2,2'-(1,3-Diazinane-1,3-diyl)diacetonitrile: a second monoclinic polymorph
Rivera, Augusto; Maldonado, Mauricio; Ríos-Motta, Jaime; Fejfarová, Karla; Dušek, Michal; Acta Crystallographica Section E 67 (2011) o2734–; doi:10.1107/S1600536811038013

data_2231875
_publ_section_title
;
 2,2'-(1,3-Diazinane-1,3-diyl)diacetonitrile: a second monoclinic
 polymorph
;
_journal_coeditor_code           GK2401
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2734
_journal_paper_doi               10.1107/S1600536811038013
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C8 H12 N4'
_chemical_formula_moiety         'C8 H12 N4'
_chemical_formula_sum            'C8 H12 N4'
_chemical_formula_weight         164.2
_chemical_name_systematic
;
2,2'-(1,3-Diazinane-1,3-diyl)diacetonitrile
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90
_cell_angle_beta                 102.066(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1300(6)
_cell_length_b                   6.3501(3)
_cell_length_c                   13.1373(7)
_cell_measurement_reflns_used    1334
_cell_measurement_temperature    120
_cell_measurement_theta_max      64.39
_cell_measurement_theta_min      3.44
_cell_volume                     907.99(8)
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2010)'
_computing_data_collection       'CrysAlis PRO (Agilent, 2010)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2010)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2005)'
_computing_publication_material  'JANA2006 (Pet\<r\'i\<cek <i>et al.</i>, 2006)'
_computing_structure_refinement  'JANA2006 (Pet\<r\'i\<cek <i>et al.</i> 2006)'
_computing_structure_solution    'SIR2002 (Burla <i>et al.</i>, 2003)'
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 10.3784
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.92
_diffrn_measurement_device       'four-cycle diffractometer'
_diffrn_measurement_device_type
'Agilent Gemini Ultra diffractometer with an Atlas CCD detector'
_diffrn_measurement_method       'Rotation method data acquisition using \w'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_av_sigmaI/netI    0.0384
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            2863
_diffrn_reflns_reduction_process
;
Integration of the CCD images was done by program CrysAlisPro
(Agilent Technologies, 2010). The same program was used for indexing of the
crystal shape and absorption correction.
;
_diffrn_reflns_theta_full        61.82
_diffrn_reflns_theta_max         64.55
_diffrn_reflns_theta_min         4.75
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.625
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.864
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2010)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.2009
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             352
_exptl_crystal_size_max          0.157
_exptl_crystal_size_mid          0.092
_exptl_crystal_size_min          0.012
_refine_diff_density_max         0.18
_refine_diff_density_min         -0.18
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.30
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_constraints    48
_refine_ls_number_parameters     109
_refine_ls_number_reflns         1404
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0387
_refine_ls_shift/su_max          0.0013
_refine_ls_shift/su_mean         0.0003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/[\s^2^(I)+0.0009I^2^]
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0841
_refine_ls_wR_factor_ref         0.0926
_reflns_number_gt                929
_reflns_number_total             1404
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            gk2401.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2231875
_cod_database_fobs_code          2231875