X-ray diffraction analysis of two hexahydropyrido[2,1-<i>b</i>][1,3,4]oxadiazines: evidence for the effect of steric congestion on anion formation at the aminonitrile centre
Chiaroni, A.; Riche, C.; Guerrier, L.; Royer, J.; Grierson, D. S.; Husson, H.-P.; Acta Crystallographica Section C 49 (1993) 1786–1789; doi:10.1107/S0108270193002136

data_2001309
_publ_section_title
;
 X-ray diffraction analysis of two
 hexahydropyrido[2,1-<i>b</i>][1,3,4]oxadiazines: evidence for the
 effect of steric congestion on anion formation at the aminonitrile
 centre
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1786
_journal_page_last               1789
_journal_paper_doi               10.1107/S0108270193002136
_journal_volume                  49
_journal_year                    1993
_chemical_formula_moiety         'C16 H21 N3 O1'
_chemical_formula_sum            'C16 H21 N3 O'
_chemical_formula_weight         271.36
_chemical_name_systematic
;
2H,3H-2-phenyl-3,4-dimethyl-6-carbonitrile 2R-[2\a,3\a,6\b,9\a]-
hexahydropyrido [2,1-b][1,3,4] oxadiazin
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_type_scat_source           IntTabIV
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.934(3)
_cell_length_b                   11.556(4)
_cell_length_c                   14.884(6)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293
_cell_measurement_theta_max      45.6
_cell_measurement_theta_min      5.9
_cell_volume                     1536.6(10)
_computing_data_collection       'Philips  PW1100/20 software 1974'
_computing_data_reduction        'PHIL (Riche, 1981)'
_computing_molecular_graphics    'R3M  (Riche,1983)  ORTEP (Johnson, 1965)'
_computing_publication_material  'ACTACIF (Riche, 1992)'
_computing_structure_refinement  'SHELX76   (Sheldrick, 1976)'
_computing_structure_solution    'SHELXS86  (Sheldrick, 1986)'
_diffrn_ambient_temperature      293
_diffrn_measurement_device       'Philips PW100 diffractometer'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.044
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5557
_diffrn_reflns_theta_max         67.94
_diffrn_reflns_theta_min         2.97
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  180
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.56
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.17
_exptl_crystal_description       prism
_exptl_crystal_F_000             584.00
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.14
_refine_diff_density_min         -0.19
_refine_ls_goodness_of_fit_obs   0.82
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         1473
_refine_ls_R_factor_obs          0.041
_refine_ls_shift/esd_max         0.09
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(F)+ 0.0053F^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.060
_reflns_number_observed          1473
_reflns_number_total             1618
_reflns_observed_criterion       I>3.0\s(I)
_cod_data_source_file            pa1042.cif
_cod_data_source_block           2R-oxadiazin
_cod_depositor_comments
;
 Adding the _atom_site_type_symbol data item.

 Antanas Vaitkus,
 2017-01-28

The following automatic conversions were performed:
'_refine_ls_matrix_type' value 'Full' changed to 'full' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_matrix_type' value 'Full' changed to 'full' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w = 1/[\s^2^(F)+
0.0053F^2^]' 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^(F)+ 0.0053F^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1536.6(9)
_cod_original_formula_sum        'C16 H21 N3 O1'
_cod_database_code               2001309