Siloles and germoles modified by partial hypercoordination through aminoxy substituents
Losehand, Udo; Mitzel, Norbert W.; Journal of the Chemical Society, Dalton Transactions  (2000) 1049–; doi:10.1039/a909547k

data_7009241
_publ_section_title
;
 Siloles and germoles modified by partial hypercoordination through
 aminoxy substituents
;
_journal_issue                   7
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1049
_journal_paper_doi               10.1039/a909547k
_journal_year                    2000
_chemical_formula_sum            'C32 H32 Ge N2 O2'
_chemical_formula_weight         549.19
_chemical_name_systematic
; 
 1,1-Bis(N,N-dimethylaminoxy)-2,3,4,5-tetraphenyl-1-germacyclopentadien
;
_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-97
_cell_angle_alpha                81.16(2)
_cell_angle_beta                 84.37(2)
_cell_angle_gamma                66.05(2)
_cell_formula_units_Z            4
_cell_length_a                   12.399(4)
_cell_length_b                   12.453(3)
_cell_length_c                   19.955(3)
_cell_measurement_reflns_used    100
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      10
_cell_volume                     2780.2(13)
_computing_cell_refinement       CAD4-Software
_computing_data_collection       CAD4-Software
_computing_data_reduction        CADSHEL
_computing_molecular_graphics    'SHELXTL 5.01'
_computing_publication_material  'SHELXTL 5.01'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.2326
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10945
_diffrn_reflns_theta_full        26.11
_diffrn_reflns_theta_max         26.11
_diffrn_reflns_theta_min         2.04
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.133
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Thin plate'
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.619
_refine_diff_density_min         -0.909
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     761
_refine_ls_number_reflns         10945
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.2201
_refine_ls_R_factor_gt           0.0659
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0821P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1401
_refine_ls_wR_factor_ref         0.1825
_reflns_number_gt                5152
_reflns_number_total             10945
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            a909547k.txt
_cod_data_source_block           los25
_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 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'None' changed to
'none' 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        2780.2(12)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7009241