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_7000621
_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
'3(C18 H36 K N2 O6), C3 H7 Ge9 Zn, 2(C7 H8), C2 H6 N2'
_chemical_formula_sum            'C73 H139 Ge9 K3 N8 O18 Zn'
_chemical_formula_weight         2252.90
_chemical_name_common            (K-(2,2,2-crypt))3(Ge9Zn(iPr))*en*2tol
_chemical_name_systematic
;
[K-(2,2,2-crypt)]3[Ge9Zn(iPr)]*en*2tol
;
_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                75.4570(10)
_cell_angle_beta                 85.3940(10)
_cell_angle_gamma                69.1790(10)
_cell_formula_units_Z            2
_cell_length_a                   13.86500(10)
_cell_length_b                   15.17060(10)
_cell_length_c                   26.0077(2)
_cell_measurement_temperature    150(2)
_cell_volume                     4949.15(7)
_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_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0261
_diffrn_reflns_av_sigmaI/netI    0.0363
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            43107
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         5.09
_exptl_absorpt_coefficient_mu    3.116
_exptl_absorpt_correction_T_max  0.6040
_exptl_absorpt_correction_T_min  0.3163
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange-yellow
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             2304
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.982
_refine_diff_density_min         -1.214
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     987
_refine_ls_number_reflns         22374
_refine_ls_number_restraints     86
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.048
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0280P)^2^+7.9296P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0791
_refine_ls_wR_factor_ref         0.0838
_reflns_number_gt                18451
_reflns_number_total             22374
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b815122a.txt
_cod_data_source_block           4
_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        4949.15(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7000621