Use of73Ge NMR Spectroscopy and X-ray Crystallography for the Study of Electronic Interactions in Substituted Tetrakis(phenyl)-, -(phenoxy)-, and -(thiophenoxy)germanes
Yoder, Claude H.; Agee, Tamara M.; Griffith, Allison K.; Schaeffer, Charles D.; Carroll, Mary J.; DeToma, Alaina S.; Fleisher, Adam J.; Gettel, Cameron J.; Rheingold, Arnold L.; Organometallics 29 (2010) 582–; doi:10.1021/om900905c

data_4067370
_publ_section_title
;
 Use of73Ge NMR Spectroscopy and X-ray Crystallography for the Study of
 Electronic Interactions in Substituted Tetrakis(phenyl)-, -(phenoxy)-,
 and -(thiophenoxy)germanes
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              582
_journal_paper_doi               10.1021/om900905c
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C28 H28 Ge O4 S4'
_chemical_formula_weight         629.33
_chemical_name_systematic
; 
 tetrakis(o-methoxythiophenoxy)germane 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.550(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.619(2)
_cell_length_b                   7.7442(9)
_cell_length_c                   19.302(2)
_cell_measurement_reflns_used    7276
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.24
_cell_measurement_theta_min      3.69
_cell_volume                     2726.8(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0362
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            11692
_diffrn_reflns_theta_full        60.00
_diffrn_reflns_theta_max         68.27
_diffrn_reflns_theta_min         3.69
_exptl_absorpt_coefficient_mu    4.668
_exptl_absorpt_correction_T_max  0.888
_exptl_absorpt_correction_T_min  0.689
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.617
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       0.00011(4)
_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_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         4697
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0374
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0202P)^2^+8.2904P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0882
_refine_ls_wR_factor_ref         0.0910
_reflns_number_gt                4123
_reflns_number_total             4697
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900905c_si_001.cif
_cod_data_source_block           schaef10
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4067370