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_7118639
_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 Pt Ru S4 W3, 3(C H Cl3), C7 H7 O3 S'
_chemical_formula_sum            'C65 H97 Cl11 O3 P2 Pt Ru S5 W3'
_chemical_formula_weight         2386.32
_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
_audit_creation_date             2015-06-17
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-10-26 deposited with the CCDC.
2015-11-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.775(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.1025(17)
_cell_length_b                   9.9658(8)
_cell_length_c                   36.424(3)
_cell_measurement_reflns_used    9964
_cell_measurement_temperature    122(2)
_cell_measurement_theta_max      25.66
_cell_measurement_theta_min      2.33
_cell_volume                     8005.7(11)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      122(2)
_diffrn_measured_fraction_theta_full 0.976
_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  0.0985
_diffrn_reflns_av_unetI/netI     0.0609
_diffrn_reflns_laue_measured_fraction_full 0.976
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            119943
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.297
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.799
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5272
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1021 before and 0.0684 after correction. The Ratio of minimum to maximum transmission is 0.7073. The \l/2 correction factor is 0.0000.'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.980
_exptl_crystal_description       Prism
_exptl_crystal_F_000             4608
_exptl_crystal_size_max          0.235
_exptl_crystal_size_mid          0.229
_exptl_crystal_size_min          0.085
_refine_diff_density_max         2.939
_refine_diff_density_min         -1.694
_refine_diff_density_rms         0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     839
_refine_ls_number_reflns         14116
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0814
_refine_ls_R_factor_gt           0.0520
_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^)+(0.0319P)^2^+83.3564P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0977
_refine_ls_wR_factor_ref         0.1056
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10743
_reflns_number_total             14116
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc08918b2.cif
_cod_data_source_block           mo_d8v630_0m-ny
_cod_original_cell_volume        8005.8(11)
_cod_database_code               7118639
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.596
_shelx_estimated_absorpt_t_min   0.298
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C59-C60 \\sim C59A-C60A
 with sigma of 0.002
 C60-C61 \\sim C60A-C61A
 with sigma of 0.002
 C62A-C61A \\sim C62-C61
 with sigma of 0.002
 C59A-C58A \\sim C59-C58
 with sigma of 0.002
 C57A-C62A \\sim C57-C62
 with sigma of 0.002
 C56-C57 \\sim C56A-C57A
 with sigma of 0.002
 C57-C58 \\sim C57A-C58A
 with sigma of 0.002
 S5A-C60A \\sim S5-C60
 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
Uanis(O1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uiso(C56A) = Uiso(C57A) = Uiso(C58A) = Uiso(C59A) = Uiso(C60A) = Uiso(C61A) =
Uiso(C62A)
Uiso(C2A) = Uiso(C3A) = Uiso(C7A) = Uiso(C6A) = Uiso(C5A) = Uiso(C4A)
Uanis(C3) = Uanis(C7) = Uanis(C6) = Uanis(C5) = Uanis(C4)
Uanis(C56) = Uanis(C57) = Uanis(C58) = Uanis(C59) = Uanis(C60) = Uanis(C61) =
Uanis(C62)
4. Others
 Sof(S5A)=Sof(O1A)=Sof(O2A)=Sof(O3A)=Sof(C60A)=Sof(C61A)=Sof(H61A)=Sof(C59A)=
 Sof(H59A)=Sof(C58A)=Sof(H58A)=Sof(C62A)=Sof(H62A)=Sof(C57A)=Sof(C56A)=
 Sof(H56D)=Sof(H56E)=Sof(H56F)=1-FVAR(1)
 Sof(S5)=Sof(O2)=Sof(O3)=Sof(O1)=Sof(C61)=Sof(H61)=Sof(C60)=Sof(C58)=Sof(H58)=
 Sof(C62)=Sof(H62)=Sof(C59)=Sof(H59)=Sof(C57)=Sof(C56)=Sof(H56A)=Sof(H56B)=
 Sof(H56C)=FVAR(1)
 Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=Sof(C3A)=Sof(C7A)=Sof(H7A)=Sof(C6A)=
 Sof(H6A)=Sof(C5A)=Sof(H5A)=Sof(C4A)=Sof(H4A)=1-FVAR(2)
 Sof(C5)=Sof(H5)=Sof(C4)=Sof(H4)=Sof(C7)=Sof(H7)=Sof(C3)=Sof(C6)=Sof(H6)=
 Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=FVAR(2)
 Sof(H46C)=Sof(H46D)=Sof(H47C)=Sof(H47D)=Sof(H44A)=Sof(H49C)=Sof(H49D)=
 Sof(C45A)=Sof(H45C)=Sof(H45D)=Sof(C48A)=Sof(H48C)=Sof(H48D)=1-FVAR(3)
 Sof(H46A)=Sof(H46B)=Sof(H47A)=Sof(H47B)=Sof(H44)=Sof(H49A)=Sof(H49B)=Sof(C45)=
 Sof(H45A)=Sof(H45B)=Sof(C48)=Sof(H48A)=Sof(H48B)=FVAR(3)
5.a Ternary CH refined with riding coordinates:
 C32(H32), C13(H13), C12(H12), C50(H50), C38(H38), C26(H26), C16(H16),
 C10(H10), C19(H19), C20(H20), C4(H4), C18(H18), C17(H17), C11(H11), C44(H44),
 C44(H44A), C7(H7), C63(H63), C65(H65), C6(H6), C64(H64), C7A(H7A), C6A(H6A),
 C5A(H5A), C4A(H4A)
5.b Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C55(H55A,H55B), C37(H37A,H37B), C30(H30A,H30B), C35(H35A,
 H35B), C21(H21A,H21B), C39(H39A,H39B), C33(H33A,H33B), C36(H36A,H36B),
 C46(H46A,H46B), C46(H46C,H46D), C51(H51A,H51B), C28(H28A,H28B), C54(H54A,H54B),
  C47(H47A,H47B), C47(H47C,H47D), C43(H43A,H43B), C22(H22A,H22B), C23(H23A,
 H23B), C27(H27A,H27B), C40(H40A,H40B), C53(H53A,H53B), C34(H34A,H34B),
 C49(H49A,H49B), C49(H49C,H49D), C25(H25A,H25B), C45(H45A,H45B), C29(H29A,H29B),
  C48(H48A,H48B), C42(H42A,H42B), C24(H24A,H24B), C41(H41A,H41B), C52(H52A,
 H52B), C45A(H45C,H45D), C48A(H48C,H48D)
5.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C61(H61), C58(H58), C62(H62), C59(H59), C61A(H61A), C59A(H59A),
 C58A(H58A), C62A(H62A)
5.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C8(H8A,H8B,H8C), C2(H2A,H2B,H2C), C56(H56A,H56B,H56C),
 C56A(H56D,H56E,H56F), C2A(H2AA,H2AB,H2AC)
;
_shelx_res_checksum              95129
_shelx_hkl_checksum              9688
_olex2_submission_special_instructions 'No special instructions were received'