Organozinc Derivatives of Deltahedral Zintl Ions: Synthesis and Characterization ofcloso-[E9Zn(C6H5)]3-(E = Si, Ge, Sn, Pb)
Goicoechea, Jose M.; Sevov, Slavi C.; Organometallics 25 (2006) 4530–; doi:10.1021/om060481g

data_4074228
_publ_section_title
;
 Organozinc Derivatives of Deltahedral Zintl Ions:&#x00A0; Synthesis and
 Characterization ofcloso-[E9Zn(C6H5)]3-(E = Si, Ge, Sn, Pb)
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              4530
_journal_paper_doi               10.1021/om060481g
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety         '3(C18 H36 K N2 O6), C6 H5 Sn9 Zn, C7 H8'
_chemical_formula_sum            'C67 H121 K3 N6 O18 Sn9 Zn'
_chemical_formula_weight         2549.58
_chemical_name_systematic
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 (K-crypt)3[Sn9Zn(C6H5)]*tol
;
_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                 94.295(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.6322(4)
_cell_length_b                   24.4665(8)
_cell_length_c                   28.0370(9)
_cell_measurement_temperature    100(2)
_cell_volume                     9325.0(5)
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004; Sheldrick, 2003)'
_computing_molecular_graphics    'XP (Sheldrick, 1998)'
_computing_publication_material  'XCIF (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0423
_diffrn_reflns_av_sigmaI/netI    0.0324
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            292407
_diffrn_reflns_theta_full        34.45
_diffrn_reflns_theta_max         34.45
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    2.812
_exptl_absorpt_correction_T_max  0.7290
_exptl_absorpt_correction_T_min  0.3847
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Blessing, R.H. (1995) Acta Cryst. A51, 33-38'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.816
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       brick
_exptl_crystal_F_000             4984
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.12
_refine_diff_density_max         3.260
_refine_diff_density_min         -2.786
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     938
_refine_ls_number_reflns         39255
_refine_ls_number_restraints     564
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0371
_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^)+(0.0102P)^2^+34.8546P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0658
_refine_ls_wR_factor_ref         0.0754
_reflns_number_gt                30153
_reflns_number_total             39255
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060481gsi20060726_034836.cif
_cod_data_source_block           '[Sn9ZnPh]3-'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4074228