Preparation of LGe(Se)OH: A Germanium Analogue of a Selenocarboxylic Acid (L = HC[(CMe)(NAr)]2, Ar = 2,6-iPr2C6H3)
Pineda, Leslie W.; Jancik, Vojtech; Oswald, Rainer B.; Roesky, Herbert W.; Organometallics 25 (2006) 2384–; doi:10.1021/om060088a

data_4075173
_publ_section_title
;
 Preparation of LGe(Se)OH:&#x00A0; A Germanium Analogue of a
 Selenocarboxylic Acid (L = HC[(CMe)(NAr)]2, Ar = 2,6-iPr2C6H3)
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_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2384
_journal_paper_doi               10.1021/om060088a
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety         'C29 H42 Ge N2 O Se, C7 H8'
_chemical_formula_sum            'C36 H50 Ge N2 O Se'
_chemical_formula_weight         678.33
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 115.82(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.974(4)
_cell_length_b                   16.195(3)
_cell_length_c                   18.151(3)
_cell_measurement_reflns_used    5949
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      58.75
_cell_measurement_theta_min      3.73
_cell_volume                     6873(3)
_computing_cell_refinement       'Bruker AXS SAINT (v 7.01A, Bruker 2003)'
_computing_data_collection       'Proteum (v 1.40, Bruker 2002)'
_computing_data_reduction        'Bruker AXS SAINT (v 7.01A, Bruker 2003)'
_computing_molecular_graphics    'Bruker AXS SHELXTL (v 6.12)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.602
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker three circle diffractometer'
_diffrn_measurement_method       'phi and omega scan'
_diffrn_radiation_monochromator  'mirror system'
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0210
_diffrn_reflns_av_sigmaI/netI    0.0231
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14278
_diffrn_reflns_theta_full        58.70
_diffrn_reflns_theta_max         58.70
_diffrn_reflns_theta_min         3.32
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.632
_exptl_absorpt_correction_T_max  0.8171
_exptl_absorpt_correction_T_min  0.6936
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            'pale green'
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2832
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.391
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         4734
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0238
_refine_ls_R_factor_gt           0.0225
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0349P)^2^+6.2439P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0608
_refine_ls_wR_factor_ref         0.0620
_reflns_number_gt                4501
_reflns_number_total             4734
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060088asi20060127_062631.cif
_cod_data_source_block           LGe(Se)OH.C7H8
_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_Hall     '-C 2yc '
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4075173