Binuclear tin and germanium calix[4]arenes
McBurnett, Brian G.; Cowley, Alan H.; Chemical Communications  (1999) 17–; doi:10.1039/a807167e

data_7110359
_publ_section_title
;
 Binuclear tin and germanium calix[4]arenes
;
_journal_issue                   1
_journal_name_full               'Chemical Communications'
_journal_page_first              17
_journal_paper_doi               10.1039/a807167e
_journal_year                    1999
_chemical_formula_sum            'C47.5 H59 Cl7 Ge2 O4'
_chemical_formula_weight         1087.28
_chemical_name_systematic
; 
 ? 
;
_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
_cell_angle_alpha                84.630(10)
_cell_angle_beta                 73.460(10)
_cell_angle_gamma                64.980(10)
_cell_formula_units_Z            2
_cell_length_a                   13.201(2)
_cell_length_b                   14.188(2)
_cell_length_c                   15.212(2)
_cell_measurement_reflns_used    71
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      12.23
_cell_measurement_theta_min      4.93
_cell_volume                     2473.8(7)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w 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  0.1596
_diffrn_reflns_av_sigmaI/netI    0.1793
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11358
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.40
_diffrn_standards_decay_%        -9800.00
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.635
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_description       needle
_exptl_crystal_F_000             1118
_exptl_crystal_size_max          1.2
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.499
_refine_diff_density_min         -1.470
_refine_diff_density_rms         0.191
_refine_ls_extinction_coef       0.0192(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.959
_refine_ls_goodness_of_fit_obs   1.140
_refine_ls_matrix_type           full
_refine_ls_number_parameters     551
_refine_ls_number_reflns         9686
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.960
_refine_ls_restrained_S_obs      1.140
_refine_ls_R_factor_all          0.1679
_refine_ls_R_factor_obs          0.0860
_refine_ls_shift/esd_max         -0.009
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1355P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2629
_refine_ls_wR_factor_obs         0.2114
_reflns_number_observed          4601
_reflns_number_total             9687
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            807167Esup1.cif
_cod_data_source_block           bmcb16
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1355P)^2^+0.0000P] 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^)+(0.1355P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2473.8(6)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C47.50 H59 Cl7 Ge2 O4'
_cod_database_code               7110359