Confluence of disparate carbido chemistries: [WRuAu<sub>2</sub>(μ-C)<sub>2</sub>Cl<sub>2</sub>(CO)<sub>2</sub>(PCy<sub>3</sub>)<sub>2</sub>(Tp*)].
Reinholdt, Anders; Bendix, Jesper; Hill, Anthony F.; Manzano, Richard A.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 14893–14896; doi:10.1039/c8dt03851a

data_7047723
_publ_section_title
;
 Confluence of disparate carbido chemistries:
 [WRuAu<sub>2</sub>(\m-C)<sub>2</sub>Cl<sub>2</sub>(CO)<sub>2</sub>(PCy<sub>3</sub>)<sub>2</sub>(Tp*)].
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14893
_journal_page_last               14896
_journal_paper_doi               10.1039/c8dt03851a
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C55 H88 Au2 B Cl3 N6 O2 P2 Ru W'
_chemical_formula_sum            'C55 H88 Au2 B Cl3 N6 O2 P2 Ru W'
_chemical_formula_weight         1723.26
_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   mixed
_audit_creation_date             2016-11-15
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2018-06-06 deposited with the CCDC.
2018-10-05 downloaded from the CCDC.
;
_cell_angle_alpha                73.1381(17)
_cell_angle_beta                 81.6834(17)
_cell_angle_gamma                65.5781(18)
_cell_formula_units_Z            2
_cell_length_a                   13.8516(3)
_cell_length_b                   14.6061(3)
_cell_length_c                   17.1538(4)
_cell_measurement_reflns_used    28949
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.5490
_cell_measurement_theta_min      3.4610
_cell_volume                     3022.92(12)
_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(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3744
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_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    -39.00  62.00   1.00   40.45    --  -11.22  57.00-150.00  101
  2  \w    -20.00  30.00   1.00   40.45    --  -11.22 -99.00 -30.00   50
  3  \w    -36.00  63.00   1.00   40.45    --  -11.22  37.00   0.00   99
  4  \w    -98.00 -34.00   1.00   40.45    --  -11.22 178.00 150.00   64
  5  \w    -83.00  17.00   1.00   40.45    --  -11.22 -57.00  60.00  100
  6  \w    -36.00  63.00   1.00   40.45    --  -11.22  37.00 120.00   99
  7  \w    -20.00  30.00   1.00   40.45    --  -11.22 -99.00 -90.00   50
  8  \w    -68.00  -3.00   1.00   40.45    --  -11.22 126.00  18.00   65
  9  \w    -36.00   5.00   1.00   40.45    --  -11.22  37.00-180.00   41
 10  \w    -17.00  84.00   1.00   40.45    --   11.30  57.00 -90.00  101
;
_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      -0.0165111000
_diffrn_orient_matrix_UB_12      0.0030154000
_diffrn_orient_matrix_UB_13      0.0406189000
_diffrn_orient_matrix_UB_21      -0.0332742000
_diffrn_orient_matrix_UB_22      0.0532061000
_diffrn_orient_matrix_UB_23      -0.0145101000
_diffrn_orient_matrix_UB_31      -0.0422564000
_diffrn_orient_matrix_UB_32      -0.0142591000
_diffrn_orient_matrix_UB_33      -0.0028132000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            61026
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.232
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.210
_exptl_absorpt_correction_T_max  0.56571
_exptl_absorpt_correction_T_min  0.55728
_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 yellowish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.893
_exptl_crystal_description       prism
_exptl_crystal_F_000             1676
_exptl_crystal_size_max          0.328
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.064
_refine_diff_density_max         2.449
_refine_diff_density_min         -1.089
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     704
_refine_ls_number_reflns         12338
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0319
_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^)+(0.0196P)^2^+17.4302P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0698
_refine_ls_wR_factor_ref         0.0734
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10824
_reflns_number_total             12338
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03851a2.cif
_cod_data_source_block           Compound_4
_cod_depositor_comments
'Adding full bibliography for 7047722--7047723.cif.'
_cod_original_cell_volume        3022.91(11)
_cod_database_code               7047723
_shelxl_version_number           2013-3
_chemical_oxdiff_formula         'C55 H88 Au2 B Cl3 N6 O2 P2 Ru W'
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H52A,H52B,H1} of C52, All C(H,H) groups, All C(H,H,H,H)
  groups
 At 1.5 times of:
  {H9A,H9B,H9C} of C9, {H5A,H5B,H5C} of C5, {H15A,H15B,H15C} of C15, {H10A,
  H10B,H10C} of C10, {H19A,H19B,H19C} of C19, {H14A,H14B,H14C} of C14
2. Uiso/Uaniso restraints and constraints
Uanis(C38A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Sof(H39C)=Sof(H39D)=Sof(H42C)=Sof(H42D)=Sof(C38A)=Sof(H38A)=Sof(C43A)=
 Sof(H43C)=Sof(H43D)=Sof(C40A)=Sof(H40C)=Sof(H40D)=Sof(C41A)=Sof(H41C)=
 Sof(H41D)=1-FVAR(1)
 Sof(H39A)=Sof(H39B)=Sof(H42A)=Sof(H42B)=Sof(C38)=Sof(H38)=Sof(C40)=Sof(H40A)=
 Sof(H40B)=Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(C41)=Sof(H41A)=Sof(H41B)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C26(H26), C44(H44), C32(H32), C20(H20), C50(H50), C38(H38), C38A(H38A)
4.b Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C30(H30A,H30B), C31(H31A,H31B), C29(H29A,H29B), C27(H27A,
 H27B), C45(H45A,H45B), C33(H33A,H33B), C22(H22A,H22B), C25(H25A,H25B),
 C21(H21A,H21B), C37(H37A,H37B), C23(H23A,H23B), C49(H49A,H49B), C54(H54A,H54B),
  C46(H46A,H46B), C34(H34A,H34B), C48(H48A,H48B), C47(H47A,H47B), C35(H35A,
 H35B), C36(H36A,H36B), C24(H24A,H24B), C53(H53A,H53B), C51(H51A,H51B),
 C55(H55A,H55B), C52(H52A,H52B), C39(H39A,H39B), C39(H39C,H39D), C42(H42A,H42B),
  C42(H42C,H42D), C40(H40A,H40B), C43(H43A,H43B), C41(H41A,H41B), C43A(H43C,
 H43D), C40A(H40C,H40D), C41A(H41C,H41D)
4.c Aromatic/amide H refined with riding coordinates:
 C17(H17), C12(H12), C7(H7)
4.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C15(H15A,H15B,H15C), C10(H10A,H10B,H10C), C5(H5A,H5B,
 H5C), C14(H14A,H14B,H14C), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              34205
_ins_header
;
TITL RuCAuCl-WCSnBu3-scale in P-1 
REM P-1 (#2 in standard setting)
CELL 0.71073  13.851560  14.606083  17.153816  73.1381  81.6834  65.5781
ZERR    2.00   0.000273   0.000266   0.000365   0.0017   0.0017   0.0018
LATT  1
SFAC C H B N O P Cl Ru Sn W Au
UNIT 120.00 200.00 2.00 12.00 6.00 4.00 8.00 2.00 2.00 2.00 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 1.918
_oxdiff_exptl_absorpt_empirical_full_min 0.810