A Heterometallic, Heterovalent CuI/SnII/IV/S Cluster with an Unprecedented Cu4Sn Core and Stannacyclopentane Units
Hari Pada Nayek; Werner Massa; Stefanie Dehnen; Inorganic Chemistry 47 (2008) 9146–9148; doi:10.1021/ic8013877

data_4306564
_publ_contact_author
;
Massa, W.

Fachbereich Chemie der Philipps-Universit\"at
Hans-Meerwein-Str.
D-35043 Marburg, Germany
;
_publ_contact_author_email       massa@chemie.uni-marburg.de
_publ_contact_author_fax         +6421-2828917
_publ_contact_author_phone       +6421-2825525
_publ_section_title
;
A Heterometallic, Heterovalent CuI/SnII/IV/S Cluster with an Unprecedented
Cu4Sn Core and Stannacyclopentane Units
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9146
_journal_page_last               9148
_journal_paper_doi               10.1021/ic8013877
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C132 H138 Cu10 P6 S12 Sn7'
_chemical_formula_sum            'C132 H138 Cu10 P6 S12 Sn7'
_chemical_formula_weight         3761.19
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 115.099(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.6227(5)
_cell_length_b                   22.6814(4)
_cell_length_c                   18.8353(5)
_cell_measurement_reflns_used    21939
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.14
_cell_measurement_theta_min      1.33
_cell_volume                     6817.7(3)
_computing_cell_refinement       'XAREA 1.38 (Stoe 2006)'
_computing_data_collection       'XAREA 1.38 (Stoe 2006)'
_computing_data_reduction        'XAREA 1.38 (Stoe 2006)'
_computing_molecular_graphics    'DIAMOND 3.1d (Crystal Impact 2006)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 6.7
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'IPDS-II (Stoe)'
_diffrn_measurement_method       omega-scans
_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  0.0514
_diffrn_reflns_av_sigmaI/netI    0.0830
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            38108
_diffrn_reflns_theta_full        26.75
_diffrn_reflns_theta_max         26.75
_diffrn_reflns_theta_min         1.33
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.081
_exptl_absorpt_correction_T_max  0.431
_exptl_absorpt_correction_T_min  0.404
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing (1995)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.832
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bipyramid
_exptl_crystal_F_000             3704
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.676
_refine_diff_density_min         -0.644
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.834
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     794
_refine_ls_number_reflns         14367
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.834
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_gt           0.0377
_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^)+(0.0300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0672
_refine_ls_wR_factor_ref         0.0734
_reflns_number_gt                8789
_reflns_number_total             14367
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8013877_si_002.cif
_cod_data_source_block           hp18am
_cod_database_code               4306564