5-Chloro-5''-(4-chlorobenzylidene)-4'-(4-chlorophenyl)-1',1''-dimethyldispiro[indoline-3,2'-pyrrolidine-3',3''-piperidine]-2,4''-dione
Farag, I. S. Ahmed; Girgis, Adel S.; Ramadan, A. A.; Moustafa, A. M.; Mabied, Ahmed F.; Acta Crystallographica Section E 70 (2014) o379–o380; doi:10.1107/S1600536814004309

data_2239472
_publ_section_title
;
 5-Chloro-5''-(4-chlorobenzylidene)-4'-(4-chlorophenyl)-1',1''-dimethyldispiro[indoline-3,2'-pyrrolidine-3',3''-piperidine]-2,4''-dione
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o379
_journal_page_last               o380
_journal_paper_doi               10.1107/S1600536814004309
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C30 H26 Cl3 N3 O2'
_chemical_formula_moiety         'C30 H26 Cl3 N3 O2'
_chemical_formula_sum            'C30 H26 Cl3 N3 O2'
_chemical_formula_weight         566.91
_chemical_melting_point_gt       510
_chemical_melting_point_lt       512
_chemical_name_systematic
5-Chloro-5''-(4-chlorobenzylidene)-4'-(4-chlorophenyl)-1',1''-dimethyldispiro[indoline-3,2'-pyrrolidine-3',3''-piperidine]-2,4''-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   difmap
_cell_angle_alpha                99.0734(8)
_cell_angle_beta                 90.1887(9)
_cell_angle_gamma                116.4041(10)
_cell_formula_units_Z            2
_cell_length_a                   11.2102(3)
_cell_length_b                   11.5909(3)
_cell_length_c                   12.3569(4)
_cell_measurement_reflns_used    8506
_cell_measurement_temperature    298
_cell_measurement_theta_max      27
_cell_measurement_theta_min      3
_cell_volume                     1415.22(7)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
;
CAMERON (Watkin <i>et al.</i>, 1996) and DIAMOND (Brandenburg,
2012)
;
_computing_publication_material
;
CRYSTALS (Betteridge <i>et al.</i>, 2003); software used to prepare
material
for publication: publCIF (Westrip, 2010)
;
_computing_structure_refinement  'CRYSTALS (Betteridge <i>et al.</i>, 2003)'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.076
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            16419
_diffrn_reflns_theta_full        26.953
_diffrn_reflns_theta_max         27.503
_diffrn_reflns_theta_min         3.351
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.356
_exptl_absorpt_correction_T_max  0.876
_exptl_absorpt_correction_T_min  0.630
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'[G\"orbitz (1999) and DENZO/SCALEPACK (Otwinowski & Minor, 1997)]'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.55
_refine_diff_density_min         -0.54
_refine_ls_extinction_coef       40E1(7)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.0046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         3663
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1157
_refine_ls_R_factor_gt           0.0565
_refine_ls_shift/su_max          0.0005037
_refine_ls_shift/su_mean         0.0000238
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin et al., 1994)
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
 Method = Robust Weighting  W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
 A~i~ are:  100. 168. 111. 49.9 14.3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1346
_refine_ls_wR_factor_gt          0.1108
_refine_ls_wR_factor_ref         0.1108
_reflns_number_gt                3663
_reflns_number_total             6508
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            zs2286sup1.cf
_cod_data_source_block           I
_cod_database_code               2239472
_cod_database_fobs_code          2239472