Structure and Dynamics of Tetrakis(thiophosphinato)resorcinarene Complexes of Silver(I), Gold(I), and Palladium(II)
Eisler, Dana J.; Puddephatt, Richard J.; Inorganic Chemistry 45 (2006) 7295–7305; doi:10.1021/ic060865z

data_4332811
_publ_section_title
;
 Structure and Dynamics of Tetrakis(thiophosphinato)resorcinarene
 Complexes of Silver(I), Gold(I), and Palladium(II)
;
_journal_issue                   18
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7295
_journal_page_last               7305
_journal_paper_doi               10.1021/ic060865z
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C144.5 H120.5 Cl17.5 O16.5 P4 Pd2 S4'
_chemical_formula_weight         3206.20
_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                95.69(3)
_cell_angle_beta                 93.33(3)
_cell_angle_gamma                99.61(3)
_cell_formula_units_Z            2
_cell_length_a                   17.021(3)
_cell_length_b                   18.537(4)
_cell_length_c                   24.719(5)
_cell_measurement_temperature    150(2)
_cell_volume                     7630(3)
_computing_cell_refinement       'Nonius DENZO'
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'Nonius DENZO'
_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      150(2)
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'phi\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  0.0044
_diffrn_reflns_av_sigmaI/netI    0.0556
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            77039
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         2.55
_exptl_absorpt_coefficient_mu    0.698
_exptl_absorpt_correction_T_max  0.8847
_exptl_absorpt_correction_T_min  0.7441
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             3266
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.757
_refine_diff_density_min         -1.244
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1417
_refine_ls_number_reflns         24835
_refine_ls_number_restraints     195
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1166
_refine_ls_R_factor_gt           0.0848
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1469P)^2^+30.9000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2389
_refine_ls_wR_factor_ref         0.2692
_reflns_number_gt                17619
_reflns_number_total             24835
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060865zsup1.cif
_cod_data_source_block           19
_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_original_formula_sum        'C144.50 H120.50 Cl17.50 O16.50 P4 Pd2 S4'
_cod_database_code               4332811