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_7000619
_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), C9 H11 Ge9 Zn'
_chemical_formula_sum            'C63 H119 Ge9 K3 N6 O18 Zn'
_chemical_formula_weight         2084.62
_chemical_name_common            (K-(2,2,2-crypt))3(Ge9Zn(C9H11))
_chemical_name_systematic
;
[K-(2,2,2-crypt)]3[Ge9Zn(C9H11)]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.0000
_cell_angle_beta                 98.0425(3)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   17.38970(10)
_cell_length_b                   22.46850(20)
_cell_length_c                   22.09430(20)
_cell_measurement_temperature    150(2)
_cell_volume                     8547.79(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      150(2)
_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  0.0285
_diffrn_reflns_av_sigmaI/netI    0.0376
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            29330
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         5.11
_exptl_absorpt_coefficient_mu    3.600
_exptl_absorpt_correction_T_max  0.7616
_exptl_absorpt_correction_T_min  0.4787
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             4232
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.774
_refine_diff_density_min         -1.090
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     901
_refine_ls_number_reflns         14916
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0561
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0698P)^2^+34.7056P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1421
_refine_ls_wR_factor_ref         0.1510
_reflns_number_gt                11538
_reflns_number_total             14916
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b815122a.txt
_cod_data_source_block           1
_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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        8547.789(119)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7000619