Synthesis and structures of the group 1 metal/germanium cage complexes [M(µ-OC6H3Ph2-2,6)3Ge] (M = Li, Na, K, Rb, Cs); periodic trends and alkali metal dependent arene bonding
Weinert, Charles S.; Fanwick, Phillip E.; Rothwell, Ian P.; Dalton Transactions  (2003) 1795–; doi:10.1039/b301623d

data_7012820
_publ_section_title
;
 Synthesis and structures of the group 1 metal/germanium cage complexes
 [M(&#x00B5;-OC6H3Ph2-2,6)3Ge] (M = Li, Na, K, Rb, Cs); periodic trends
 and alkali metal dependent arene bonding
;
_journal_issue                   9
_journal_name_full               'Dalton Transactions'
_journal_page_first              1795
_journal_paper_doi               10.1039/b301623d
_journal_year                    2003
_chemical_formula_moiety         'C54 H39 Ge1 Li1 O3,C6 H6'
_chemical_formula_sum            'C60 H45 Ge Li O3'
_chemical_formula_weight         893.56
_chemical_name_systematic        ' ?'
_space_group_IT_number           146
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_atom_type_scat_source
'International Tables for Crystallography (Vol C)'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   15.7846(6)
_cell_length_b                   15.7846(6)
_cell_length_c                   15.839(2)
_cell_measurement_reflns_used    5130
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      2
_cell_volume                     3417.6(5)
_computing_cell_refinement       DENZO/SCALEPACK_(Otwinowski,_1996)
_computing_data_collection       Collect_(Nonius,_1998)
_computing_data_reduction        DENZO/SCALEPACK_(Otwinowski,_1996)
_computing_molecular_graphics
;
ORTEP (Johnson, 1976)
PLUTON (Spek, 1991)
;
_computing_publication_material  CIF_VAX_MolEN_(Fair,_1990)
_computing_structure_refinement  SHELX97_(Sheldrick,_1997)
_computing_structure_solution    Direct_methods_(SIR97,_Altomare_et_al.,_1997)
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.9536
_diffrn_measured_fraction_theta_max 0.8447
_diffrn_measurement_device_type  Nonius_KappaCCD
_diffrn_radiation_type           MO-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.034
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5130
_diffrn_reflns_theta_full        21.7
_diffrn_reflns_theta_max         27.89
_diffrn_reflns_theta_min         2.58
_exptl_absorpt_coefficient_mu    0.707
_exptl_absorpt_correction_T_max  0.8234
_exptl_absorpt_correction_T_min  0.7140
_exptl_absorpt_correction_type   refined_empirical_(Otwinowski_&_Minor,_1996
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.30
_exptl_crystal_description       chunk
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.37
_refine_diff_density_min         -0.34
_refine_ls_abs_structure_details
'Flack H. D. (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.282(8)
_refine_ls_extinction_coef       0.14E-02
_refine_ls_extinction_method     SHELXL97_(Sheldrick_1997)
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    H_atoms_riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     198
_refine_ls_number_reflns         3021
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.031
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'1/[\s^2^(Fo^2^)+(0.0109P)^2^+0.7616P] where P=(Fo^2^+2Fc^2^)/3  '
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.061
_reflns_number_gt                2952
_reflns_number_total             3028
_reflns_threshold_expression     >2.0\s(I)
_cod_data_source_file            b301623d.txt
_cod_data_source_block           SW2255
_cod_depositor_comments
;
The following automatic conversions were performed:
'_refine_ls_weighting_scheme' value 'calc ' changed to 'calc' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

'_geom_angle_publ_flag'
value 'YES' changed to 'yes' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (62
times).

'_geom_bond_publ_flag' value 'YES' changed to 'yes' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (34 times).

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        3417.7(7)
_cod_original_sg_symbol_H-M      'R 3'
_cod_original_formula_sum        'C60 H45 Ge1 Li1 O3'
_cod_database_code               7012820
_reflns_friedl_coverage          0.8045