N-Salicylidene aniline derivatives based on the N′-thiophosphorylated thiourea scaffold
Safin, Damir A.; Babashkina, Maria G.; Robeyns, Koen; Bolte, Michael; Garcia, Yann; CrystEngComm 16 (2014) 7053–; doi:10.1039/C4CE00598H

data_7216250
_publ_section_title
;
 N-Salicylidene aniline derivatives based on the
 N&#x2032;-thiophosphorylated thiourea scaffold
;
_journal_issue                   30
_journal_name_full               CrystEngComm
_journal_page_first              7053
_journal_paper_doi               10.1039/C4CE00598H
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety         'C19 H23 Cl2 N4 O3 P S2'
_chemical_formula_sum            'C19 H23 Cl2 N4 O3 P S2'
_chemical_formula_weight         521.40
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                98.558(7)
_cell_angle_beta                 106.445(7)
_cell_angle_gamma                97.060(7)
_cell_formula_units_Z            2
_cell_length_a                   9.0052(8)
_cell_length_b                   11.7572(10)
_cell_length_c                   12.3225(11)
_cell_measurement_reflns_used    27751
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.825
_cell_measurement_theta_min      3.375
_cell_volume                     1218.5(2)
_computing_cell_refinement       'X-Area (Stoe & Cie, 2001)'
_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2001)'
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 1991)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0656
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            23183
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.462
_diffrn_reflns_theta_min         3.378
_exptl_absorpt_coefficient_mu    0.532
_exptl_absorpt_correction_T_max  0.9537
_exptl_absorpt_correction_T_min  0.8317
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'X-Area (Stoe & Cie, 2001)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             540
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.436
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         4997
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0436
_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^)+(0.0445P)^2^+0.4312P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0955
_refine_ls_wR_factor_ref         0.1001
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4205
_reflns_number_total             4997
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4ce00598h2.cif
_cod_data_source_block           ba16
_cod_depositor_comments
'Adding full bibliography for 7216246--7216251.cif.'
_cod_original_cell_volume        1218.47(19)
_cod_database_code               7216250
_shelx_estimated_absorpt_t_min   0.832
_shelx_estimated_absorpt_t_max   0.954
_shelxl_version_number           2013-3
_shelx_res_checksum              88290