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_2016529
_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          'C16 H30 N4 O2 S2'
_chemical_formula_moiety         'C16 H30 N4 O2 S2'
_chemical_formula_sum            'C16 H30 N4 O2 S2'
_chemical_formula_weight         374.56
_chemical_name_systematic
;
3,3,3',3'-tetraethyl-1,1'-(butane-1,4-diyldicarbonyl)bis(thiourea)
;
_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
_cell_angle_alpha                85.532(3)
_cell_angle_beta                 86.985(3)
_cell_angle_gamma                81.894(3)
_cell_formula_units_Z            1
_cell_length_a                   4.8287(9)
_cell_length_b                   6.3977(12)
_cell_length_c                   15.661(3)
_cell_measurement_reflns_used    1762
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.128
_cell_measurement_theta_min      2.6115
_cell_volume                     477.09(16)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0588
_diffrn_reflns_av_sigmaI/netI    0.0600
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            4902
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.61
_exptl_absorpt_coefficient_mu    0.296
_exptl_absorpt_correction_T_max  0.9854
_exptl_absorpt_correction_T_min  0.8736
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             202
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.900
_refine_diff_density_min         -0.298
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     111
_refine_ls_number_reflns         1847
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.163
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0622
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc w=1/[\\s\^2\^(Fo\^2\^)+(0.0857P)\^2\^]
where P=(Fo\^2\^+2Fc\^2\^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1501
_refine_ls_wR_factor_ref         0.1556
_reflns_number_gt                1611
_reflns_number_total             1847
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            tr3036.cif
_cod_data_source_block           II
_cod_database_code               2016529
_cod_database_fobs_code          2016529