Synthesis and molecular structures of N,N-dimethylhydroxylamino-trichlorosilane and -germane †
Losehand, Udo; Mitzel, Norbert W.; Rankin, David W. H.; Journal of the Chemical Society, Dalton Transactions  (1999) 4291–; doi:10.1039/a906688h

data_7027775
_publ_section_title
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 Synthesis and molecular structures of
 N,N-dimethylhydroxylamino-trichlorosilane and -germane&#x200A;&#x2020;
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_journal_issue                   24
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4291
_journal_paper_doi               10.1039/a906688h
_journal_year                    1999
_chemical_formula_sum            'C2 H6 Cl3 N O Si'
_chemical_formula_weight         194.52
_chemical_name_systematic
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 O-Trichlorsilyl-N,N-dimethylhydroxylamin 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 98.37(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.585(1)
_cell_length_b                   7.487(1)
_cell_length_c                   19.069(2)
_cell_measurement_reflns_used    96
_cell_measurement_temperature    149(2)
_cell_measurement_theta_max      23
_cell_measurement_theta_min      18
_cell_volume                     1636.4(3)
_computing_cell_refinement       'CAD4 5.0'
_computing_data_collection       'CAD4 5.0'
_computing_data_reduction        CADSHEL
_computing_molecular_graphics    'SHELXTL 5.01'
_computing_publication_material  'SHELXTL 5.01'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      149(2)
_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  0.0320
_diffrn_reflns_av_sigmaI/netI    0.0159
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3642
_diffrn_reflns_theta_max         26.92
_diffrn_reflns_theta_min         3.25
_diffrn_standards_decay_%        None
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.184
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_description       Column
_exptl_crystal_F_000             784
_exptl_crystal_size_max          1.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.539
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       0.0016(5)
_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   1.103
_refine_ls_goodness_of_fit_obs   1.128
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         3532
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.174
_refine_ls_restrained_S_obs      1.128
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_obs          0.0355
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0576P)^2^+0.5440P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1029
_refine_ls_wR_factor_obs         0.0897
_reflns_number_observed          2944
_reflns_number_total             3545
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            906688hsup1.cif
_cod_data_source_block           los10
_cod_depositor_comments
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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 2.4.2 from
2011-04-26.

'_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 2.4.2 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^)+(0.0576P)^2^+0.5440P] 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^)+(0.0576P)^2^+0.5440P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7027775