Coupling Reactions of Functionalized Zintl Ions [E9Cd(C6H5)]3- (E = Sn, Pb) with Tributyltinhydride: Synthesis and Isolation of {Sn9CdSn[(CH2)3CH3]3}3-
Binbin Zhou; Mark S. Denning; Thomas A. D. Chapman; Jose M. Goicoechea; Inorganic Chemistry 48 (2009) 2899–2907; doi:10.1021/ic8022826

data_4301840
_publ_section_title
;
Coupling Reactions of Functionalized Zintl Ions [E9Cd(C6H5)]3- (E = Sn,
Pb) with Tributyltinhydride: Synthesis and Isolation of
{Sn9CdSn[(CH2)3CH3]3}3-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2899
_journal_page_last               2907
_journal_paper_doi               10.1021/ic8022826
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety
'2(C12 H27 Sn10 Cd), 6(C18 H36 K N2 O6), 7(C7H8), C5 H5 N'
_chemical_formula_sum            'C179 H323 Cd2 K6 N13 O36 Sn20'
_chemical_formula_weight         6066.70
_chemical_melting_point          ?
_chemical_name_systematic
; 
[K-(2,2,2-crypt)]6[Sn9CdSn(C4H9)3]2*6tol*py
;
_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                78.8039(2)
_cell_angle_beta                 75.0316(2)
_cell_angle_gamma                76.5925(3)
_cell_formula_units_Z            2
_cell_length_a                   15.5506(1)
_cell_length_b                   28.2557(2)
_cell_length_c                   28.9528(2)
_cell_measurement_reflns_used    52691
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      5.097
_cell_volume                     11832.36(14)
_computing_cell_refinement
;
KappaCCD software "DENZO" (Otwinowski & Minor, 1996)
;
_computing_data_collection
;
KappaCCD software "Collect" (Nonius, 2000)
;
_computing_data_reduction
;
KappaCCD software "DENZO" (Otwinowski & Minor, 1996)
;
_computing_molecular_graphics    'WinGX (Farrugia, 2005)'
_computing_publication_material  'XCIF (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phi and 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  0.0540
_diffrn_reflns_av_sigmaI/netI    0.0746
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            100829
_diffrn_reflns_theta_full        27.59
_diffrn_reflns_theta_max         27.59
_diffrn_reflns_theta_min         5.12
_exptl_absorpt_coefficient_mu    2.409
_exptl_absorpt_correction_T_max  0.8689
_exptl_absorpt_correction_T_min  0.4102
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.703
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       plate
_exptl_crystal_F_000             5972
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.885
_refine_diff_density_min         -1.980
_refine_diff_density_rms         0.156
_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     2106
_refine_ls_number_reflns         53966
_refine_ls_number_restraints     235
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1001
_refine_ls_R_factor_gt           0.0523
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0648P)^2^+13.5499P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1278
_refine_ls_wR_factor_ref         0.1519
_reflns_number_gt                33105
_reflns_number_total             53966
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8022826_si_001_3.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        11832.37(14)
_cod_database_code               4301840