Efficient solvent-controlled crystallization of pure polymorphs of 1-nitro-4-(4-nitrophenylmethylthio)benzene
Wan, Chong-Qing; Li, Ai-Min; Al-Thabaiti, Shaeel A.; El-Mosslamy, El-Sayed H.; Mak, Thomas C. W.; CrystEngComm 16 (2014) 8960–; doi:10.1039/C4CE00753K

data_7216730
_publ_section_title
;
 Efficient solvent-controlled crystallization of pure polymorphs of
 1-nitro-4-(4-nitrophenylmethylthio)benzene
;
_journal_issue                   38
_journal_name_full               CrystEngComm
_journal_page_first              8960
_journal_paper_doi               10.1039/C4CE00753K
_journal_volume                  16
_journal_year                    2014
_chemical_formula_sum            'C13 H10 N2 O4 S'
_chemical_formula_weight         290.29
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                81.809(4)
_cell_angle_beta                 71.861(3)
_cell_angle_gamma                79.628(3)
_cell_formula_units_Z            8
_cell_length_a                   13.1030(7)
_cell_length_b                   13.8660(8)
_cell_length_c                   15.6862(10)
_cell_measurement_temperature    296(2)
_cell_volume                     2652.7(3)
_computing_cell_refinement       '<i>APEX2</i> and <i>SAINT</i> (Bruker 2007)'
_computing_data_collection       '<i>APEX2</i> (Bruker 2007)'
_computing_data_reduction        <i>SAINT</i>
_computing_molecular_graphics    '<i>SHELXTL</i> (Sheldrick, 2008)'
_computing_publication_material  '<i>SHELXTL</i> and <i>PLATON</i> (Spek,2009)'
_computing_structure_refinement  '<i>SHELXL-97</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SHELXS-97</i> (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_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  0.1028
_diffrn_reflns_av_sigmaI/netI    0.1610
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24715
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.37
_exptl_absorpt_coefficient_mu    0.258
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6364
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '<i>SADABS</i> (Bruker, 2007)'
_exptl_crystal_colour            White
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.763
_refine_diff_density_min         -0.585
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     721
_refine_ls_number_reflns         9332
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.2340
_refine_ls_R_factor_gt           0.0877
_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^)+(0.1158P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2065
_refine_ls_wR_factor_ref         0.2894
_reflns_number_gt                3256
_reflns_number_total             9332
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ce00753k2.cif
_cod_data_source_block           IV
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'Multi-SCAN'
changed to 'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/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 

 Adding full bibliography for 7216727--7216731.cif.
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7216730