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_4080630
_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            'C56 H52 Cu2 F12 N14 P2 Pd S2'
_chemical_formula_weight         1508.66
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.757(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.9642(17)
_cell_length_b                   22.8560(18)
_cell_length_c                   23.8791(19)
_cell_measurement_reflns_used    9943
_cell_measurement_temperature    198(2)
_cell_measurement_theta_max      23.60
_cell_measurement_theta_min      2.29
_cell_volume                     12387.3(17)
_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      198(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX'
_diffrn_measurement_method       '\f and \w scans'
_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  0.1499
_diffrn_reflns_av_sigmaI/netI    0.0792
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            97291
_diffrn_reflns_theta_full        25.15
_diffrn_reflns_theta_max         25.15
_diffrn_reflns_theta_min         1.26
_exptl_absorpt_coefficient_mu    1.174
_exptl_absorpt_correction_T_max  0.9120
_exptl_absorpt_correction_T_min  0.6511
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Sheldrick, G. M. (2008). <i>SADABS</i>. University of G\"ottingen, Germany.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             6080
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.074
_refine_diff_density_min         -0.708
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     873
_refine_ls_number_reflns         11060
_refine_ls_number_restraints     882
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0924
_refine_ls_R_factor_gt           0.0561
_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^)+(0.0605P)^2^+42.5697P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1304
_refine_ls_wR_factor_ref         0.1557
_reflns_number_gt                7591
_reflns_number_total             11060
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400143u_si_003.cif
_cod_data_source_block           sho19
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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      C2/c
_cod_database_code               4080630