Electronic Influences on Metallophilic Interactions in [Pt(tpy)X][Au(C6F5)2] Double Salts
Val Phillips; Kathryn J. Willard; James A. Golen; Curtis J. Moore; Arnold L. Rheingold; Linda H. Doerrer; Inorganic Chemistry 49 (2010) 9265–9274; doi:10.1021/ic1008208

data_4316732
_publ_section_title
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 Electronic Influences on Metallophilic Interactions in
 [Pt(tpy)X][Au(C6F5)2] Double Salts
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9265
_journal_page_last               9274
_journal_paper_doi               10.1021/ic1008208
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C49 H41 F12 N7 O2 P2 Pt2'
_chemical_formula_weight         1440.01
_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                89.604(4)
_cell_angle_beta                 69.444(4)
_cell_angle_gamma                71.091(4)
_cell_formula_units_Z            2
_cell_length_a                   13.1966(17)
_cell_length_b                   14.043(2)
_cell_length_c                   14.635(2)
_cell_measurement_reflns_used    3075
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      2.66
_cell_volume                     2384.9(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.907
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0450
_diffrn_reflns_av_sigmaI/netI    0.0486
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            37063
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    6.024
_exptl_absorpt_correction_T_max  0.7139
_exptl_absorpt_correction_T_min  0.3788
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            bronze
_exptl_crystal_density_diffrn    2.005
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1388
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         3.033
_refine_diff_density_min         -2.075
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     732
_refine_ls_number_reflns         10818
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1301
_refine_ls_wR_factor_ref         0.1446
_reflns_number_gt                8425
_reflns_number_total             10818
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1008208_si_001_2.cif
_cod_data_source_block           lhd209_Compound_2
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
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_cod_original_cell_volume        2384.8(6)
_cod_database_code               4316732
_comments
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Hydrogen atoms on DMF were not located. Eight were added to the 
unit card to correct the molecular formula and density and F000 value. 

Disorder of C(O)-H with CH3 noted and treated using EXYZ/EADP.

alert 417 - type A - short H...H contact . Various attempts were made
to located hydrogen atom positions on atom O2 of water and all resulted in
alert 417 - type A. Hydrogen atoms H2b and H2c were kept in the unit card and 
listing to illustrate the bonding arragnement. 
;