Synthesis, Decomposition, and Structural Studies in the Gas Phase and Solid State of N,N-Dimethylaminoxygermane
Norbert W. Mitzel; Udo Losehand; Sarah L. Hinchley; David W. H. Rankin; Inorganic Chemistry 40 (2001) 661–666; doi:10.1021/ic0007409

data_4319239
_publ_section_title
;
 Synthesis, Decomposition, and Structural Studies in the Gas Phase and
 Solid State of N,N-Dimethylaminoxygermane
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              661
_journal_page_last               666
_journal_paper_doi               10.1021/ic0007409
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C2 H9 Ge N O'
_chemical_formula_weight         135.69
_chemical_melting_point          251.15
_chemical_name_systematic
; 
 N,N-Dimethyl-O-germyl-hydroxylamine
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.1280(12)
_cell_length_b                   9.7037(15)
_cell_length_c                   7.0722(12)
_cell_measurement_reflns_used    100
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      20
_cell_volume                     557.80(15)
_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      153(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius CAD4 Turbo'
_diffrn_measurement_method       'omega scan'
_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  0.0399
_diffrn_reflns_av_sigmaI/netI    0.0266
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4749
_diffrn_reflns_theta_full        34.94
_diffrn_reflns_theta_max         34.94
_diffrn_reflns_theta_min         3.56
_diffrn_standards_decay_%        None
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.350
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Cylinder
_exptl_crystal_F_000             272
_exptl_crystal_size_max          0.9
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.575
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.111
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     48
_refine_ls_number_reflns         1286
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0249
_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^)+(0.0433P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0620
_refine_ls_wR_factor_ref         0.0638
_reflns_number_gt                1166
_reflns_number_total             1286
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0007409.cif
_cod_data_source_block           los23
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '-22' was changed to '251.15' - it
was converted from degrees Celsius(C) to Kelvins(K).

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'None' changed to
'none' according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4319239