Stepwise Deprotonation of a Thiol-Functionalized Bis(1,2,4-triazolium) Salt as a Selective Route to Heterometallic NHC Complexes
Seitz, Stefanie C.; Rominger, Frank; Straub, Bernd F.; Organometallics 32 (2013) 2427–; doi:10.1021/om400143u

data_4080629
_publ_section_title
;
 Stepwise Deprotonation of a Thiol-Functionalized Bis(1,2,4-triazolium)
 Salt as a Selective Route to Heterometallic NHC Complexes
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              2427
_journal_paper_doi               10.1021/om400143u
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C27.24 H24 F8.28 N6 O3.72 P0.76 S2.24'
_chemical_formula_weight         747.61
_chemical_name_systematic
; 
 ? 
;
_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                91.690(5)
_cell_angle_beta                 104.044(5)
_cell_angle_gamma                101.925(4)
_cell_formula_units_Z            2
_cell_length_a                   9.8719(12)
_cell_length_b                   12.4986(14)
_cell_length_c                   13.3487(17)
_cell_measurement_reflns_used    2437
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      22.65
_cell_measurement_theta_min      2.44
_cell_volume                     1557.8(3)
_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      200(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II Quazar'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'ImuS microsource'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0813
_diffrn_reflns_av_sigmaI/netI    0.0602
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            18031
_diffrn_reflns_theta_full        23.53
_diffrn_reflns_theta_max         23.53
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    0.321
_exptl_absorpt_correction_T_max  0.9873
_exptl_absorpt_correction_T_min  0.9242
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platte
_exptl_crystal_F_000             762
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.263
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     572
_refine_ls_number_reflns         4601
_refine_ls_number_restraints     528
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0945
_refine_ls_R_factor_gt           0.0587
_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^)+(0.0559P)^2^+2.0405P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1350
_refine_ls_wR_factor_ref         0.1534
_reflns_number_gt                3058
_reflns_number_total             4601
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400143u_si_003.cif
_cod_data_source_block           sho11
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4080629