Crystal structure of 4,5,6,7,8,8-hexachloro-2-(3,4-dimethoxyphenethyl)-3a,4,7,7a-tetrahydro-1<i>H</i>-4,7-methanoisoindole-1,3(2<i>H</i>)-dione [+solvent]
Manohar, R.; Harikrishna, M.; Etti, S. Harikrishna; Ramanathan, C.; Gunasekaran, K.; Acta Crystallographica Section E 75 (2019) 562–564; doi:10.1107/S2056989019004109

data_2242884
_publ_section_title
;
 Crystal structure of
 4,5,6,7,8,8-hexachloro-2-(3,4-dimethoxyphenethyl)-3a,4,7,7a-tetrahydro-1<i>H</i>-4,7-methanoisoindole-1,3(2<i>H</i>)-dione
 [+solvent]
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              562
_journal_page_last               564
_journal_paper_doi               10.1107/S2056989019004109
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          'C19 H15 Cl6 N O4 [+ solvent]'
_chemical_formula_moiety         'C19 H15 Cl6 N O4'
_chemical_formula_sum            'C19 H15 Cl6 N O4'
_chemical_formula_weight         534.02
_chemical_name_systematic
4,5,6,7,8,8-Hexachloro-2-(3,4-dimethoxyphenethyl)-3a,4,7,7a-tetrahydro-1<i>H</i>-4,7-methanoisoindole-1,3(2<i>H</i>)-dione
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a'
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_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            16
_cell_length_a                   29.6250(9)
_cell_length_b                   29.6250(9)
_cell_length_c                   10.2427(4)
_cell_measurement_reflns_used    5181
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.232
_cell_measurement_theta_min      2.750
_cell_volume                     8989.4(5)
_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)
;
_computing_publication_material
;
SHELXL2018 (Sheldrick, 2015) and PLATON (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL2018 (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 0.847
_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  0.0209
_diffrn_reflns_av_unetI/netI     0.0418
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10728
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.232
_diffrn_reflns_theta_min         2.750
_exptl_absorpt_coefficient_mu    0.791
_exptl_absorpt_correction_T_max  0.863
_exptl_absorpt_correction_T_min  0.752
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Bruker, 2008)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_description       block
_exptl_crystal_F_000             4320
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.326
_refine_diff_density_min         -0.210
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         5181
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0781
_refine_ls_R_factor_gt           0.0414
_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^)+(0.0460P)^2^+2.6033P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0914
_refine_ls_wR_factor_ref         0.1011
_reflns_number_gt                3330
_reflns_number_total             5181
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            su5485sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        8989.4(6)
_cod_database_code               2242884
_cod_database_fobs_code          2242884
_shelx_hkl_checksum              78419
_shelx_res_checksum              33447
_shelx_fab_checksum              84427