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

data_7119335
_publ_section_title
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 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
'C27 H46 Br4 P2 W, C27 H48 Br4 P2 W, C H1.59 Cl2, C H1.88 Cl2'
_chemical_formula_sum            'C56 H98 Br8 Cl4 P4 W2'
_chemical_formula_weight         2044.00
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-09-27
_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                 100.001(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.5723(3)
_cell_length_b                   15.8298(3)
_cell_length_c                   25.1171(6)
_cell_measurement_reflns_used    24976
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      28.8710
_cell_measurement_theta_min      3.5760
_cell_volume                     7272.1(3)
_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      150.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3744
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.998
_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  30.00   1.00   70.00    --  -11.22 -99.00 150.00   50
  2  \w    -86.00  13.00   1.00   70.00    --  -11.22 -37.00 -30.00   99
  3  \w    -44.00  65.00   1.00   70.00    --  -11.22  77.00 120.00  109
  4  \w    -44.00  65.00   1.00   70.00    --  -11.22  77.00-180.00  109
  5  \w    -36.00  63.00   1.00   70.00    --  -11.22  37.00 -60.00   99
  6  \w    -86.00  13.00   1.00   70.00    --  -11.22 -37.00-120.00   99
  7  \w     35.00  80.00   1.00   70.00    --   11.30 178.00 120.00   45
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0015303000
_diffrn_orient_matrix_UB_12      -0.0001760000
_diffrn_orient_matrix_UB_13      0.0284180000
_diffrn_orient_matrix_UB_21      0.0377209000
_diffrn_orient_matrix_UB_22      -0.0102624000
_diffrn_orient_matrix_UB_23      0.0037299000
_diffrn_orient_matrix_UB_31      0.0088738000
_diffrn_orient_matrix_UB_32      0.0436094000
_diffrn_orient_matrix_UB_33      0.0009956000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0730
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            109424
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         3.257
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.825
_exptl_absorpt_correction_T_max  0.55842
_exptl_absorpt_correction_T_min  0.55028
_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 brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.867
_exptl_crystal_description       plate
_exptl_crystal_F_000             3960
_exptl_crystal_recrystallization_method
'Vapour diffusion of pentane into a conc. solution of DCM.'
_exptl_crystal_size_max          0.205
_exptl_crystal_size_mid          0.116
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.226
_refine_diff_density_min         -0.876
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     705
_refine_ls_number_reflns         12804
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0411
_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^)+(0.0113P)^2^+41.1681P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0678
_refine_ls_wR_factor_ref         0.0721
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10322
_reflns_number_total             12804
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc08946a2.cif
_cod_data_source_block           Compound_2d
_cod_database_code               7119335
_shelxl_version_number           2013-3
_chemical_oxdiff_formula         C29H48Br2O2P2W
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_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) groups
2. Uiso/Uaniso restraints and constraints
Uanis(Cl4A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Sof(Cl1A)=Sof(Cl2A)=1-FVAR(1)
 Sof(Cl1)=Sof(Cl2)=Sof(H9BA)=Sof(H9BB)=FVAR(1)
 Sof(H31)=Sof(Cl4A)=Sof(Cl3A)=1-FVAR(2)
 Sof(Cl3)=Sof(Cl4)=Sof(H31A)=Sof(H31B)=FVAR(2)
4.a Ternary CH refined with riding coordinates:
 C9(H9), C15(H15), C8BA(H8BA), C20(H20), C0BA(H0BA), C2AA(H2AA), C9AA(H9AA),
 C1BA(H1BA)
4.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C13(H13A,H13B), C10(H10A,H10B), C11(H11A,H11B), C14(H14A,
 H14B), C17(H17A,H17B), C0AA(H0AA,H0AB), C24(H24A,H24B), C25(H25A,H25B),
 C26(H26A,H26B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C32(H32A,H32B),
  C36(H36A,H36B), C37(H37A,H37B), C39(H39A,H39B), C40(H40A,H40B), C42(H42A,
 H42B), C45(H45A,H45B), C46(H46A,H46B), C8AA(H8AA,H8AB), C3AA(H3AA,H3AB),
 C7AA(H7AA,H7AB), C4AA(H4AA,H4AB), C7BA(H7BA,H7BB), C5AA(H5AA,H5AB), C6AA(H6AA,
 H6AB), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C27(H27A,H27B),
 C2BA(H2BA,H2BB), C34(H34A,H34B), C38(H38A,H38B), C3BA(H3BA,H3BB), C43(H43A,
 H43B), C4BA(H4BA,H4BB), C5BA(H5BA,H5BB), C6BA(H6BA,H6BB), C16(H16A,H16B),
 C19(H19A,H19B), C9BA(H9BA,H9BB), C31(H31A,H31B)
4.c Aromatic/amide H refined with riding coordinates:
 C31(H31), C0CA(H0CA), C1CA(H1CA)
;
_shelx_fab_checksum              28696
_ins_header
;
TITL RK11_scaled2 in P2(1)/c 
REM P2(1)/c (#14 in standard setting)
CELL 0.71073  18.572260  15.829825  25.117115  90.0000 100.0005  90.0000
ZERR   11.00   0.000338   0.000265   0.000636   0.0000   0.0021   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2 
SFAC C H O P Br W
UNIT 319.00 528.00 22.00 22.00 22.00 11.00
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 1.496
_oxdiff_exptl_absorpt_empirical_full_min 0.852