KOH-catalyzed highly efficient aminohalogenation of β-nitrostyrenes with t-butyl N,N-dichlorocarbamate as nitrogen/halogen source
Mei, Haibo; Han, Jianlin; Li, Guigen; Pan, Yi; RSC Advances 1 (2011) 429–; doi:10.1039/c1ra00174d

data_7238399
_publ_section_title
;
 KOH-catalyzed highly efficient aminohalogenation of \b-nitrostyrenes with
 t-butyl N,N-dichlorocarbamate as nitrogen/halogen source
;
_journal_issue                   3
_journal_name_full               'RSC Advances'
_journal_page_first              429
_journal_paper_doi               10.1039/c1ra00174d
_journal_volume                  1
_journal_year                    2011
_chemical_formula_moiety         'C13 H15 Cl2 N2 O4'
_chemical_formula_sum            'C13 H15 Cl2 N2 O4'
_chemical_formula_weight         334.17
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.7762(8)
_cell_length_b                   9.6032(13)
_cell_length_c                   28.672(4)
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.360
_cell_volume                     1590.4(4)
_computing_cell_refinement       'Bruker SHELXTL Program'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        Saint
_computing_molecular_graphics    'Bruker SHELXTL Program'
_computing_publication_material  'Bruker SHELXTL Program'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Apex II CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.1228
_diffrn_reflns_av_sigmaI/netI    0.0829
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            8921
_diffrn_reflns_theta_full        26.36
_diffrn_reflns_theta_max         26.36
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    0.424
_exptl_absorpt_correction_T_max  0.903
_exptl_absorpt_correction_T_min  0.881
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangle
_exptl_crystal_F_000             692.0
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.444
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         3236
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0517
_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^)+(0.0675P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1346
_refine_ls_wR_factor_ref         0.1374
_reflns_number_gt                2986
_reflns_number_total             3236
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1ra00174d.txt
_cod_data_source_block           2110328e_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               7238399