Molecular CHEVREL-like Clusters [(RhPPh3)6(μ3-Se)8] and [Pd6(μ3-Te)8](4.).
Thiele, Günther; You, Zhiliang; Dehnen, Stefanie; Inorganic chemistry 54 (2015) 2491–2493; doi:10.1021/ic502409r

data_4342536
_publ_section_title
;
 Molecular CHEVREL-like Clusters [(RhPPh3)6(\m3-Se)8] and
 [Pd6(\m3-Te)8](4.).
;
_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2491
_journal_page_last               2493
_journal_paper_doi               10.1021/ic502409r
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C108 H90 P6 Rh6 Se8, C H4 N'
_chemical_formula_sum            'C109 H94 N P6 Rh6 Se8'
_chemical_formula_weight         2852.92
_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_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                64.416(3)
_cell_angle_beta                 67.409(3)
_cell_angle_gamma                62.898(3)
_cell_formula_units_Z            1
_cell_length_a                   14.1332(6)
_cell_length_b                   14.5044(6)
_cell_length_c                   15.4160(7)
_cell_measurement_temperature    100(2)
_cell_volume                     2467.3(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.9967
_diffrn_measured_fraction_theta_max 0.9906
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0974
_diffrn_reflns_av_unetI/netI     0.0834
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            31827
_diffrn_reflns_theta_full        26.0000
_diffrn_reflns_theta_max         26.74
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    4.077
_exptl_absorpt_correction_T_max  0.8080
_exptl_absorpt_correction_T_min  0.4622
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'STOE X-AREA'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.9200
_exptl_crystal_description       stick
_exptl_crystal_F_000             1380.6790
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.0885
_refine_diff_density_min         -1.1757
_refine_diff_density_rms         0.1997
_refine_ls_d_res_high            0.7898
_refine_ls_d_res_low             12.2652
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   0.9532
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    106
_refine_ls_number_parameters     633
_refine_ls_number_reflns         10392
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.9532
_refine_ls_R_factor_all          0.0637
_refine_ls_R_factor_gt           0.0417
_refine_ls_shift/su_max          0.0006
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0603P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1016
_refine_ls_wR_factor_ref         0.1098
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              17
_reflns_limit_h_min              -16
_reflns_limit_k_max              18
_reflns_limit_k_min              -16
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                7800
_reflns_number_total             10392
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ic502409r_si_002.cif
_cod_data_source_block           Compound1
_cod_depositor_comments
'Adding full bibliography for 4342536--4342537.cif.'
_cod_database_code               4342536
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
2. Others
 Sof(C47A)=Sof(H47A)=Sof(C48A)=Sof(H48A)=Sof(C50A)=Sof(H50A)=Sof(C51A)=
 Sof(H51A)=1-FVAR(1)
 Sof(C47)=Sof(H47)=Sof(C48)=Sof(H48)=Sof(C50)=Sof(H50)=Sof(C51)=Sof(H51)=FVAR(1)
 Fixed Sof: C100(0.5) H10a(0.5) H10b(0.5) N100(0.5) H10c(0.33333)
 H10d(0.33333) H10e(0.33333)
3.a Secondary CH2 refined with riding coordinates:
 C100(H10a,H10b)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C21(H21), C22(H22),
  C23(H23), C24(H24), C25(H25), C27(H27), C28(H28), C29(H29), C30(H30),
 C31(H31), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37), C41(H41), C42(H42),
  C43(H43), C44(H44), C45(H45), C47(H47), C47A(H47A), C48(H48), C48A(H48A),
 C49(H49), C50(H50), C50A(H50A), C51(H51), C51A(H51A), C53(H53), C54(H54),
 C55(H55), C56(H56), C57(H57)
3.c Idealised Me refined as rotating group:
 N100(H10c,H10d,H10e)
;