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_2012524
_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 H17 Cl N4'
_chemical_formula_moiety         'C19 H17 Cl N4'
_chemical_formula_sum            'C19 H17 Cl N4'
_chemical_formula_weight         336.82
_chemical_melting_point          513
_chemical_name_systematic
;
5-(4-Chlorophenyl)-3-methyl-1-phenyl-1,6,7,8-
tetrahydropyrazolo[3,4-b][1,4]diazepine
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     odirect
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                115.73(3)
_cell_angle_beta                 101.02(3)
_cell_angle_gamma                98.83(3)
_cell_formula_units_Z            6
_cell_length_a                   9.0066(18)
_cell_length_b                   17.969(4)
_cell_length_c                   18.007(4)
_cell_measurement_reflns_used    11212
_cell_measurement_temperature    120.0(10)
_cell_measurement_theta_max      27.64
_cell_measurement_theta_min      2.99
_cell_volume                     2483.0(13)
_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 .991
_diffrn_measured_fraction_theta_max .969
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f scans and \w scans with \k offsets'
_diffrn_radiation_monochromator  graphite
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_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .1079
_diffrn_reflns_av_sigmaI/netI    .0974
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            37371
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.64
_diffrn_reflns_theta_min         2.99
_diffrn_standards_decay_%        negligible
_exptl_absorpt_coefficient_mu    .238
_exptl_absorpt_correction_T_max  .9766
_exptl_absorpt_correction_T_min  .8943
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(DENZO-SMN; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          .48
_exptl_crystal_size_mid          .12
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     652
_refine_ls_number_reflns         11212
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          .1207
_refine_ls_R_factor_gt           .0822
_refine_ls_shift/su_max          .000
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1172P)^2^+1.3813P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          .2064
_refine_ls_wR_factor_ref         .2263
_reflns_number_gt                7499
_reflns_number_total             11212
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk1526.cif
_cod_data_source_block           II
_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_cell_volume        2483.1(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2012524
_cod_database_fobs_code          2012524