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_7118636
_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 Mo3 P2 Pd Ru S4, C37 H65.77 Cl5 P2 Pd Ru, C H Cl3, C2.19 H4.56 Cl1.81 O0.4'
_chemical_formula_sum
'C95.19 H158.44 Cl11.82 Mo3 O0.39 P4 Pd2 Ru2 S4'
_chemical_formula_weight         2682.91
_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
_audit_creation_date             2015-10-21
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2015-10-26 deposited with the CCDC.
2015-11-18 downloaded from the CCDC.
;
_cell_angle_alpha                80.217(2)
_cell_angle_beta                 75.331(2)
_cell_angle_gamma                84.330(3)
_cell_formula_units_Z            2
_cell_length_a                   13.8281(9)
_cell_length_b                   17.5883(11)
_cell_length_c                   23.8941(16)
_cell_measurement_reflns_used    9519
_cell_measurement_temperature    122(2)
_cell_measurement_theta_max      29.54
_cell_measurement_theta_min      2.53
_cell_volume                     5530.7(6)
_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_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  0.0605
_diffrn_reflns_av_unetI/netI     0.0375
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            125278
_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         25.681
_diffrn_reflns_theta_min         2.248
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.374
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6521
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/3 (Bruker,2014/3) was used for absorption correction. wR2(int) was 0.1221 before and 0.0584 after correction. The Ratio of minimum to maximum transmission is 0.8742. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_description       plate
_exptl_crystal_F_000             2727
_exptl_crystal_size_max          0.279
_exptl_crystal_size_mid          0.264
_exptl_crystal_size_min          0.142
_refine_diff_density_max         2.244
_refine_diff_density_min         -1.827
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1132
_refine_ls_number_reflns         20984
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0314
_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^)+(0.0257P)^2^+8.7618P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0630
_refine_ls_wR_factor_ref         0.0686
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16923
_reflns_number_total             20984
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc08918b2.cif
_cod_data_source_block           mo_d8v972_0m-ny
_cod_database_code               7118636
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.829
_shelx_estimated_absorpt_t_min   0.701
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H94a,H94b,H94} of C94, All C(H,H) groups, All C(H,H,H,H)
  groups
 At 1.5 times of:
  {H15a,H15b,H15c} of C15, {H3a,H3b,H3c} of C3, {H95a,H95b,H95c} of C95,
  {H97a,H97b,H97c} of C97, {H9a,H9b,H9c} of C9
2. Uiso/Uaniso restraints and constraints
Uanis(C4) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C95) = Uanis(O1) = Uanis(C96) = Uanis(C97)
3. Others
 Sof(H94a)=Sof(H94b)=Sof(O1)=Sof(C96)=Sof(H96a)=Sof(H96b)=Sof(C97)=Sof(H97a)=
 Sof(H97b)=Sof(H97c)=Sof(C95)=Sof(H95a)=Sof(H95b)=Sof(H95c)=1-FVAR(1)
 Sof(Cl12)=Sof(Cl11)=Sof(Cl13)=Sof(H94)=FVAR(1)
 Sof(H69a)=Sof(H72c)=Sof(H72d)=Sof(H70c)=Sof(H70d)=Sof(C74A)=Sof(H74c)=
 Sof(H74d)=Sof(C71A)=Sof(H71c)=Sof(H71d)=1-FVAR(2)
 Sof(H73a)=Sof(H73b)=Sof(C74)=Sof(H74a)=Sof(H74b)=Sof(H69)=Sof(H72a)=Sof(H72b)=
 Sof(H70a)=Sof(H70b)=Sof(C71)=Sof(H71a)=Sof(H71b)=FVAR(2)
4.a Ternary CH refined with riding coordinates:
 C39(H39), C75(H75), C87(H87), C69(H69), C69(H69a), C33(H33), C8(H8), C57(H57),
  C13(H13), C93(H93), C51(H51), C21(H21), C7(H7), C63(H63), C27(H27), C19(H19),
 C5(H5), C45(H45), C17(H17), C81(H81), C18(H18), C94(H94), C20(H20), C11(H11),
 C6(H6), C12(H12), C14(H14)
4.b Secondary CH2 refined with riding coordinates:
 C28(H28a,H28b), C48(H48a,H48b), C29(H29a,H29b), C60(H60a,H60b), C64(H64a,
 H64b), C61(H61a,H61b), C68(H68a,H68b), C73(H73a,H73b), C79(H79a,H79b),
 C74(H74a,H74b), C77(H77a,H77b), C86(H86a,H86b), C49(H49a,H49b), C59(H59a,H59b),
  C38(H38a,H38b), C66(H66a,H66b), C83(H83a,H83b), C88(H88a,H88b), C62(H62a,
 H62b), C30(H30a,H30b), C56(H56a,H56b), C47(H47a,H47b), C80(H80a,H80b),
 C78(H78a,H78b), C72(H72c,H72d), C72(H72a,H72b), C76(H76a,H76b), C85(H85a,H85b),
  C37(H37a,H37b), C31(H31a,H31b), C23(H23a,H23b), C50(H50a,H50b), C22(H22a,
 H22b), C92(H92a,H92b), C52(H52a,H52b), C24(H24a,H24b), C91(H91a,H91b),
 C90(H90a,H90b), C34(H34a,H34b), C53(H53a,H53b), C84(H84a,H84b), C70(H70a,H70b),
  C70(H70c,H70d), C36(H36a,H36b), C46(H46a,H46b), C58(H58a,H58b), C32(H32a,
 H32b), C54(H54a,H54b), C55(H55a,H55b), C82(H82a,H82b), C89(H89a,H89b),
 C26(H26a,H26b), C35(H35a,H35b), C25(H25a,H25b), C41(H41a,H41b), C67(H67a,H67b),
  C94(H94a,H94b), C43(H43a,H43b), C40(H40a,H40b), C44(H44a,H44b), C71(H71a,
 H71b), C42(H42a,H42b), C65(H65a,H65b), C96(H96a,H96b), C74A(H74c,H74d),
 C71A(H71c,H71d)
4.c Idealised Me refined as rotating group:
 C9(H9a,H9b,H9c), C15(H15a,H15b,H15c), C3(H3a,H3b,H3c), C97(H97a,H97b,H97c),
 C95(H95a,H95b,H95c)
;
_shelx_res_checksum              76261
_shelx_hkl_checksum              9267
_olex2_submission_special_instructions 'No special instructions were received'