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_7012821
_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 K1 O3,C6 H6'
_chemical_formula_sum            'C60 H45 Ge K O3'
_chemical_formula_weight         925.72
_chemical_name_systematic        ' ?'
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_type_scat_source
'International Tables for Crystallography (Vol C)'
_audit_creation_date             18-11-02
_audit_creation_method           from_MolEN_and_SHELXL
_audit_update_record             ' ?'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.7319(3)
_cell_length_b                   16.9873(3)
_cell_length_c                   31.0061(5)
_cell_measurement_reflns_used    29711
_cell_measurement_temperature    150
_cell_measurement_theta_max      23
_cell_measurement_theta_min      1
_cell_volume                     9339.6(3)
_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 0.9952
_diffrn_measured_fraction_theta_max 0.9952
_diffrn_measurement_device_type  Nonius_KappaCCD
_diffrn_measurement_method       \w
_diffrn_radiation_type           MO-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.056
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            29711
_diffrn_reflns_theta_full        23.3
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         1.20
_exptl_absorpt_coefficient_mu    0.780
_exptl_absorpt_correction_T_max  0.9157
_exptl_absorpt_correction_T_min  0.6241
_exptl_absorpt_correction_type   refined_empirical_(Otwinowski_&_Minor,_1996
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.32
_exptl_crystal_description       plate
_exptl_crystal_F_000             3840
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.35
_refine_diff_density_min         -0.33
_refine_ls_abs_structure_details
'Flack H. D. (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.557(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    H_atoms_riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1172
_refine_ls_number_reflns         12796
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.038
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'1/[\s^2^(Fo^2^)+(0.0177P)^2^+4.9324P] where P=(Fo^2^+2Fc^2^)/3  '
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.078
_reflns_number_gt                11910
_reflns_number_total             12809
_reflns_threshold_expression     >2.0\s(I)
_cod_data_source_file            b301623d.txt
_cod_data_source_block           SW3329
_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 (408
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 (170 times).

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_formula_sum        'C60 H45 Ge1 K1 O3'
_cod_database_code               7012821
_reflns_friedl_coverage          0.9345