1'-(1,3-Diphenyl-1<i>H</i>-pyrazol-4-yl)-2',3',5',6',7',7a'-hexahydro-1'<i>H</i>-dispiro[acenaphthylene-1,3'-pyrrolizine-2',3''-chromane]-2,4''(1<i>H</i>)-dione
Jagadeesan, G.; Kathirvelan, D.; Haribabu, J.; Reddy, B. S. R.; Sethusankar, K.; Acta Crystallographica Section E 69 (2013) o711–; doi:10.1107/S1600536813009562

data_2237997
_publ_section_title
;
 1'-(1,3-Diphenyl-1<i>H</i>-pyrazol-4-yl)-2',3',5',6',7',7a'-hexahydro-1'<i>H</i>-dispiro[acenaphthylene-1,3'-pyrrolizine-2',3''-chromane]-2,4''(1<i>H</i>)-dione
;
_journal_coeditor_code           RK2396
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o711
_journal_paper_doi               10.1107/S1600536813009562
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C41 H31 N3 O3'
_chemical_formula_moiety         'C41 H31 N3 O3'
_chemical_formula_sum            'C41 H31 N3 O3'
_chemical_formula_weight         613.69
_chemical_name_systematic
1'-(1,3-Diphenyl-1<i>H</i>-pyrazol-4-yl)-2',3',5',6',7',7a'-hexahydro-1'<i>H</i>-dispiro[acenaphthylene-1,3'-pyrrolizine-2',3''-chromane]-2,4''(1<i>H</i>)-dione
_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
_audit_creation_method           SHELXL97
_cell_angle_alpha                114.365(2)
_cell_angle_beta                 96.960(2)
_cell_angle_gamma                92.281(2)
_cell_formula_units_Z            2
_cell_length_a                   10.0183(4)
_cell_length_b                   12.7374(5)
_cell_length_c                   13.2489(5)
_cell_measurement_reflns_used    9207
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      30.93
_cell_measurement_theta_min      2.06
_cell_volume                     1521.17(11)
_computing_cell_refinement       '<i>SAINT</i> (Bruker, 2008)'
_computing_data_collection       '<i>APEX2</i> (Bruker, 2008)'
_computing_data_reduction        '<i>SAINT</i> (Bruker, 2008)'
_computing_molecular_graphics    '<i>ORTEP-3 for Windows</i> (Farrugia, 2012)'
_computing_publication_material
'<i>SHELXL97</i> (Sheldrick, 2008)  and <i>PLATON</i> (Spek, 2009)'
_computing_structure_refinement  '<i>SHELXL97</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SHELXS97</i> (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine--focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_sigmaI/netI    0.0479
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            32812
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.93
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_T_max  0.9832
_exptl_absorpt_correction_T_min  0.9749
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Bruker, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             644
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.464
_refine_diff_density_min         -0.319
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         9207
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.1144
_refine_ls_R_factor_gt           0.0546
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0652P)^2^+0.4938P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1291
_refine_ls_wR_factor_ref         0.1655
_reflns_number_gt                5094
_reflns_number_total             9207
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            rk2396.cif
_cod_data_source_block           I
_cod_database_code               2237997
_cod_database_fobs_code          2237997