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_7118641
_publ_section_title
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 Delivering carbide ligands to sulfide-rich clusters.
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_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_absolute_configuration ad
_chemical_formula_moiety
'C43 H78 Ag Cl2 P2 Ru S3, C F3 O3 S, C2.92 H6.77 Cl1.08 O0.64'
_chemical_formula_sum            'C46.92 H84.77 Ag Cl3.08 F3 O3.64 P2 Ru S4'
_chemical_formula_weight         1272.44
_chemical_name_systematic
;
 ?
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_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-10-21
_audit_creation_method
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Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
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_audit_update_record
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2015-10-26 deposited with the CCDC.
2015-11-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5010(4)
_cell_length_b                   22.3773(10)
_cell_length_c                   27.2642(11)
_cell_measurement_reflns_used    9990
_cell_measurement_temperature    122(2)
_cell_measurement_theta_max      24.09
_cell_measurement_theta_min      2.27
_cell_volume                     5796.6(4)
_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 0.976
_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  0.1039
_diffrn_reflns_av_unetI/netI     0.0639
_diffrn_reflns_laue_measured_fraction_full 0.976
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            61707
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.270
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.987
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6588
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014/3) was used for absorption correction.
wR2(int) was 0.0747 before and 0.0648 after correction.
The Ratio of minimum to maximum transmission is 0.8837.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_description       rod
_exptl_crystal_F_000             2639
_exptl_crystal_size_max          0.159
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.068
_refine_diff_density_max         1.087
_refine_diff_density_min         -0.580
_refine_diff_density_rms         0.101
_refine_ls_abs_structure_details
;
 Flack x determined using 3198 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.321(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     633
_refine_ls_number_reflns         10245
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0442
_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^)+(0.0311P)^2^+8.4829P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0823
_refine_ls_wR_factor_ref         0.0919
_reflns_Friedel_coverage         0.796
_reflns_friedel_fraction_full    0.975
_reflns_friedel_fraction_max     1.000
_reflns_number_gt                8283
_reflns_number_total             10245
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc08918b2.cif
_cod_data_source_block           mo_d8v651_0m-ny
_cod_database_code               7118641
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.936
_shelx_estimated_absorpt_t_min   0.859
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H46,H46a,H46b} of C46, All C(H,H) groups
 At 1.5 times of:
  {H45a,H45b,H45c} of C45, {H48a,H48b,H48c} of C48
2. Uiso/Uaniso restraints and constraints
Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(F2) \\sim Ueq, Uanis(F3A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(F1) \\sim Ueq, Uanis(F2A) \\sim Ueq, Uanis(F3) \\sim Ueq: with sigma of
0.002 and sigma for terminal atoms of 0.004
Uanis(C27) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C16) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C48) = Uanis(C47) = Uanis(O4) = Uanis(C46) = Uanis(C45)
3. Others
 Sof(Cl4)=Sof(Cl3)=Sof(Cl5)=Sof(H46)=1-FVAR(1)
 Sof(O4)=Sof(C48)=Sof(H48a)=Sof(H48b)=Sof(H48c)=Sof(C45)=Sof(H45a)=Sof(H45b)=
 Sof(H45c)=Sof(C47)=Sof(H47a)=Sof(H47b)=Sof(H46a)=Sof(H46b)=FVAR(1)
 Sof(F1)=Sof(F3)=Sof(F2)=1-FVAR(2)
 Sof(F1A)=Sof(F3A)=Sof(F2A)=FVAR(2)
 Sof(O3)=Sof(O1)=Sof(O2)=1-FVAR(3)
 Sof(O3A)=Sof(O2A)=Sof(O1A)=FVAR(3)
4.a Ternary CH refined with riding coordinates:
 C14(H14), C8(H8), C20(H20), C26(H26), C38(H38), C32(H32), C46(H46)
4.b Secondary CH2 refined with riding coordinates:
 C15(H15a,H15b), C13(H13a,H13b), C12(H12a,H12b), C11(H11a,H11b), C10(H10a,
 H10b), C9(H9a,H9b), C21(H21a,H21b), C25(H25a,H25b), C31(H31a,H31b), C30(H30a,
 H30b), C27(H27a,H27b), C43(H43a,H43b), C39(H39a,H39b), C33(H33a,H33b),
 C37(H37a,H37b), C18(H18a,H18b), C36(H36a,H36b), C17(H17a,H17b), C29(H29a,H29b),
  C19(H19a,H19b), C28(H28a,H28b), C34(H34a,H34b), C7(H7a,H7b), C16(H16a,H16b),
 C6(H6a,H6b), C41(H41a,H41b), C24(H24a,H24b), C35(H35a,H35b), C2(H2a,H2b),
 C40(H40a,H40b), C23(H23a,H23b), C22(H22a,H22b), C5(H5a,H5b), C42(H42a,H42b),
 C3(H3a,H3b), C4(H4a,H4b), C47(H47a,H47b), C46(H46a,H46b)
4.c Idealised Me refined as rotating group:
 C48(H48a,H48b,H48c), C45(H45a,H45b,H45c)
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_shelx_res_checksum              40234
_shelx_hkl_checksum              98163
_olex2_submission_special_instructions 'No special instructions were received'