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_4301838
_publ_contact_author             'Jose M. Goicoechea'
_publ_contact_author_address
;    
Chemistry Research Laboratory,
University of Oxford,
Mansfield Road, 
Oxford OX1 3TA. UK.
;
_publ_contact_author_email       jose.goicoechea@chem.ox.ac.uk
_publ_contact_author_fax         '+44 1865 272690'
_publ_contact_author_phone       '+44 1865 275961'
_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
'3(C18 H36 K N2 O6), 0.8(C6 H5 Sn9 Cd), 0.2(Sn9), C2 H6 N2'
_chemical_formula_sum            'C61 H120 Cd K3 N8 O18 Sn9'
_chemical_formula_weight         2551.56
_chemical_melting_point          ?
_chemical_name_systematic
; 
[K-(2,2,2-crypt)]3[Sn9Cd(C6H5)]0.8[Sn9]0.2*en
;
_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                91.0976(4)
_cell_angle_beta                 95.6698(4)
_cell_angle_gamma                113.5806(4)
_cell_formula_units_Z            2
_cell_length_a                   15.2071(1)
_cell_length_b                   15.4662(1)
_cell_length_c                   21.4652(2)
_cell_measurement_reflns_used    246605
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      5.097
_cell_volume                     4594.79(6)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Nonius KappaCCD'
_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  0.0241
_diffrn_reflns_av_sigmaI/netI    0.0337
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            31323
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         5.10
_exptl_absorpt_coefficient_mu    2.822
_exptl_absorpt_correction_T_max  0.8489
_exptl_absorpt_correction_T_min  0.3981
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.844
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       rod
_exptl_crystal_F_000             2482
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.668
_refine_diff_density_min         -1.000
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     969
_refine_ls_number_reflns         16029
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0331
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0234P)^2^+13.8290P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0730
_refine_ls_wR_factor_ref         0.0764
_reflns_number_gt                13299
_reflns_number_total             16029
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8022826_si_001_1.cif
_cod_data_source_block           1
_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 

The following automatic conversions were performed:
data name '_contact_author_fax' replaced with
'_publ_contact_author_fax' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 4998 2017-03-02 13:24:31Z antanas 
;
_cod_database_code               4301838