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

data_7119334
_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         '2(C33 H53 Br3 P2 W)'
_chemical_formula_sum            'C66 H106 Br6 P4 W2'
_chemical_formula_weight         1870.54
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-11-08
_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                81.8120(17)
_cell_angle_beta                 88.384(2)
_cell_angle_gamma                84.131(2)
_cell_formula_units_Z            2
_cell_length_a                   11.7140(4)
_cell_length_b                   15.8440(3)
_cell_length_c                   20.4006(4)
_cell_measurement_reflns_used    26714
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      73.4680
_cell_measurement_theta_min      3.3010
_cell_volume                     3727.68(16)
_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 0.991
_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   -105.00 -10.00   1.00    4.00    --  -37.20 -77.00 120.00   95
  2  \w    -64.00  30.00   1.00    4.00    --  -37.20  77.00-120.00   94
  3  \w    -32.00 106.00   1.00    4.00    --   37.20   0.00 -90.00  138
  4  \w      8.00 109.00   1.00    4.00    --   37.20  19.00-120.00  101
  5  \w     23.00  91.00   1.00    4.00    --   37.20-125.00-150.00   68
  6  \w     23.00  91.00   1.00    4.00    --   37.20-125.00   0.00   68
  7  \w      1.00  76.00   1.00    4.00    --   37.20 -99.00 -60.00   75
  8  \w    -30.00  54.00   1.00    4.00    --   37.20 -57.00-150.00   84
  9  \w    -32.00  56.00   1.00    4.00    --   37.20 -38.00  90.00   88
 10  \w     10.00 105.00   1.00    4.00    --   37.20  77.00 -30.00   95
 11  \w     23.00  91.00   1.00    4.00    --   37.20-125.00  30.00   68
 12  \w    -32.00  56.00   1.00    4.00    --   37.20 -38.00   0.00   88
 13  \w     27.00  80.00   1.00    4.00    --   37.20-112.00  60.00   53
 14  \w     31.00  73.00   1.00    4.00    --   37.20-125.00 150.00   42
 15  \w     62.00 106.00   1.00    4.00    --   37.20  38.00  30.00   44
 16  \w    -30.00   3.00   1.00    4.00    --   37.20 -57.00  90.00   33
 17  \w     19.00  53.00   1.00    4.00    --   37.20  38.00  30.00   34
 18  \w     54.00  81.00   1.00    4.00    --   37.20-125.00 120.00   27
 19  \w      2.00  27.00   1.00    4.00    --   37.20 -99.00 120.00   25
 20  \w     44.00 128.00   1.00   16.00    --  111.00 -50.00 -60.00   84
 21  \w     86.00 120.00   1.00   16.00    --  111.00 -50.00 -30.00   34
 22  \w     50.00  77.00   1.00   16.00    --  111.00 -50.00 -30.00   27
 23  \w     42.00  69.00   1.00   16.00    --  111.00-111.00-180.00   27
 24  \w     98.00 132.00   1.00   16.00    --  111.00  38.00-180.00   34
 25  \w    104.00 147.00   1.00   16.00    --  111.00 178.00-150.00   43
 26  \w     73.00 100.00   1.00   16.00    --  111.00 -77.00 150.00   27
 27  \w     86.00 136.00   1.00   16.00    --  111.00 -25.00  90.00   50
 28  \w    129.00 156.00   1.00   16.00    --  111.00  64.00-120.00   27
 29  \w     85.00 112.00   1.00   16.00    --  111.00-111.00   0.00   27
 30  \w    148.00 175.00   1.00   16.00    --  111.00 111.00  60.00   27
 31  \w     77.00 135.00   1.00   16.00    --  111.00 -25.00-120.00   58
 32  \w     73.00 100.00   1.00   16.00    --  111.00 178.00 150.00   27
 33  \w     42.00  87.00   1.00   16.00    --  111.00-111.00 -60.00   45
 34  \w    115.00 157.00   1.00   16.00    --  111.00 -12.00  60.00   42
