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_4074229
_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 Pb9 Zn, 0.5(C7 H8), C2 H8 N2'
_chemical_formula_sum            'C65.5 H125 K3 N8 O18 Pb9 Zn'
_chemical_formula_weight         3360.11
_chemical_name_systematic
; 
 (K-crypt)6[Pb9Zn(C6H5)]2*2en*tol
;
_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                87.793(2)
_cell_angle_beta                 74.942(2)
_cell_angle_gamma                89.428(2)
_cell_formula_units_Z            4
_cell_length_a                   15.8267(4)
_cell_length_b                   22.4460(7)
_cell_length_c                   27.5057(8)
_cell_measurement_temperature    100(2)
_cell_volume                     9428.8(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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0781
_diffrn_reflns_av_sigmaI/netI    0.0570
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            252039
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         0.77
_exptl_absorpt_coefficient_mu    16.447
_exptl_absorpt_correction_T_max  0.2429
_exptl_absorpt_correction_T_min  0.0493
_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    2.367
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       brick
_exptl_crystal_F_000             6172
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         3.555
_refine_diff_density_min         -3.788
_refine_diff_density_rms         0.295
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1883
_refine_ls_number_reflns         33188
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0416
_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^)+(0.0619P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1011
_refine_ls_wR_factor_ref         0.1090
_reflns_number_gt                25459
_reflns_number_total             33188
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060481gsi20060726_034836.cif
_cod_data_source_block           '[Pb9ZnPh]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_values 1715 2011-07-08 13:25:40Z adriana 

2026-02-27
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C131 H250 K6 N16 O36 Pb18 Zn2'
_cod_original_formula_weight         6720.23
_cod_original_formula_moiety
'6(C18 H36 K N2 O6), 2(C6 H5 Pb9 Zn), C7 H8, 2(C2 H8 N2)'
_cod_original_formula_units_Z            2
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4074229