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_7118640
_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
'C43 H78 Cl2 Cu P2 Ru S3, C H Cl3, B F4, 1.5(C2 H5 O0.5)'
_chemical_formula_sum            'C47 H86.5 B Cl5 Cu F4 O0.75 P2 Ru S3'
_chemical_formula_weight         1250.45
_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                91.100(14)
_cell_angle_beta                 97.986(16)
_cell_angle_gamma                99.976(12)
_cell_formula_units_Z            2
_cell_length_a                   9.636(3)
_cell_length_b                   17.256(5)
_cell_length_c                   18.491(7)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    122(2)
_cell_measurement_theta_max      0.000
_cell_measurement_theta_min      0.000
_cell_volume                     2995.9(17)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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 0.979
_diffrn_measured_fraction_theta_max 0.981
_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  0.0327
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_laue_measured_fraction_full 0.979
_diffrn_reflns_laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            42665
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.878
_diffrn_reflns_theta_min         2.227
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.032
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.7055
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/3 (Bruker,2014/3) was used for absorption correction. wR2(int) was 0.0545 before and 0.0429 after correction. The Ratio of minimum to maximum transmission is 0.9455. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_description       prism
_exptl_crystal_F_000             1303
_exptl_crystal_size_max          0.274
_exptl_crystal_size_mid          0.243
_exptl_crystal_size_min          0.206
_refine_diff_density_max         2.372
_refine_diff_density_min         -1.770
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         14016
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0547
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0887P)^2^+8.5581P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1475
_refine_ls_wR_factor_ref         0.1593
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11571
_reflns_number_total             14016
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc08918b2.cif
_cod_data_source_block           sortextsort15093214-1
_cod_original_cell_volume        2995.8(16)
_cod_original_formula_sum        'C47 H86.50 B Cl5 Cu F4 O0.75 P2 Ru S3'
_cod_database_code               7118640
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.816
_shelx_estimated_absorpt_t_min   0.765
_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. Uiso/Uaniso restraints and constraints
Uanis(C108) \\sim Ueq, Uanis(C109) \\sim Ueq, Uanis(C110) \\sim Ueq,
Uanis(C111) \\sim Ueq, Uanis(C112) \\sim Ueq, Uanis(C113) \\sim Ueq: with sigma
of 0.02 and sigma for terminal atoms of 0.01
Uanis(C142) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.005
Uanis(C108) = Uanis(C109) = Uanis(C110) = Uanis(C111) = Uanis(C112) =
Uanis(C113)
Uanis(C50) = Uanis(C49) = Uanis(O2)
3. Others
 Sof(C108)=Sof(H108)=Sof(C109)=Sof(H10C)=Sof(H10D)=Sof(C110)=Sof(H11C)=
 Sof(H11D)=Sof(C111)=Sof(H11E)=Sof(H11F)=Sof(C112)=Sof(H11G)=Sof(H11H)=
 Sof(C113)=Sof(H11I)=Sof(H11J)=1-FVAR(1)
 Sof(C8)=Sof(H8)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(C9)=Sof(H9A)=Sof(H9B)=
 Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(C10)=Sof(H10A)=
 Sof(H10B)=FVAR(1)
 Sof(C143)=Sof(H14A)=Sof(H14B)=Sof(C142)=Sof(H14C)=Sof(H14D)=1-FVAR(2)
 Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(C42)=Sof(H42A)=Sof(H42B)=FVAR(2)
 Sof(C141)=Sof(H14E)=Sof(H14F)=Sof(C140)=Sof(H14G)=Sof(H14H)=Sof(S102)=
 Sof(C139)=Sof(H13C)=Sof(H13D)=Sof(C138)=Sof(H13E)=Sof(H13F)=1-FVAR(3)
 Sof(S2)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(C41)=
 Sof(H41A)=Sof(H41B)=Sof(C40)=Sof(H40A)=Sof(H40B)=FVAR(3)
 Fixed Sof: O1(0.5) C45(0.5) H45A(0.5) H45B(0.5) C46(0.5) H46A(0.5) H46B(0.5)
 H46C(0.5) C47(0.5) H47A(0.25) H47B(0.25) H47C(0.25) H47D(0.25) O2(0.25)
 C49(0.5) H49A(0.5) H49B(0.5) C50(0.5) H50A(0.5) H50B(0.5) H50C(0.5) C148(0.25)
 H14I(0.25) H14J(0.25) H14K(0.25) C48(0.25) H48A(0.25) H48B(0.25) H48C(0.25)
4.a Ternary CH refined with riding coordinates:
 C26(H26), C32(H32), C8(H8), C20(H20), C14(H14), C2(H2), C44(H44), C108(H108)
4.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C19(H19A,H19B), C23(H23A,H23B), C27(H27A,H27B), C37(H37A,
 H37B), C17(H17A,H17B), C29(H29A,H29B), C33(H33A,H33B), C3(H3A,H3B), C31(H31A,
 H31B), C7(H7A,H7B), C5(H5A,H5B), C16(H16A,H16B), C18(H18A,H18B), C28(H28A,
 H28B), C30(H30A,H30B), C36(H36A,H36B), C21(H21A,H21B), C22(H22A,H22B),
 C24(H24A,H24B), C35(H35A,H35B), C6(H6A,H6B), C34(H34A,H34B), C25(H25A,H25B),
 C4(H4A,H4B), C45(H45A,H45B), C47(H47A,H47B), C47(H47C,H47D), C49(H49A,H49B),
 C13(H13A,H13B), C9(H9A,H9B), C12(H12A,H12B), C11(H11A,H11B), C10(H10A,H10B),
 C109(H10C,H10D), C110(H11C,H11D), C111(H11E,H11F), C112(H11G,H11H), C113(H11I,
 H11J), C43(H43A,H43B), C42(H42A,H42B), C143(H14A,H14B), C142(H14C,H14D),
 C38(H38A,H38B), C39(H39A,H39B), C41(H41A,H41B), C40(H40A,H40B), C141(H14E,
 H14F), C140(H14G,H14H), C139(H13C,H13D), C138(H13E,H13F)
4.c Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C50(H50A,H50B,H50C), C148(H14I,H14J,H14K), C48(H48A,H48B,
 H48C)
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_shelx_res_checksum              65766
_shelx_hkl_checksum              79939
_olex2_submission_special_instructions 'No special instructions were received'