Delivering carbide ligands to sulfide-rich clusters.
Reinholdt, Anders; Herbst, Konrad; Bendix, Jesper; Chemical communications (Cambridge, England) 52 (2016) 2015–2018; doi:10.1039/c5cc08918b

data_7118638
_publ_section_title
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 Delivering carbide ligands to sulfide-rich clusters.
;
_journal_issue                   10
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2015
_journal_page_last               2018
_journal_paper_doi               10.1039/c5cc08918b
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety
'C55 H87 Cl2 P2 Pd Ru S4 W3, C37 H66 Cl5 P2 Pd Ru, 1.78(C H Cl3), 0.22(C4 O)'
_chemical_formula_sum
'C94.65 H154.79 Cl12.35 O0.22 P4 Pd2 Ru2 S4 W3'
_chemical_formula_weight         2952.62
_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             2015-06-16
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
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2015-10-26 deposited with the CCDC.
2015-11-18 downloaded from the CCDC.
;
_cell_angle_alpha                80.2950(10)
_cell_angle_beta                 75.2550(10)
_cell_angle_gamma                83.9490(10)
_cell_formula_units_Z            2
_cell_length_a                   13.8702(4)
_cell_length_b                   17.6143(5)
_cell_length_c                   23.8397(8)
_cell_measurement_reflns_used    9876
_cell_measurement_temperature    122(2)
_cell_measurement_theta_max      28.64
_cell_measurement_theta_min      2.54
_cell_volume                     5540.0(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      122(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            84030
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         2.173
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.156
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6477
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0658 before and 0.0513 after correction. The Ratio of minimum to maximum transmission is 0.8685. The \l/2 correction factor is 0.0000.'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.770
_exptl_crystal_description       Rod
_exptl_crystal_F_000             2921
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         3.397
_refine_diff_density_min         -2.140
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1119
_refine_ls_number_reflns         21806
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0359
_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^)+(0.0235P)^2^+37.4360P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0755
_refine_ls_wR_factor_ref         0.0839
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17617
_reflns_number_total             21806
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc08918b2.cif
_cod_data_source_block           mo_d8v200_0m-ny
_cod_database_code               7118638
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.851
_shelx_estimated_absorpt_t_min   0.732
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C97-C98 \\sim C96-C95
 with sigma of 0.002
 O1-C95 \\sim O1-C97
 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uiso(C96) = Uiso(C95) = Uiso(O1) = Uiso(C97) = Uiso(C98)
4. Others
 Sof(Cl11)=Sof(Cl12)=Sof(Cl13)=Sof(C94)=Sof(H94)=1-FVAR(1)
 Sof(C96)=Sof(O1)=Sof(C98)=Sof(C97)=Sof(C95)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C51(H51), C87(H87), C57(H57), C93(H93), C69(H69), C63(H63), C81(H81),
 C39(H39), C75(H75), C45(H45), C12(H12), C20(H20), C11(H11), C19(H19), C14(H14),
  C8(H8), C33(H33), C13(H13), C5(H5), C21(H21), C27(H27), C7(H7), C6(H6),
 C18(H18), C17(H17), C94(H94)
5.b Secondary CH2 refined with riding coordinates:
 C88(H88A,H88B), C89(H89A,H89B), C56(H56A,H56B), C60(H60A,H60B), C77(H77A,
 H77B), C82(H82A,H82B), C49(H49A,H49B), C76(H76A,H76B), C68(H68A,H68B),
 C54(H54A,H54B), C61(H61A,H61B), C72(H72A,H72B), C73(H73A,H73B), C65(H65A,H65B),
  C90(H90A,H90B), C79(H79A,H79B), C55(H55A,H55B), C58(H58A,H58B), C92(H92A,
 H92B), C80(H80A,H80B), C74(H74A,H74B), C59(H59A,H59B), C47(H47A,H47B),
 C66(H66A,H66B), C48(H48A,H48B), C70(H70A,H70B), C62(H62A,H62B), C50(H50A,H50B),
  C46(H46A,H46B), C71(H71A,H71B), C64(H64A,H64B), C52(H52A,H52B), C85(H85A,
 H85B), C91(H91A,H91B), C53(H53A,H53B), C67(H67A,H67B), C86(H86A,H86B),
 C83(H83A,H83B), C78(H78A,H78B), C84(H84A,H84B), C42(H42A,H42B), C38(H38A,H38B),
  C40(H40A,H40B), C28(H28A,H28B), C41(H41A,H41B), C43(H43A,H43B), C44(H44A,
 H44B), C32(H32A,H32B), C34(H34A,H34B), C26(H26A,H26B), C31(H31A,H31B),
 C37(H37A,H37B), C29(H29A,H29B), C35(H35A,H35B), C30(H30A,H30B), C22(H22A,H22B),
  C24(H24A,H24B), C36(H36A,H36B), C23(H23A,H23B), C25(H25A,H25B)
5.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C15(H15A,H15B,H15C), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              3566
_shelx_hkl_checksum              79314
_olex2_submission_special_instructions 'No special instructions were received'