Synthesis, crystal structure, and photoluminescence studies of a ruthenocenyl-decorated sn/s cluster.
Leusmann, Eliza; Wagner, Mona; Rosemann, Nils W.; Chatterjee, Sangam; Dehnen, Stefanie; Inorganic chemistry 53 (2014) 4228–4233; doi:10.1021/ic500367y

data_4338089
_publ_section_title
;
 Synthesis, crystal structure, and photoluminescence studies of a
 ruthenocenyl-decorated sn/s cluster.
;
_journal_issue                   8
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4228
_journal_page_last               4233
_journal_paper_doi               10.1021/ic500367y
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C72 H92 N8 Ru4 S10 Sn6'
_chemical_formula_sum            'C72 H92 N8 Ru4 S10 Sn6'
_chemical_formula_weight         2506.55
_chemical_name_systematic        '[(RcAcN=NCMeCH2CMe2Sn)4Sn2S10]'
_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             2013-10-17
_audit_creation_method
;
  Olex2 1.2
  (compiled Dec  5 2012 16:17:34, GUI svn.r4385)
;
_cell_angle_alpha                95.154(6)
_cell_angle_beta                 102.536(5)
_cell_angle_gamma                92.727(6)
_cell_formula_units_Z            1
_cell_length_a                   11.3247(8)
_cell_length_b                   11.4359(8)
_cell_length_c                   21.0917(15)
_cell_measurement_temperature    100.0
_cell_volume                     2649.3(3)
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0990
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            11191
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.71
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    2.173
_exptl_absorpt_correction_T_max  0.8005
_exptl_absorpt_correction_T_min  0.5932
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-RED32; Stoe & Cie, 2002'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.571
_exptl_crystal_description       plate
_exptl_crystal_F_000             1216
_exptl_crystal_recrystallization_method
'reaction solution layered with toluene, darkness, three months'
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.081
_refine_diff_density_min         -1.629
_refine_diff_density_rms         0.173
_refine_ls_extinction_coef       0.0017(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.895
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         11171
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.895
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0472
_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^)+(0.0961P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1319
_refine_ls_wR_factor_ref         0.1357
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7709
_reflns_number_total             11171
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic500367y_si_003.cif
_cod_data_source_block           Compound2
_cod_depositor_comments
'Adding full bibliography for 4338088--4338089.cif.'
_cod_database_code               4338089
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H15 of C15, H18 of C18, H34 of C34, H32 of C32, H36 of C36, H14 of C14, H35
  of C35, H29 of C29, H30 of C30, H28 of C28, H31 of C31, H33 of C33, H17 of
  C17, H16 of C16, {H22A,H22B} of C22, {H4A,H4B} of C4, H12 of C12, H10 of C10,
  H11 of C11, H13 of C13
 At 1.5 times of:
  {H26A,H26B,H26C} of C26, {H6A,H6B,H6C} of C6, {H24A,H24B,H24C} of C24, {H2A,
  H2B,H2C} of C2, {H20A,H20B,H20C} of C20, {H21A,H21B,H21C} of C21, {H8A,H8B,
  H8C} of C8, {H3A,H3B,H3C} of C3
2.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C22(H22A,H22B)
2.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C11(H11), C10(H10), C12(H12), C31(H31), C28(H28), C30(H30),
 C29(H29), C35(H35), C14(H14), C36(H36), C32(H32), C34(H34), C18(H18), C15(H15),
  C33(H33), C17(H17), C16(H16)
2.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C8(H8A,H8B,H8C), C21(H21A,H21B,H21C), C20(H20A,H20B,H20C),
 C2(H2A,H2B,H2C), C24(H24A,H24B,H24C), C6(H6A,H6B,H6C), C26(H26A,H26B,H26C)
;
_shelxl_version_number           2013-3