Structures and Conformational Dynamics of Gold(I) Halide Complexes of Resorcinarene Tetraphosphinite Ligands
Dana J. Eisler; Richard J. Puddephatt; Inorganic Chemistry 42 (2003) 6352–6365; doi:10.1021/ic034430c

data_4314361
_publ_section_title
;
 Structures and Conformational Dynamics of Gold(I) Halide Complexes of
 Resorcinarene Tetraphosphinite Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6352
_journal_page_last               6365
_journal_paper_doi               10.1021/ic034430c
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C146 H136 Au4 Br4 O16.5 P4 S4'
_chemical_formula_weight         3514.17
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 114.7290(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   39.2913(3)
_cell_length_b                   17.43990(10)
_cell_length_c                   24.9380(2)
_cell_measurement_temperature    200(2)
_cell_volume                     15521.4(2)
_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      200(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.064
_diffrn_reflns_av_sigmaI/netI    0.0428
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            119810
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    4.950
_exptl_absorpt_correction_T_max  0.5655
_exptl_absorpt_correction_T_min  0.2142
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6896
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         2.939
_refine_diff_density_min         -2.179
_refine_diff_density_rms         0.195
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     763
_refine_ls_number_reflns         17808
_refine_ls_number_restraints     142
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0743
_refine_ls_R_factor_gt           0.0506
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1092P)^2^+77.9038P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1626
_refine_ls_wR_factor_ref         0.1790
_reflns_number_gt                13242
_reflns_number_total             17808
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034430csi20030423_013503_10.cif
_cod_data_source_block           10b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 
;
_cod_original_cell_volume        15521.35(19)
_cod_original_formula_sum        'C146 H136 Au4 Br4 O16.50 P4 S4'
_cod_database_code               4314361