13-Benzyl-4,11-dihydroxy-1,8-diphenyl-2,9-dithia-13-azadispiro[4.1.4.3]tetradecan-6-one
Vinotha, G.; Sundar, T. V.; Sharmila, N.; IUCrData 6 (2021) x210210–; doi:10.1107/S2414314621002108

data_1560707
_publ_section_title
;
 13-Benzyl-4,11-dihydroxy-1,8-diphenyl-2,9-dithia-13-azadispiro[4.1.4.3]tetradecan-6-one
;
_journal_coeditor_code           BV4035
_journal_issue                   2
_journal_name_full               IUCrData
_journal_page_first              x210210
_journal_paper_doi               10.1107/S2414314621002108
_journal_volume                  6
_journal_year                    2021
_chemical_formula_iupac          'C30 H31 N O3 S2'
_chemical_formula_moiety         'C30 H31 N O3 S2'
_chemical_formula_sum            'C30 H31 N O3 S2'
_chemical_formula_weight         517.68
_chemical_melting_point          476.15
_chemical_name_systematic
13-Benzyl-4,11-dihydroxy-1,8-diphenyl-2,9-dithia-13-azadispiro[4.1.4.3]tetradecan-6-one
_space_group_crystal_system      tetragonal
_space_group_IT_number           114
_space_group_name_Hall           'P -4 2n'
_space_group_name_H-M_alt        'P -4 21 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.3750(4)
_cell_length_b                   25.3750(4)
_cell_length_c                   8.6456(2)
_cell_measurement_reflns_used    6903
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.277
_cell_measurement_theta_min      1.135
_cell_volume                     5566.82(18)
_computing_cell_refinement
;
SAINT (Bruker, 2008)
;
_computing_data_collection
;
APEX2 (Bruker, 2008)
;
_computing_data_reduction
;
SAINT (Bruker, 2008)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012) and <i>Qmol</i> (Gans & Shalloway,
2001)
;
_computing_publication_material
;
<i>SHELXL2018/3</i> (Sheldrick, 2015) and PLATON (Spek, 2020)'
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEXII area-detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            30401
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.277
_diffrn_reflns_theta_min         1.795
_exptl_absorpt_coefficient_mu    0.222
_exptl_absorpt_correction_T_max  0.742
_exptl_absorpt_correction_T_min  0.685
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 1996)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_description       block
_exptl_crystal_F_000             2192
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.271
_refine_diff_density_min         -0.149
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 2151 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   -0.04(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         6899
_refine_ls_number_restraints     408
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0430
_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^)+(0.0659P)^2^+0.1922P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1038
_refine_ls_wR_factor_ref         0.1102
_reflns_number_gt                5681
_reflns_number_total             6899
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            bv4035sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        5566.8(2)
_cod_database_code               1560707
_shelx_estimated_absorpt_t_min   0.940
_shelx_estimated_absorpt_t_max   0.957
_shelx_hkl_checksum              55058
_shelx_res_checksum              66205
_shelx_fab_checksum              90241
_cod_database_fobs_code 1560707