00  31.63   88
 60  \w    135.00 161.00   1.00    1.00    --  111.00  38.00 150.00   26
 61  \w     75.00 116.00   1.00    1.00    --  111.00-111.00 -90.00   41
 62  \w    117.00 143.00   1.00    1.00    --  111.00  38.00  60.00   26
 63  \w     99.00 125.00   1.00    1.00    --  111.00 -77.00-180.00   26
 64  \w     54.00  84.00   1.00    1.00    --  111.00 -50.00 -30.00   30
 65  \w     94.00 139.00   1.00    1.00    --  111.00  50.00 120.00   45
 66  \w     43.00 108.00   1.00    1.00    --  111.00 -50.00 -90.00   65
 67  \w     92.00 133.00   1.00    1.00    --  111.00  64.00-125.03   41
 68  \w     58.00  83.00   1.00    1.00    --  111.00 -25.00  90.00   25
 69  \w     84.00 110.00   1.00    1.00    --  111.00 -77.00 150.00   26
 70  \w    104.00 130.00   1.00    1.00    --  111.00 -92.00 -90.00   26
 71  \w     53.00  78.00   1.00    1.00    --  111.00 -92.00  60.00   25
 72  \w     83.00 114.00   1.00    1.00    --  111.00 -81.00  83.87   31
;
_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      0.0254962000
_diffrn_orient_matrix_UB_12      -0.0148056000
_diffrn_orient_matrix_UB_13      0.0663694000
_diffrn_orient_matrix_UB_21      -0.1344013000
_diffrn_orient_matrix_UB_22      -0.0105577000
_diffrn_orient_matrix_UB_23      0.0000503000
_diffrn_orient_matrix_UB_31      0.0093691000
_diffrn_orient_matrix_UB_32      -0.1112479000
_diffrn_orient_matrix_UB_33      -0.0088422000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0486
_diffrn_reflns_av_unetI/netI     0.0212
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            55340
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.351
_diffrn_reflns_theta_min         3.762
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.322
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.10723
_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 orangish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_description       plate
_exptl_crystal_F_000             1672
_exptl_crystal_preparation
'slow evaporation of pentane/chloroform solution'
_exptl_crystal_recrystallization_method 'achieved in air'
_exptl_crystal_size_max          0.454
_exptl_crystal_size_mid          0.262
_exptl_crystal_size_min          0.042
_refine_diff_density_max         1.321
_refine_diff_density_min         -2.190
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         7242
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0339
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0652P)^2^+2.5986P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0908
_refine_ls_wR_factor_ref         0.0914
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7100
_reflns_number_total             7242
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc08946a2.cif
_cod_data_source_block           rk08_scaled
_cod_original_cell_volume        3588.01(6)
_cod_database_code               7119333
_shelxl_version_number           2013-3
_chemical_oxdiff_formula         C35H53BrO2P2W
_reflns_odcompleteness_completeness 98.59
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C12(H12), C30(H30), C24(H24), C18(H18)
2.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C14(H14A,H14B), C15(H15A,H15B), C13(H13A,H13B), C16(H16A,
 H16B), C31(H31A,H31B), C35(H35A,H35B), C20(H20A,H20B), C19(H19A,H19B),
 C23(H23A,H23B), C25(H25A,H25B), C26(H26A,H26B), C32(H32A,H32B), C29(H29A,H29B),
  C22(H22A,H22B), C34(H34A,H34B), C21(H21A,H21B), C28(H28A,H28B), C33(H33A,
 H33B), C27(H27A,H27B), C10(H10A,H10B), C11(H11A,H11B)
2.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C4(H4), C5(H5), C3(H3)
;
_ins_header
;
TITL RK08_scaled in P2(1)/n 
REM P2(1)/n (#14 in standard setting)
CELL 1.54184  11.410255  13.667622  23.366128  90.0000 100.0542  90.0000
ZERR    5.00   0.000113   0.000120   0.000262   0.0000   0.0010   0.0000
LATT  1
SYMM -x+1/2, y+1/2,-z+1/2 
SFAC C H O P Br W
UNIT 175.00 265.00 10.00 10.00 5.00 5.00
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 5.434
_oxdiff_exptl_absorpt_empirical_full_min 0.595