Supramolecular hydrogen-bonded hexamers in two 5-aryl-3-methyl-1-phenyl-1,6,7,8-tetrahydropyrazolo[3,4-<i>b</i>][1,4]diazepines
Low, John Nicolson; Cobo, Justo; Insuasty, Braulio; Insuasty, Henry; Nogueras, Manuel; Sánchez, Adolfo; Acta Crystallographica Section C 58 (2002) o103–o105; doi:10.1107/S0108270101020625

data_2012523
_publ_section_title
;Supramolecular hydrogen-bonded hexamers in two
 5-aryl-3-methyl-1-phenyl-1,6,7,8-tetrahydropyrazolo[3,4-<i>b</i>][1,4]diazepines
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o103
_journal_page_last               o105
_journal_paper_doi               10.1107/S0108270101020625
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          'C19 H18 N4'
_chemical_formula_moiety         'C19 H18 N4'
_chemical_formula_sum            'C19 H18 N4'
_chemical_formula_weight         302.38
_chemical_melting_point          493
_chemical_name_systematic
;
3-methyl-1,5-diphenyl-1,6,7,8-tetrahydropyrazolo[3,4-b][1,4]diazepine
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            18
_cell_length_a                   30.5212(7)
_cell_length_b                   30.5212(7)
_cell_length_c                   8.8689(2)
_cell_measurement_reflns_used    3272
_cell_measurement_temperature    120.0(10)
_cell_measurement_theta_max      27.09
_cell_measurement_theta_min      3.07
_cell_volume                     7154.9(3)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics
'ORTEPII (Johnson, 1976) and PLATON (Spek, 2001)'
_computing_publication_material
'SHELXL97 and WordPerfect macro PRPKAPPA (Ferguson, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120.0(10)
_diffrn_measured_fraction_theta_full .959
_diffrn_measured_fraction_theta_max .934
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f scans and \w scans with \k offsets'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .037
_diffrn_reflns_av_sigmaI/netI    .0417
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            40810
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.09
_diffrn_reflns_theta_min         3.07
_diffrn_standards_decay_%        negligible
_exptl_absorpt_coefficient_mu    .078
_exptl_absorpt_correction_T_max  .9923
_exptl_absorpt_correction_T_min  .9809
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(DENZO-SMN; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          .25
_exptl_crystal_size_mid          .15
_exptl_crystal_size_min          .10
_refine_diff_density_max         .395
_refine_diff_density_min         -.460
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3272
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          .0662
_refine_ls_R_factor_gt           .0497
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0676P)^2^+6.7105P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          .1234
_refine_ls_wR_factor_ref         .1334
_reflns_number_gt                2600
_reflns_number_total             3272
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk1526.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' 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      'R -3'
_cod_database_code               2012523
_cod_database_fobs_code          2012523