The 143 and 300K polymorphs of hexamethylenetetraminium 2,4-dinitrophenolate monohydrate
Anwar Usman; Suchada Chantrapromma; Hoong-Kun Fun; Acta Crystallographica Section C 57 (2001) 1443–1446; doi:10.1107/S0108270101016742

data_2012391
_publ_section_title
;
 The 143 and 300K polymorphs of hexamethylenetetraminium
 2,4-dinitrophenolate monohydrate
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1443
_journal_page_last               1446
_journal_paper_doi               10.1107/S0108270101016742
_journal_volume                  57
_journal_year                    2001
_chemical_formula_iupac          'C6 H13 N4 1+, C6 H3 N2 O5 1-, H2 O'
_chemical_formula_moiety         'C6 H13 N4 1+, C6 H3 N2 O5 1-, H2 O'
_chemical_formula_sum            'C12 H18 N6 O6'
_chemical_formula_weight         342.32
_chemical_name_systematic
;
3,5,7-triaza-1-azoniatricyclo[3.3.1.1^3,7^]decane
2,4-dinitrophenolate monohydrate
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_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                 94.9150(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.8610(5)
_cell_length_b                   6.5980(4)
_cell_length_c                   14.4339(9)
_cell_measurement_reflns_used    3560
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      29.56
_cell_measurement_theta_min      1.42
_cell_volume                     745.89(8)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material
;
SHELXTL, PARST (Nardelli, 1995) and PLATON (Spek, 1990)
;
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 1997)'
_diffrn_ambient_temperature      300(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full .967
_diffrn_measured_fraction_theta_max .967
_diffrn_measurement_device_type  'Siemens SMART CCD area-detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .0686
_diffrn_reflns_av_sigmaI/netI    .0957
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5088
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.60
_diffrn_standards_decay_%        negligible
_exptl_absorpt_coefficient_mu    .124
_exptl_absorpt_correction_T_max  .9757
_exptl_absorpt_correction_T_min  .9498
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             360
_exptl_crystal_size_max          .42
_exptl_crystal_size_mid          .24
_exptl_crystal_size_min          .20
_refine_diff_density_max         .334
_refine_diff_density_min         -.313
_refine_ls_extinction_coef       .145(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXTL
_refine_ls_goodness_of_fit_ref   .948
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         1900
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      .948
_refine_ls_R_factor_all          .0743
_refine_ls_R_factor_gt           .0589
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0622P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          .1374
_refine_ls_wR_factor_ref         .1437
_reflns_number_gt                1288
_reflns_number_total             1900
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk1495.cif
_cod_data_source_block           Iat300K
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 
;
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               2012391
_cod_database_fobs_code          2012391