Synthesis, spectroscopic and crystallographic study of some carbamates from an azabicyclic chloroformate and primary heterocyclic amines
Isabel Iriepa; F. Javier Villasante; Enrique Gálvez; Juana Bellanato; Avelino Martín; Pilar Gómez-Sal; New J. Chem. 28 (2004) 618–624; doi:10.1039/b309065e

data_7050183
_publ_section_title
;
 Synthesis, spectroscopic and crystallographic study of some carbamates
 from an azabicyclic chloroformate and primary heterocyclic amines
;
_journal_issue                   5
_journal_name_full               'New J. Chem.'
_journal_page_first              618
_journal_page_last               624
_journal_paper_doi               10.1039/b309065e
_journal_volume                  28
_journal_year                    2004
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C17 H22 N4 O2'
_chemical_formula_structural     'C17 N4 O2 H22'
_chemical_formula_sum            'C17 H22 N4 O2'
_chemical_formula_weight         314.38
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_conform_dict_location     ftp://ftp.iucr.org/cifdics/cif_core2.1beta.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1beta3
_audit_creation_date             2000-03-10T11:19:08-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 106.640(12)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.644(3)
_cell_length_b                   14.574(5)
_cell_length_c                   17.816(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13
_cell_measurement_theta_min      6
_cell_measurement_wavelength     0.71073
_cell_volume                     3394.3(16)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius TurboCAD4'
_diffrn_measurement_method       'non-profiled omega-theta scans'
_diffrn_orient_matrix_type
;
x-axis points to radiation source
the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_UB_11      0.4211E-2
_diffrn_orient_matrix_UB_12      -0.40253E-1
_diffrn_orient_matrix_UB_13      -0.44403E-1
_diffrn_orient_matrix_UB_21      0.59624E-1
_diffrn_orient_matrix_UB_22      0.36487E-1
_diffrn_orient_matrix_UB_23      -0.5616E-2
_diffrn_orient_matrix_UB_31      0.48012E-1
_diffrn_orient_matrix_UB_32      -0.04175
_diffrn_orient_matrix_UB_33      0.37916E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0925
_diffrn_reflns_av_sigmaI/netI    0.1273
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            6212
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         3.04
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.084
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.653
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         5948
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.227
_refine_ls_R_factor_gt           0.0846
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1641P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2287
_refine_ls_wR_factor_ref         0.3129
_reflns_number_gt                2376
_reflns_number_total             5948
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b309065e.txt
_cod_data_source_block           iic2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1641P)^2^+0.0000P] 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^)+(0.1641P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7050183
_diffrn_standards_decay_corr_max 1.025
_diffrn_standards_decay_corr_min 0.965