Crystal structure of (1<i>S</i>,2<i>R</i>,6<i>R</i>,7<i>R</i>,8<i>S</i>,12<i>S</i>)-4,10,17-triphenyl-15-thia-4,10-diazapentacyclo[5.5.5.0^1,16^.0^2,6^.0^8,12^]heptadeca-13,16-diene-3,5,9,11-tetrone <i>p</i>-xylene hemisolvate
Noland, Wayland E.; Kroll, Neil J.; Huisenga, Matthew P.; Yue, Ruixian A.; Lang, Simon B.; Klein, Nathan D.; Tritch, Kenneth J.; Acta Crystallographica Section E 70 (2014) 550–554; doi:10.1107/S1600536814025094

data_2240236
_publ_section_title
;
 Crystal structure of
 (1<i>S</i>,2<i>R</i>,6<i>R</i>,7<i>R</i>,8<i>S</i>,12<i>S</i>)-4,10,17-triphenyl-15-thia-4,10-diazapentacyclo[5.5.5.0^1,16^.0^2,6^.0^8,12^]heptadeca-13,16-diene-3,5,9,11-tetrone
 <i>p</i>-xylene hemisolvate
;
_journal_coeditor_code           SU5020
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              550
_journal_page_last               554
_journal_paper_doi               10.1107/S1600536814025094
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C32 H22 N2 O4 S, 0.5C8 H10'
_chemical_formula_moiety         'C32 H22 N2 O4 S, 0.5(C8 H10)'
_chemical_formula_sum            'C36 H27 N2 O4 S'
_chemical_formula_weight         583.65
_chemical_melting_point          554
_chemical_name_common            14156a
_chemical_name_systematic
'(1<i>S</i>,2<i>R</i>,6<i>R</i>,7<i>R</i>,8<i>S</i>,12<i>S</i>)-4,10,17-Triphenyl-15-thia-4,10-diazapentacyclo[5.5.5.0^1,16^.0^2,6^.0^8,12^]heptadeca-13,16-diene-3,5,9,11-tetrone <i>p</i>-xylene hemisolvate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 99.675(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5944(14)
_cell_length_b                   26.529(4)
_cell_length_c                   10.4286(14)
_cell_measurement_reflns_used    2771
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.38
_cell_measurement_theta_min      3.07
_cell_volume                     2889.4(7)
_computing_cell_refinement
;
SAINT (Bruker, 2007)
;
_computing_data_collection
;
APEX2 (Bruker, 2007)
;
_computing_data_reduction
;
SAINT (Bruker, 2007)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>, 2008)
;
_computing_publication_material
;
SHELXTL2008 (Sheldrick, 2008), enCIFer (Allen <i>et al.</i>,
2004) and
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            33190
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.406
_diffrn_reflns_theta_min         1.950
_exptl_absorpt_coefficient_mu    0.157
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6850
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 1996)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1220
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.220
_refine_diff_density_max         0.375
_refine_diff_density_min         -0.362
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         6576
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0399
_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^)+(0.0547P)^2^+1.9057P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1049
_refine_ls_wR_factor_ref         0.1091
_reflns_number_gt                5803
_reflns_number_total             6576
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            su5020sup1.cif
_cod_data_source_block           I
_cod_database_code               2240236
_cod_database_fobs_code          2240236
_shelx_estimated_absorpt_t_min   0.933
_shelx_estimated_absorpt_t_max   0.966
_shelx_hkl_checksum              58430
_shelx_res_checksum              43611
_shelxl_version_number           2.014