Tetraphosphinitoresorcinarene Complexes: Dynamic Clusters with Silver(I) and Copper(I) Halides
Dana J. Eisler; Christopher W. Kirby; Richard J. Puddephatt; Inorganic Chemistry 42 (2003) 7626–7634; doi:10.1021/ic034717+

data_4327480
_publ_section_title
;
 Tetraphosphinitoresorcinarene Complexes: Dynamic Clusters with Silver(I)
 and Copper(I) Halides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7626
_journal_page_last               7634
_journal_paper_doi               10.1021/ic034717+
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C134.5 H111 Ag2 Cl6.5 F3 O15.25 P4 S5'
_chemical_formula_weight         2758.58
_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                79.25(3)
_cell_angle_beta                 73.09(3)
_cell_angle_gamma                63.73(3)
_cell_formula_units_Z            2
_cell_length_a                   18.426(4)
_cell_length_b                   19.698(4)
_cell_length_c                   21.242(4)
_cell_measurement_temperature    150(2)
_cell_volume                     6600(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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.078
_diffrn_reflns_av_sigmaI/netI    0.1098
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            62659
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         2.58
_exptl_absorpt_coefficient_mu    0.621
_exptl_absorpt_correction_T_max  0.9072
_exptl_absorpt_correction_T_min  0.8453
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_description       block
_exptl_crystal_F_000             2823
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.093
_refine_diff_density_min         -1.276
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1401
_refine_ls_number_reflns         22445
_refine_ls_number_restraints     82
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1484
_refine_ls_R_factor_gt           0.0913
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1391P)^2^+38.1600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2436
_refine_ls_wR_factor_ref         0.2822
_reflns_number_gt                13776
_reflns_number_total             22445
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0347172Bsi20030623_114635_3.cif
_cod_data_source_block           16
_cod_original_cell_volume        6600(2)
_cod_original_formula_sum        'C134.50 H111 Ag2 Cl6.50 F3 O15.25 P4 S5'
_cod_database_code               4327480