Low-Melting Dialkyl- and Bis(polyfluoroalkyl)-Substituted 1,1‘-Methylenebis(imidazolium) and 1,1‘-Methylenebis(1,2,4-triazolium) Bis(trifluoromethanesulfonyl)amides: Ionic Liquids Leading to Bis(N-heterocyclic carbene) Complexes of Palladium
Jin, Chuan-Ming; Twamley, Brendan; Shreeve, Jean'ne M.; Organometallics 24 (2005) 3020–; doi:10.1021/om050210q

data_4075857
_publ_section_title
;
 Low-Melting Dialkyl- and Bis(polyfluoroalkyl)-Substituted
 1,1&#x2018;-Methylenebis(imidazolium) and
 1,1&#x2018;-Methylenebis(1,2,4-triazolium)
 Bis(trifluoromethanesulfonyl)amides:&#x00A0; Ionic Liquids Leading to
 Bis(N-heterocyclic carbene) Complexes of Palladium
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              3020
_journal_paper_doi               10.1021/om050210q
_journal_volume                  24
_journal_year                    2005
_chemical_formula_sum            'C16 H25.5 Cl2 N4.5 Pd'
_chemical_formula_weight         458.21
_chemical_name_common            'bis-diazolePdCl2 + 0.5MeCN'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 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                 102.214(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.1787(5)
_cell_length_b                   14.5223(6)
_cell_length_c                   13.3650(6)
_cell_measurement_reflns_used    9594
_cell_measurement_temperature    86(2)
_cell_measurement_theta_max      29.96
_cell_measurement_theta_min      2.29
_cell_volume                     1930.87(15)
_computing_cell_refinement       'Bruker SAINT+ v. 6.45'
_computing_data_collection       'Bruker SMART v. 5.626'
_computing_data_reduction        'Bruker SAINT+ v. 6.45'
_computing_molecular_graphics    'XP, Bruker SHELXTL v. 6.12'
_computing_publication_material  'XCIF, Bruker SHELXTL v. 6.12'
_computing_structure_refinement  'XL, Bruker SHELXTL v. 6.12'
_computing_structure_solution    'XS, Bruker SHELXTL v. 6.12'
_diffrn_ambient_temperature      86(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker/Siemens SMART APEX'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_sigmaI/netI    0.0355
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            29197
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.40
_diffrn_standards_decay_%        <0.01
_exptl_absorpt_coefficient_mu    1.244
_exptl_absorpt_correction_T_max  0.8963
_exptl_absorpt_correction_T_min  0.6168
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; SAINT+, 2001)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.576
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             932
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.263
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.104
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     429
_refine_ls_number_reflns         8854
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0311
_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^)+(0.0330P)^2^+1.9199P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0721
_refine_ls_wR_factor_ref         0.0725
_reflns_number_gt                8625
_reflns_number_total             8854
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om050210qsi20050425_112401.cif
_cod_data_source_block           bt682
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      Pn
_cod_original_formula_sum        'C16 H25.50 Cl2 N4.50 Pd'
_cod_database_code               4075857