Crystal structure of 2'-[(2',4'-difluorobiphenyl-4-yl)carbonyl]-1'-phenyl-1',2',5',6',7',7a'-hexahydrospiro[indole-3,3'-pyrrolizin]-2(1<i>H</i>)-one
Fathimunnisa, M.; Manikandan, H.; Selvanayagam, S.; Sridhar, B.; Acta Crystallographica Section E 71 (2015) 915–918; doi:10.1107/S2056989015012931

data_2240919
_publ_section_title
;
 Crystal structure of
 2'-[(2',4'-difluorobiphenyl-4-yl)carbonyl]-1'-phenyl-1',2',5',6',7',7a'-hexahydrospiro[indole-3,3'-pyrrolizin]-2(1<i>H</i>)-one
;
_journal_coeditor_code           GK2637
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              915
_journal_page_last               918
_journal_paper_doi               10.1107/S2056989015012931
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C33 H26 F2 N2 O2'
_chemical_formula_moiety         'C33 H26 F2 N2 O2'
_chemical_formula_sum            'C33 H26 F2 N2 O2'
_chemical_formula_weight         520.56
_chemical_melting_point          451
_chemical_name_systematic
2'-[(2',4'-Difluorobiphenyl-4-yl)carbonyl]-1'-phenyl-1',2',5',6',7',7a'-hexahydrospiro[indole-3,3'-pyrrolizin]-2(1<i>H</i>)-one
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 98.805(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.6019(13)
_cell_length_b                   9.3128(10)
_cell_length_c                   22.441(2)
_cell_measurement_reflns_used    18178
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      27.2
_cell_measurement_theta_min      2.2
_cell_volume                     2602.6(5)
_computing_cell_refinement
;
SAINT (Bruker, 2001)
;
_computing_data_collection
;
SMART (Bruker, 2001)
;
_computing_data_reduction
;
SAINT (Bruker, 2001)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012) and PLATON (Spek, 2009)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015) and PLATON (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      292(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            29662
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.325
_diffrn_reflns_theta_min         1.749
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.203
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         6300
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0726
_refine_ls_R_factor_gt           0.0565
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0756P)^2^+0.7147P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1435
_refine_ls_wR_factor_ref         0.1549
_reflns_number_gt                4886
_reflns_number_total             6300
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            gk2637sup1.cif
_cod_data_source_block           I
_cod_database_code               2240919
_cod_database_fobs_code          2240919
_shelx_hkl_checksum              30971
_shelx_res_checksum              52013