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_7118637
_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 Pt Ru S4, 3(C H Cl3), C7 H7 O3 S'
_chemical_formula_sum            'C65 H97 Cl11 Mo3 O3 P2 Pt Ru S5'
_chemical_formula_weight         2122.59
_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             2015-06-18
_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                 93.738(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.0554(19)
_cell_length_b                   9.9627(9)
_cell_length_c                   36.388(3)
_cell_measurement_reflns_used    9810
_cell_measurement_temperature    122(2)
_cell_measurement_theta_max      26.45
_cell_measurement_theta_min      2.24
_cell_volume                     7978.6(12)
_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 0.976
_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  0.0701
_diffrn_reflns_av_unetI/netI     0.0540
_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       -26
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            107771
_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         2.244
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.972
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5753
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1047 before and 0.0591 after correction.
The Ratio of minimum to maximum transmission is 0.7717.
The \l/2 correction factor is 0.0000.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.767
_exptl_crystal_description       Prism
_exptl_crystal_F_000             4224
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.189
_refine_diff_density_min         -1.243
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     884
_refine_ls_number_reflns         14078
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_gt           0.0553
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+69.7287P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1049
_refine_ls_wR_factor_ref         0.1117
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11168
_reflns_number_total             14078
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc08918b2.cif
_cod_data_source_block           mo_d8v726_0m-ny
_cod_original_cell_volume        7978.5(12)
_cod_database_code               7118637
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.797
_shelx_estimated_absorpt_t_min   0.383
_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
 C61-C60 \\sim C61A-C60A
 with sigma of 0.002
 C60-C59 \\sim C60A-C59A
 with sigma of 0.002
 C61A-C62A \\sim C61-C62
 with sigma of 0.002
 C58-C59 \\sim C58A-C59A
 with sigma of 0.002
 C57A-C62A \\sim C57-C62
 with sigma of 0.002
 C57-C58 \\sim C57A-C58A
 with sigma of 0.002
 C57A-C56A \\sim C57-C56
 with sigma of 0.002
 S5-C60 \\sim S5A-C60A
 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
Uanis(C4) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(O2)
\\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O3A) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C9) \\sim Ueq, Uanis(C13) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.1
Uiso(C56A) = Uiso(C57A) = Uiso(C62A) = Uiso(C58A) = Uiso(C59A) = Uiso(C61A) =
Uiso(C60A)
Uanis(C57) = Uanis(C56) = Uanis(C62) = Uanis(C58) = Uanis(C61) = Uanis(C60) =
Uanis(C59)
4. Others
 Sof(O2A)=Sof(O3A)=Sof(O1A)=Sof(S5A)=Sof(C60A)=Sof(C59A)=Sof(H59A)=Sof(C61A)=
 Sof(H61A)=Sof(C62A)=Sof(H62A)=Sof(C58A)=Sof(H58A)=Sof(C57A)=Sof(C56A)=
 Sof(H56D)=Sof(H56E)=Sof(H56F)=1-FVAR(1)
 Sof(S5)=Sof(O1)=Sof(O3)=Sof(O2)=Sof(C59)=Sof(H59)=Sof(C60)=Sof(C62)=Sof(H62)=
 Sof(C58)=Sof(H58)=Sof(C61)=Sof(H61)=Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(H56C)=
 Sof(C57)=FVAR(1)
 Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=Sof(C9A)=Sof(C12A)=Sof(H12A)=Sof(C10A)=
 Sof(H10A)=Sof(C11A)=Sof(H11A)=Sof(H13A)=1-FVAR(2)
 Sof(C10)=Sof(H10)=Sof(C12)=Sof(H12)=Sof(C9)=Sof(C11)=Sof(H11)=Sof(C8)=
 Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(H13)=FVAR(2)
 Sof(H26A)=Sof(H28C)=Sof(H28D)=Sof(H29C)=Sof(H29D)=Sof(H31C)=Sof(H31D)=
 Sof(C30A)=Sof(H30C)=Sof(H30D)=Sof(C27A)=Sof(H27C)=Sof(H27D)=1-FVAR(3)
 Sof(H26)=Sof(H28A)=Sof(H28B)=Sof(H29A)=Sof(H29B)=Sof(C27)=Sof(H27A)=Sof(H27B)=
 Sof(H31A)=Sof(H31B)=Sof(C30)=Sof(H30A)=Sof(H30B)=FVAR(3)
5.a Ternary CH refined with riding coordinates:
 C50(H50), C16(H16), C63(H63), C5(H5), C32(H32), C6(H6), C38(H38), C10(H10),
 C64(H64), C44(H44), C4(H4), C18(H18), C12(H12), C17(H17), C11(H11), C26(H26),
 C26(H26A), C20(H20), C65(H65), C19(H19), C7(H7), C12A(H12A), C10A(H10A),
 C11A(H11A), C13(H13), C13(H13A)
5.b Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C43(H43A,H43B), C46(H46A,H46B), C39(H39A,H39B), C37(H37A,
 H37B), C49(H49A,H49B), C51(H51A,H51B), C53(H53A,H53B), C48(H48A,H48B),
 C42(H42A,H42B), C35(H35A,H35B), C34(H34A,H34B), C55(H55A,H55B), C45(H45A,H45B),
  C47(H47A,H47B), C36(H36A,H36B), C40(H40A,H40B), C41(H41A,H41B), C52(H52A,
 H52B), C54(H54A,H54B), C25(H25A,H25B), C24(H24A,H24B), C28(H28A,H28B),
 C28(H28C,H28D), C29(H29A,H29B), C29(H29C,H29D), C27(H27A,H27B), C31(H31A,H31B),
  C31(H31C,H31D), C21(H21A,H21B), C30(H30A,H30B), C22(H22A,H22B), C23(H23A,
 H23B), C30A(H30C,H30D), C27A(H27C,H27D)
5.c Aromatic/amide H refined with riding coordinates:
 C59(H59), C62(H62), C58(H58), C61(H61), C59A(H59A), C61A(H61A), C62A(H62A),
 C58A(H58A)
5.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C2(H2A,H2B,H2C), C8(H8A,H8B,H8C), C56(H56A,H56B,H56C),
 C56A(H56D,H56E,H56F), C8A(H8AA,H8AB,H8AC)
;
_shelx_res_checksum              92870
_shelx_hkl_checksum              69522
_olex2_submission_special_instructions 'No special instructions were received'