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_7217379
_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 H24 Br N4 O3 P S2'
_chemical_formula_sum            'C19 H24 Br N4 O3 P S2'
_chemical_formula_weight         531.42
_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                98.558(15)
_cell_angle_beta                 108.643(15)
_cell_angle_gamma                97.790(15)
_cell_formula_units_Z            2
_cell_length_a                   8.5957(13)
_cell_length_b                   11.821(2)
_cell_length_c                   12.807(2)
_cell_measurement_reflns_used    2742
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.2389
_cell_measurement_theta_min      1.7110
_cell_volume                     1195.8(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.933
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_device_type  'MAR345 image plate'
_diffrn_measurement_method       '79 images, \D\F 3.0\%'
_diffrn_radiation_monochromator  'Zr filter'
_diffrn_radiation_source         'Rigaku Ultra 18 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_av_sigmaI/netI    0.0498
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8518
_diffrn_reflns_theta_full        25.29
_diffrn_reflns_theta_max         25.29
_diffrn_reflns_theta_min         2.53
_exptl_absorpt_coefficient_mu    1.987
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70214
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.66
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.685
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         4077
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0424
_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^)+(0.0562P)^2^+1.0846P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1101
_refine_ls_wR_factor_ref         0.1141
_reflns_number_gt                3618
_reflns_number_total             4077
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7216249
_cod_data_source_file            c4ce00598h2.cif
_cod_data_source_block           4
_cod_database_code               7217379