The First X-ray Study of Alkoxynitrosoamines
Irina Yu. Bagryanskaya; Tatyana V. Rybalova; Yuri V. Gatilov; Vadim K. Khlestkin; Dmitrii G. Mazhukin; Acta Crystallographica Section C 54 (1998) IUC9800073–; doi:10.1107/S0108270198099120

data_2008012
_publ_section_title
;
 The First X-ray Study of Alkoxynitrosoamines
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              IUC9800073
_journal_paper_doi               10.1107/S0108270198099120
_journal_volume                  54
_journal_year                    1998
_chemical_formula_moiety         'C9 H19 N3 O4'
_chemical_formula_sum            'C9 H19 N3 O4'
_chemical_formula_weight         233.27
_chemical_melting_point          93
_chemical_name_systematic
;
N-formyl-N'-nitroso-N,N'-dimethoxy-2,3-dimethyl-2,3-butanediamine
;
_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'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 109.740(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.4240(10)
_cell_length_b                   13.611(2)
_cell_length_c                   7.2310(10)
_cell_measurement_reflns_used    28
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      35.1
_cell_measurement_theta_min      30.6
_cell_volume                     595.10(16)
_computing_cell_refinement       'Syntex P21 software'
_computing_data_collection       'Syntex P21 software'
_computing_data_reduction        'Syntex XTAPE'
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measurement_device_type  'Syntex P2~1~'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.027
_diffrn_reflns_av_sigmaI/netI    0.0175
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1345
_diffrn_reflns_theta_max         69.97
_diffrn_reflns_theta_min         6.50
_diffrn_standards_decay_%        2.0
_diffrn_standards_interval_count 97
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.859
_exptl_absorpt_correction_T_max  0.841
_exptl_absorpt_correction_T_min  0.686
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Numerical absorption correction for crystal defined
by faces (SHELX-76).
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             252
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.249
_refine_diff_density_min         -0.118
_refine_ls_extinction_coef       0.018(3)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.085
_refine_ls_goodness_of_fit_obs   1.122
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         1132
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_restrained_S_obs      1.122
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_obs          0.0360
_refine_ls_shift/su_max          -0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0561P)^2^+0.0941P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1020
_refine_ls_wR_factor_obs         0.1003
_reflns_number_observed          1033
_reflns_number_total             1132
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            qa0066.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0561P)^2^+0.0941P] 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^)+(0.0561P)^2^+0.0941P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        595.1(2)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2008012