 35  \w    101.00 134.00   1.00   16.00    --  111.00 111.00  60.00   33
 36  \w     47.00  74.00   1.00   16.00    --  111.00 -77.00  90.00   27
 37  \w     99.00 126.00   1.00   16.00    --  111.00  25.00-150.00   27
 38  \w     42.00 105.00   1.00   16.00    --  111.00 -12.00  60.00   63
 39  \w    105.00 130.00   1.00   16.00    --  111.00 -77.00  90.00   25
 40  \w    113.00 152.00   1.00   16.00    --  111.00  77.00   0.00   39
 41  \w    100.00 125.00   1.00   16.00    --  111.00 -50.00 120.00   25
 42  \w     43.00 109.00   1.00   16.00    --  111.00 -92.00 150.00   66
 43  \w     54.00  96.00   1.00   16.00    --  111.00 -77.00 -30.00   42
 44  \w     96.00 130.00   1.00   16.00    --  111.00  38.00 -90.00   34
 45  \w    132.00 162.00   1.00   16.00    --  111.00  38.00 -90.00   30
 46  \w     47.00  74.00   1.00   16.00    --  111.00 -64.00 150.00   27
 47  \w     94.00 121.00   1.00   16.00    --  111.00 -64.00 150.00   27
 48  \w     75.00 116.00   1.00   16.00    --  111.00-111.00  30.00   41
 49  \w     71.00 114.00   1.00   16.00    --  111.00-111.00-120.00   43
 50  \w     86.00 120.00   1.00   16.00    --  111.00 -50.00 150.00   34
 51  \w    103.00 140.00   1.00   16.00    --  111.00 -92.00 -30.00   37
 52  \w    112.00 144.00   1.00   16.00    --  111.00 178.00 -90.00   32
 53  \w     42.00  68.00   1.00   16.00    --  111.00 -92.00 -30.00   26
 54  \w     58.00  83.00   1.00   16.00    --  111.00 178.00-150.00   25
 55  \w    118.00 157.00   1.00   16.00    --  111.00  77.00  60.00   39
 56  \w     43.00  69.00   1.00   16.00    --  111.00 -38.00 120.00   26
 57  \w     90.00 130.00   1.00   16.00    --  111.00 -38.00  90.00   40
 58  \w    105.00 146.00   1.00   16.00    --  111.00 -92.00-150.00   41
 59  \w     42.00  75.00   1.00   16.00    --  111.00 -38.00 -30.00   33
 60  \w     95.00 123.00   1.00   16.00    --  111.00 -64.00 -60.00   28
 61  \w     97.00 150.00   1.00   16.00    --  111.00  38.00 -30.00   53
 62  \w     42.00  71.00   1.00   16.00    --  111.00 -92.00-150.00   29
 63  \w    101.00 128.00   1.00   16.00    --  111.00 -50.00-180.00   27
 64  \w    116.00 172.00   1.00   16.00    --  111.00  50.00  30.00   56
 65  \w    144.00 177.00   1.00   16.00    --  111.00  77.00 -90.00   33
 66  \w     88.00 120.00   1.00   16.00    --  111.00 -38.00 -30.00   32
 67  \w    101.00 169.00   1.00   16.00    --  111.00 111.00  30.00   68
 68  \w     42.00 111.00   1.00   16.00    --  111.00-111.00 150.00   69
 69  \w    100.00 130.00   1.00   16.00    --  111.00 -38.00 120.00   30
 70  \w     66.00  93.00   1.00   16.00    --  111.00 178.00 -90.00   27
 71  \w     94.00 131.00   1.00   16.00    --  111.00  77.00 -90.00   37
 72  \w     98.00 147.00   1.00   16.00    --  111.00  38.00  60.00   49
 73  \w     70.00 114.00   1.00   16.00    --  111.00-111.00 -90.00   44
 74  \w     90.00 116.00   1.00   16.00    --  111.00-111.00 -30.00   26
 75  \w     90.00 116.00   1.00   16.00    --  111.00-111.00-180.00   26
 76  \w    121.00 146.00   1.00   16.00    --  111.00 178.00 150.00   25
 77  \w     46.00  73.00   1.00   16.00    --  111.00 -64.00-180.00   27
 78  \w     88.00 128.00   1.00   16.00    --  111.00 -64.00   0.00   40
 79  \w     81.00 122.00   1.00   16.00    --  111.00 -34.00   6.69   41
 80  \w     70.00  97.00   1.00   16.00    --  111.00 178.00  30.00   27
 81  \w     97.00 122.00   1.00   16.00    --  111.00 -79.00 -14.95   25
;
