Bistrimethylsilylamide Transition-Metal Complexes as Starting Reagents in the Synthesis of Ternary Cd-Mn-Se Cluster Complexes
Andreas Eichhöfer; Oliver Hampe; Sergei Lebedkin; Florian Weigend; Inorganic Chemistry 49 (2010) 7331–7339; doi:10.1021/ic100310w

data_4316214
_publ_section_title
;
 Bistrimethylsilylamide Transition-Metal Complexes as Starting Reagents in
 the Synthesis of Ternary Cd-Mn-Se Cluster Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7331
_journal_page_last               7339
_journal_paper_doi               10.1021/ic100310w
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         '[Cd4Mn4S(SeC6H5)14(P(C3H7)3)2]*3C4H10O2'
_chemical_formula_sum            'C114 H141 Cd4 Mn4 O6 P2 S Se14'
_chemical_formula_weight         3476.07
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                95.86(3)
_cell_angle_beta                 91.76(3)
_cell_angle_gamma                112.93(3)
_cell_formula_units_Z            2
_cell_length_a                   14.520(3)
_cell_length_b                   17.857(4)
_cell_length_c                   26.787(5)
_cell_measurement_reflns_used    63307
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      25.60
_cell_measurement_theta_min      1.25
_cell_volume                     6344(3)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0552
_diffrn_reflns_av_sigmaI/netI    0.0516
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            56155
_diffrn_reflns_theta_full        25.15
_diffrn_reflns_theta_max         25.15
_diffrn_reflns_theta_min         1.25
_exptl_absorpt_coefficient_mu    5.148
_exptl_absorpt_correction_T_max  0.4158
_exptl_absorpt_correction_T_min  0.2351
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   STOE-XRED32
_exptl_crystal_colour            'pale red'
_exptl_crystal_density_diffrn    1.820
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3374
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.290
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.693
_refine_diff_density_min         -1.020
_refine_diff_density_rms         0.119
_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     1310
_refine_ls_number_reflns         22545
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0493
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0698P)^2^+6.4619P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1210
_refine_ls_wR_factor_ref         0.1288
_reflns_number_gt                17883
_reflns_number_total             22545
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100310w_si_003.cif
_cod_data_source_block           p-1
_cod_original_cell_volume        6344(2)
_cod_database_code               4316214