Syntheses of, and structural studies on, benzo-fused 1,2,4-thiadiazines
Clark, Ewan R.; Hayward, John J.; Leontowicz, Bryce J.; Eisler, Dana J.; Rawson, Jeremy M.; CrystEngComm 16 (2014) 1755–; doi:10.1039/c3ce42205d

data_7214075
_publ_section_title
;
 Syntheses of, and structural studies on, benzo-fused 1,2,4-thiadiazines
;
_journal_issue                   9
_journal_name_full               CrystEngComm
_journal_page_first              1755
_journal_paper_doi               10.1039/c3ce42205d
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety         'C14 H9 F3 N2 S'
_chemical_formula_sum            'C14 H9 F3 N2 S'
_chemical_formula_weight         294.29
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.959(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   14.857(2)
_cell_length_b                   13.0971(19)
_cell_length_c                   26.970(4)
_cell_measurement_reflns_used    17034
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      0.76
_cell_volume                     5247.2(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT, SADABS and XPREP'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_sigmaI/netI    0.0596
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            17034
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         0.76
_exptl_absorpt_coefficient_mu    0.272
_exptl_absorpt_correction_T_max  0.9839
_exptl_absorpt_correction_T_min  0.9228
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2400
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.796
_refine_diff_density_min         -0.814
_refine_diff_density_rms         0.151
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.1(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         7611
_refine_ls_number_restraints     326
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.1131
_refine_ls_R_factor_gt           0.1056
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1726P)^2^+98.2599P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3009
_refine_ls_wR_factor_ref         0.3112
_reflns_number_gt                7072
_reflns_number_total             7611
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce42205d.txt
_cod_data_source_block           compound_9
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        5247.0(13)
_cod_original_sg_symbol_H-M      Cc
_cod_database_code               7214075