Synthesis and first complexes of C(4/5) P-bifunctional imidazole-2-thiones.
Majhi, Paresh Kumar; Sauerbrey, Susanne; Leiendecker, Alexander; Schnakenburg, Gregor; Arduengo, 3rd, Anthony J; Streubel, Rainer; Dalton transactions (Cambridge, England : 2003) 42 (2013) 13126–13136; doi:10.1039/c3dt51557e

data_7023598
_publ_section_title
;
 Synthesis and first complexes of C(4/5) P-bifunctional
 imidazole-2-thiones.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13126
_journal_page_last               13136
_journal_paper_doi               10.1039/c3dt51557e
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C32 H32 N2 O2 P2 S'
_chemical_formula_sum            'C32 H32 N2 O2 P2 S'
_chemical_formula_weight         570.60
_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                104.978(4)
_cell_angle_beta                 104.629(3)
_cell_angle_gamma                111.483(3)
_cell_formula_units_Z            2
_cell_length_a                   11.6761(9)
_cell_length_b                   11.7150(11)
_cell_length_c                   12.7206(13)
_cell_measurement_reflns_used    2486
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.67
_cell_measurement_theta_min      2.77
_cell_volume                     1442.7(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker X8-KappaApexII'
_diffrn_measurement_method       '\f and \w CCD rotation images, thin slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_av_sigmaI/netI    0.0729
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12940
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.11
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.256
_exptl_absorpt_correction_T_max  0.9924
_exptl_absorpt_correction_T_min  0.9798
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (2009/2), Bruker AXS 2009'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.397
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.062
_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     354
_refine_ls_number_reflns         5525
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0762
_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
'calc w=1/[\s^2^(Fo^2^)+(0.0485P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0961
_refine_ls_wR_factor_ref         0.1079
_reflns_number_gt                3939
_reflns_number_total             5525
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt51557e.txt
_cod_data_source_block           Greg1608f
_cod_database_code               7023598