2,7-di-p-Chlorobenzoylnaphtho[2?3?-4 : 5]thiepin: a conformationally flexible new host molecule showing solvatochromic effects
Ballie, Laura; Farrugia, Louis J.; MacNicol, David D.; MacSween, Ross; CrystEngComm 6 (2004) 326–; doi:10.1039/b414315a

data_7216188
_publ_section_title
;
 2,7-di-p-Chlorobenzoylnaphtho[2?3?-4 : 5]thiepin: a conformationally
 flexible new host molecule showing solvatochromic effects
;
_journal_issue                   58
_journal_name_full               CrystEngComm
_journal_page_first              326
_journal_paper_doi               10.1039/b414315a
_journal_volume                  6
_journal_year                    2004
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C28 H16 Cl2 O2 S'
_chemical_formula_sum            'C28 H16 Cl2 O2 S'
_chemical_formula_weight         487.37
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2004-03-08T16:27:37-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 99.564(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9910(13)
_cell_length_b                   10.2442(8)
_cell_length_c                   15.5461(13)
_cell_measurement_reflns_used    5303
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      2.19
_cell_measurement_wavelength     0.71073
_cell_volume                     2197.2(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.588179E-1
_diffrn_orient_matrix_UB_12      -0.246627E-1
_diffrn_orient_matrix_UB_13      0.426907E-1
_diffrn_orient_matrix_UB_21      -0.422453E-1
_diffrn_orient_matrix_UB_22      -0.27774E-1
_diffrn_orient_matrix_UB_23      0.426435E-1
_diffrn_orient_matrix_UB_31      -0.30717E-2
_diffrn_orient_matrix_UB_32      -0.902734E-1
_diffrn_orient_matrix_UB_33      -0.24783E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.041
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            5040
_diffrn_reflns_reduction_process
;
Scaled and merged with SORTAV
R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.39
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.416
_exptl_absorpt_correction_T_max  0.955
_exptl_absorpt_correction_T_min  0.873
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
P. Coppens, L. Leiserowitz, D Rabinovich, Acta Cryst.
(1965), 18, 1035-1038
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.284
_refine_diff_density_min         -0.28
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         5040
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0541P)^2^+0.8037P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1025
_refine_ls_wR_factor_ref         0.1099
_reflns_number_gt                4060
_reflns_number_total             5040
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b414315a.txt
_cod_data_source_block           unsolvated
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_database_code               7216188