First structurally characterized self-assembly of bipodal N-thiophosphorylated bis-thiourea with Co(II): magnetic properties and thermal decomposition.
Safin, Damir A.; Babashkina, Maria G.; Railliet, Antoine P.; Tumanov, Nikolay A.; Robeyns, Koen; Devlin, Eamonn; Sanakis, Yiannis; Filinchuk, Yaroslav; Garcia, Yann; Dalton transactions (Cambridge, England : 2003) 42 (2013) 5532–5538; doi:10.1039/c3dt50254f

data_7022914
_publ_section_title
;
 First structurally characterized self-assembly of bipodal
 N-thiophosphorylated bis-thiourea with Co(II): magnetic properties and
 thermal decomposition.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5532
_journal_page_last               5538
_journal_paper_doi               10.1039/c3dt50254f
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C4 H12 N2, 2(C2 H3 O2)'
_chemical_formula_sum            'C8 H18 N2 O4'
_chemical_formula_weight         206.24
_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                117.795(16)
_cell_angle_beta                 100.317(9)
_cell_angle_gamma                90.118(9)
_cell_formula_units_Z            1
_cell_length_a                   5.7855(3)
_cell_length_b                   7.0039(11)
_cell_length_c                   7.4459(11)
_cell_measurement_reflns_used    2246
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.6183
_cell_measurement_theta_min      3.1525
_cell_volume                     261.32(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection       MAR
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.925
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_device_type  'MAR345 image plate'
_diffrn_measurement_method       '180 images, \D\F 1.5\% '
_diffrn_radiation_monochromator  'Xenocs Fox3D mirror'
_diffrn_radiation_source         'Rigaku UltraX 18 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0194
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            913
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         25.70
_diffrn_reflns_theta_min         3.16
_exptl_absorpt_coefficient_mu    0.104
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97985
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colour
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             112
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.190
_refine_diff_density_min         -0.198
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.194
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     66
_refine_ls_number_reflns         913
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.194
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0448
_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^)+(0.0217P)^2^+0.2673P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1093
_refine_ls_wR_factor_ref         0.1096
_reflns_number_gt                898
_reflns_number_total             913
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt50254f.txt
_cod_data_source_block           safin262
_cod_original_cell_volume        261.32(6)
_cod_database_code               7022914