The molecular and supramolecular structures of four 1,5,6,10b-tetrahydropyrazolo[1,5-<i>c</i>]quinazolines
Low, John Nicolson; Cobo, Justo; Nogueras, Manuel; Sánchez, Adolfo; Torres, Harlen; Insuasty, Braulio; Acta Crystallographica Section C 58 (2002) o305–o310; doi:10.1107/S0108270102006200

data_2012706
_publ_section_title
;
 The molecular and supramolecular structures of four
 1,5,6,10b-tetrahydropyrazolo[1,5-<i>c</i>]quinazolines
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o305
_journal_page_last               o310
_journal_paper_doi               10.1107/S0108270102006200
_journal_volume                  58
_journal_year                    2002
_chemical_formula_moiety         'C22 H17 Br Cl N3'
_chemical_formula_sum            'C22 H17 Br Cl N3'
_chemical_formula_weight         438.7534
_chemical_melting_point          487
_chemical_name_systematic
;
5-(4-Bromophenyl)-2-(4-chlorophenyl)-1,5,6,10b-tetrahydropyrazolo[1,5-c]
quinazoline
;
_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     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                77.9230(9)
_cell_angle_beta                 83.0060(8)
_cell_angle_gamma                87.8140(10)
_cell_formula_units_Z            2
_cell_length_a                   5.55600(10)
_cell_length_b                   12.2526(2)
_cell_length_c                   14.0827(3)
_cell_measurement_reflns_used    4188
_cell_measurement_temperature    120.0(10)
_cell_measurement_theta_max      27.44
_cell_measurement_theta_min      2.98
_cell_volume                     930.41(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, 2002)'
_computing_publication_material  'SHELXL97 and 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 0.994
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_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           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.068
_diffrn_reflns_av_sigmaI/netI    0.048
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14350
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         2.98
_diffrn_standards_decay_%        negligible
_exptl_absorpt_coefficient_mu    2.365
_exptl_absorpt_correction_T_max  0.843
_exptl_absorpt_correction_T_min  0.492
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(DENZO-SMN; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             444
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.49
_refine_diff_density_min         -0.68
_refine_ls_extinction_coef       0.0130(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         4188
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.042
_refine_ls_R_factor_gt           0.034
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0266P)^2^+0.6775P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.076
_refine_ls_wR_factor_ref         0.080
_reflns_number_gt                3683
_reflns_number_total             4188
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gg1111.cif
_cod_data_source_block           IV
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_Hall     -P_1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2012706
_cod_database_fobs_code          2012706