3,4',5-Trichlorobiphenyl-4-yl 2,2,2-trichloroethyl sulfate
Lehmler, Hans-Joachim; He, Xianran; Duffel, Michael W.; Parkin, Sean; Acta Crystallographica Section E 69 (2013) o620–; doi:10.1107/S1600536813007976

data_2237740
_publ_section_title
;
 3,4',5-Trichlorobiphenyl-4-yl 2,2,2-trichloroethyl sulfate
;
_journal_coeditor_code           YK2088
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o620
_journal_paper_doi               10.1107/S1600536813007976
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C14 H8 Cl6 O4 S'
_chemical_formula_moiety         'C14 H8 Cl6 O4 S'
_chemical_formula_sum            'C14 H8 Cl6 O4 S'
_chemical_formula_weight         484.96
_chemical_name_systematic
;
3,4',5-Trichlorobiphenyl-4-yl 2,2,2-trichloroethyl sulfate
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.993(3)
_cell_length_b                   9.1890(18)
_cell_length_c                   28.778(6)
_cell_measurement_reflns_used    9992
_cell_measurement_temperature    90.0(2)
_cell_measurement_theta_max      68.29
_cell_measurement_theta_min      3.07
_cell_volume                     3700.3(13)
_computing_cell_refinement       'SAINT (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'SAINT (Bruker, 2006)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008) and local procedures
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90.0(2)
_diffrn_detector_area_resol_mean 5.6
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker X8 Proteum'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'graded multilayer optics'
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0619
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_diffrn_reflns_limit_h_max       16
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_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            45894
_diffrn_reflns_theta_full        68.40
_diffrn_reflns_theta_max         68.40
_diffrn_reflns_theta_min         3.07
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.705
_exptl_absorpt_correction_T_max  0.830
_exptl_absorpt_correction_T_min  0.504
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2006)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.741
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       flake
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.963
_refine_diff_density_min         -0.846
_refine_ls_abs_structure_details 'Flack (1983), 3176 Friedel pairs'
_refine_ls_abs_structure_Flack   0.15(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         6651
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.152
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0643
_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^)+(0.0514P)^2^+21.3733P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1580
_refine_ls_wR_factor_ref         0.1605
_reflns_number_gt                6238
_reflns_number_total             6651
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            yk2088.cif
_cod_data_source_block           I
_cod_database_code               2237740
_cod_database_fobs_code          2237740