3-[5-(4-Bromophenyl)-1<i>H</i>-pyrazol-3-ylamino]-5,5-dimethylcyclohex-2-en-1-one–(<i>Z</i>)-3-(4-bromophenyl)-3-chloroacrylonitrile (2/1): a stoichiometric cocrystal of a reaction product with one of its early precursors
Cruz, Silvia; Quiroga, Jairo; Torre, José M. de la; Cobo, Justo; Low, John N.; Glidewell, Christopher; Acta Crystallographica Section C 62 (2006) o608–o611; doi:10.1107/S0108270106033968

data_2015596
_publ_section_title
;3-[5-(4-Bromophenyl)-1<i>H</i>-pyrazol-3-ylamino]-5,5-dimethylcyclohex-2-en-1-one--(<i>Z</i>)-3-(4-bromophenyl)-3-chloroacrylonitrile
 (2/1): a stoichiometric cocrystal of a reaction product with one of its early
 precursors
;
_journal_coeditor_code           FA3037
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o608
_journal_page_last               o611
_journal_paper_doi               10.1107/S0108270106033968
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '2C17 H18 Br N3 O , C9 H5 Br Cl N'
_chemical_formula_moiety         '2C17 H18 Br N3 O , C9 H5 Br Cl N'
_chemical_formula_sum            'C43 H41 Br3 Cl N7 O2'
_chemical_formula_weight         963.01
_chemical_name_systematic
;
3-[5-(4-Bromophenyl)-1H-pyrazol-3-ylamino]-5,5-dimethylcyclohex-
2-en-1-one--(Z)-3-(4-bromophenyl)-3-chloroacrylonitrile (2:1)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 93.050(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.4390(4)
_cell_length_b                   13.8680(4)
_cell_length_c                   46.1620(15)
_cell_measurement_reflns_used    9729
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.70
_cell_volume                     8591.1(5)
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997) and COLLECT'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'DENZO and COLLECT'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL97 and PRPKAPPA (Ferguson, 1999)'
_computing_structure_refinement
'OSCAIL (McArdle, 2003) and SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR2004 (Burla <i>et al.</i>,  2005)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker Nonius KappaCCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_sigmaI/netI    0.0395
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       59
_diffrn_reflns_limit_l_min       -59
_diffrn_reflns_number            49869
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.70
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.924
_exptl_absorpt_correction_T_max  0.557
_exptl_absorpt_correction_T_min  0.338
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3888
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.618
_refine_diff_density_min         -0.726
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         9729
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0984
_refine_ls_R_factor_gt           0.0512
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0539P)^2^+16.273P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1165
_refine_ls_wR_factor_ref         0.1364
_reflns_number_gt                5997
_reflns_number_total             9729
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fa3037.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2015596
_cod_database_fobs_code          2015596