Reductive cleavage of Zn‒C bonds by group 14 Zintl anions: synthesis and characterisation of [E9ZnR]3− (E = Ge, Sn, Pb; R = Mes, iPr)
Zhou, Binbin; Denning, Mark S.; Jones, Carl; Goicoechea, Jose M.; Dalton Transactions  (2009) 1571–1578; doi:10.1039/b815122a

data_7000623
_publ_section_title
;
 Reductive cleavage of Zn--C bonds by group 14 Zintl anions: synthesis
 and characterisation of [E9ZnR]3&#x2212; (E = Ge, Sn, Pb; R = Mes,
 iPr)
;
_journal_issue                   9
_journal_name_full               'Dalton Transactions'
_journal_page_first              1571
_journal_page_last               1578
_journal_paper_doi               10.1039/b815122a
_journal_year                    2009
_chemical_formula_moiety
'6(C18 H36 K N2 O6), 2(C3 H7 Pb9 Zn), C2 H8 N2'
_chemical_formula_sum            'C116 H238 K6 N14 O36 Pb18 Zn2'
_chemical_formula_weight         6498.28
_chemical_name_common            (K-(2,2,2-crypt))6(Pb9Zn(iPr))2*en
_chemical_name_systematic
;
[K-(2,2,2-crypt)]6[Pb9Zn(iPr)]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                112.1484(3)
_cell_angle_beta                 100.0104(3)
_cell_angle_gamma                92.2170(3)
_cell_formula_units_Z            2
_cell_length_a                   14.08810(10)
_cell_length_b                   25.57220(20)
_cell_length_c                   27.13480(20)
_cell_measurement_temperature    100(2)
_cell_volume                     8858.10(12)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0536
_diffrn_reflns_av_sigmaI/netI    0.0650
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            54321
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         5.09
_exptl_absorpt_coefficient_mu    17.501
_exptl_absorpt_correction_T_max  0.3349
_exptl_absorpt_correction_T_min  0.1448
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'dark purple/black'
_exptl_crystal_density_diffrn    2.436
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             5938
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.196
_refine_diff_density_min         -4.999
_refine_diff_density_rms         0.339
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1729
_refine_ls_number_reflns         30777
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0486
_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^)+(0.0779P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1199
_refine_ls_wR_factor_ref         0.1287
_reflns_number_gt                23264
_reflns_number_total             30777
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b815122a.txt
_cod_data_source_block           6
_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 
;
_cod_original_cell_volume        8858.104(116)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7000623