_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      -0.1272975000
_diffrn_orient_matrix_UB_12      0.0044532000
_diffrn_orient_matrix_UB_13      0.0216200000
_diffrn_orient_matrix_UB_21      -0.0346226000
_diffrn_orient_matrix_UB_22      -0.0042126000
_diffrn_orient_matrix_UB_23      -0.0716676000
_diffrn_orient_matrix_UB_31      0.0088798000
_diffrn_orient_matrix_UB_32      -0.0985318000
_diffrn_orient_matrix_UB_33      0.0147691000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            61566
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.082
_diffrn_reflns_theta_min         2.188
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.458
_exptl_absorpt_correction_T_max  0.43727
_exptl_absorpt_correction_T_min  0.37910
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_description       prism
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.251
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.025
_refine_diff_density_max         1.948
_refine_diff_density_min         -2.363
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     710
_refine_ls_number_reflns         15029
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0510P)^2^+4.9249P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0968
_refine_ls_wR_factor_ref         0.1018
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13010
_reflns_number_total             15029
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc08946a2.cif
_cod_data_source_block           rk12_scaled
_cod_original_cell_volume        3727.67(17)
_cod_database_code               7119334
_shelxl_version_number           2013-3
_chemical_oxdiff_formula         C33H53Br3P2W
_reflns_odcompleteness_completeness 98.47
_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, All C(H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C2AB) = Uanis(C4AB) = Uanis(C3AB)
Uanis(C1AA) = Uanis(C2AA) = Uanis(C4AA) = Uanis(C3AA)
3. Others
 Sof(H1BC)=Sof(H1BD)=Sof(H2B)=Sof(C1AB)=Sof(H1AE)=Sof(H1AF)=Sof(C2AB)=
 Sof(H2AC)=Sof(H2AD)=Sof(C4AB)=Sof(H4AC)=Sof(H4AD)=Sof(C3AB)=Sof(H3AC)=
 Sof(H3AD)=1-FVAR(1)
 Sof(H1AA)=Sof(H1AB)=Sof(H2A)=Sof(C2AA)=Sof(H2AA)=Sof(H2AB)=Sof(C1AA)=
 Sof(H1AC)=Sof(H1AD)=Sof(C3AA)=Sof(H3AA)=Sof(H3AB)=Sof(C4AA)=Sof(H4AA)=
 Sof(H4AB)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C10(H10), C13(H13), C16(H16), C17(H17), C2(H2A),
 C2(H2B)
4.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C12(H12A,H12B), C15(H15A,
 H15B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C24(H24A,H24B),
 C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C30(H30A,H30B),
  C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C35(H35A,H35B), C36(H36A,
 H36B), C0AA(H0AA,H0AB), C38(H38A,H38B), C40(H40A,H40B), C41(H41A,H41B),
 C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B), C49(H49A,H49B),
  C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B), C57(H57A,
 H57B), C60(H60A,H60B), C61(H61A,H61B), C62(H62A,H62B), C63(H63A,H63B),
 C67(H67A,H67B), C1(H1AA,H1AB), C1(H1BC,H1BD), C2AA(H2AA,H2AB), C1AA(H1AC,H1AD),
  C3AA(H3AA,H3AB), C4AA(H4AA,H4AB), C1AB(H1AE,H1AF), C2AB(H2AC,H2AD), C4AB(H4AC,
 H4AD), C3AB(H3AC,H3AD)
4.c Aromatic/amide H refined with riding coordinates:
 C18(H18), C43(H43), C50(H50), C58(H58), C59(H59), C66(H66), C68(H68),
 C69(H69), C72(H72), C73(H73)
;
_shelx_fab_checksum              54166
_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 1.576
_oxdiff_exptl_absorpt_empirical_full_min 0.624