Haloaurate and halopalladate imidazolium salts: structures, properties, and use as precursors for catalytic metal nanoparticles.
Serpell, Christopher J.; Cookson, James; Thompson, Amber L.; Brown, Christopher M.; Beer, Paul D.; Dalton transactions (Cambridge, England : 2003) 42 (2013) 1385–1393; doi:10.1039/c2dt31984e

data_7020782
_publ_section_title
;
 Haloaurate and halopalladate imidazolium salts: structures, properties,
 and use as precursors for catalytic metal nanoparticles.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1385
_journal_page_last               1393
_journal_paper_doi               10.1039/c2dt31984e
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         '2(C11 H21 N2), Cl4 Pd'
_chemical_formula_sum            'C22 H42 Cl4 N4 Pd'
_chemical_formula_weight         610.81
_chemical_melting_point          477
_chemical_name_systematic
;
1,3-Di-tert-butyl-1H-imidazol-3-ium tetrachloropalladate
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             10-07-01
_audit_creation_method           CRYSTALS_ver_14.07
_cell_angle_alpha                90
_cell_angle_beta                 125.898(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.3545(7)
_cell_length_b                   9.4171(5)
_cell_length_c                   10.5259(5)
_cell_measurement_reflns_used    1422
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     1393.50(12)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.031
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5045
_diffrn_reflns_theta_full        25.567
_diffrn_reflns_theta_max         27.491
_diffrn_reflns_theta_min         5.212
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.066
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.73
_refine_diff_density_min         -0.88
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9309
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     91
_refine_ls_number_reflns         1673
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0344
_refine_ls_shift/su_max          0.0073888
_refine_ls_shift/su_mean         0.0019629
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
8.34 11.1 5.53 1.66
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0943
_refine_ls_wR_factor_gt          0.0769
_refine_ls_wR_factor_ref         0.0943
_reflns_limit_h_max              18
_reflns_limit_h_min              -22
_reflns_limit_k_max              12
_reflns_limit_k_min              0
_reflns_limit_l_max              13
_reflns_limit_l_min              0
_reflns_number_gt                1361
_reflns_number_total             1673
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.05
_oxford_diffrn_Wilson_scale      62.87
_oxford_refine_ls_r_factor_ref   0.0504
_oxford_refine_ls_scale          0.18245(16)
_oxford_reflns_number_all        1673
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 029CJS10
_cod_data_source_file            c2dt31984e.txt
_cod_data_source_block           4c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'C 2/m '
_cod_original_formula_sum        'C22 H42 Cl4 N4 Pd1'
_cod_database_code               7020782