Synthesis and Structure of [K±(2,2)diaza-[18]-crown-6][K3Ge9].2Ethylenediamine: Stabilization of the Two-Dimensional Layer 2\ιnfty[K3Ge91-]
Craig Downie; Jiang-Gao Mao; Arnold M. Guloy; Inorganic Chemistry 40 (2001) 4721–4725; doi:10.1021/ic001107q

data_4320141
_publ_section_title
;
 Synthesis and Structure of
 [K+-(2,2)diaza-[18]-crown-6][K3Ge9].2Ethylenediamine: Stabilization of
 the Two-Dimensional Layer 2\\infty[K3Ge91-]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4721
_journal_page_last               4725
_journal_paper_doi               10.1021/ic001107q
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C16 H42 Ge9 K4 N6 O4'
_chemical_formula_weight         1192.27
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 114.7380(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.7398(9)
_cell_length_b                   15.8121(13)
_cell_length_c                   12.3259(10)
_cell_measurement_temperature    293(2)
_cell_volume                     1901.1(3)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0320
_diffrn_reflns_av_sigmaI/netI    0.0265
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10813
_diffrn_reflns_theta_max         26.04
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    7.478
_exptl_crystal_density_diffrn    2.083
_exptl_crystal_F_000             1152
_refine_diff_density_max         0.880
_refine_diff_density_min         -0.648
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.024
_refine_ls_goodness_of_fit_obs   1.053
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         3888
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_restrained_S_obs      1.053
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_obs          0.0318
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0597P)^2^+0.5836P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0898
_refine_ls_wR_factor_obs         0.0842
_reflns_number_observed          3279
_reflns_number_total             3889
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic001107q.cif
_cod_data_source_block           IC001107Q
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0597P)^2^+0.5836P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0597P)^2^+0.5836P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 1 21/c 1'
_cod_database_code               4320141