Bipodal 1,1'-acyl-3,3,3',3'-tetraalkylbis(thiourea) ligands with flexible C~3~, C~4~ and C~6~ spacer groups
Stockmann, Susanne; Bruce, Jocelyn; Miller, Jorn; Koch, Klaus R.; Acta Crystallographica Section C 64 (2008) o166–o170; doi:10.1107/S0108270108002783

data_2016528
_publ_section_title
;
 Bipodal 1,1'-acyl-3,3,3',3'-tetraalkylbis(thiourea) ligands with
 flexible C~3~, C~4~ and C~6~ spacer groups
;
_journal_coeditor_code           TR3036
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o166
_journal_page_last               o170
_journal_paper_doi               10.1107/S0108270108002783
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C15 H28 N4 O2 S2'
_chemical_formula_moiety         'C15 H28 N4 O2 S2'
_chemical_formula_sum            'C15 H28 N4 O2 S2'
_chemical_formula_weight         360.53
_chemical_name_systematic
;
3,3,3',3'-Tetraethyl-1,1'-(propane-1,3-diyldicarbonyl)bis(thiourea)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 93.026(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.1475(18)
_cell_length_b                   27.999(7)
_cell_length_c                   9.387(2)
_cell_measurement_reflns_used    1566
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.97
_cell_measurement_theta_min      2.29
_cell_volume                     1875.9(8)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        'SAINT (Bruker, 2002)'
_computing_molecular_graphics
;
X-Seed (Version 2.0; Barbour, 2001)
;
_computing_publication_material
;
X-Seed (Version 2.0; Barbour, 2001)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX I CCD area-detector'
_diffrn_measurement_method       \\w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0503
_diffrn_reflns_av_sigmaI/netI    0.0635
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            10628
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.45
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.298
_exptl_absorpt_correction_T_max  0.9483
_exptl_absorpt_correction_T_min  0.9373
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.662
_refine_diff_density_min         -0.472
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         3685
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0525
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc w=1/[\\s\^2\^(Fo\^2\^)+(0.0666P)\^2\^]
where P=(Fo\^2\^+2Fc\^2\^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1199
_refine_ls_wR_factor_ref         0.1293
_reflns_number_gt                2845
_reflns_number_total             3685
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            tr3036.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2016528
_cod_database_fobs_code          2016528