Auration, Argentation, and Mercuration Reactions of an Iridaphosphirene
Markus Brym; Cameron Jones; James D. E. T. Wilton-Ely; Inorganic Chemistry 44 (2005) 3275–3282; doi:10.1021/ic048532u

data_4308829
_publ_contact_author_name        'James D. Wilton-Ely'
_publ_section_title
;
Auration, Argentation, and Mercuration Reactions of an Iridaphosphirene
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3275
_journal_page_last               3282
_journal_paper_doi               10.1021/ic048532u
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C77.5 H77 Au F3 Ir O4 P4 S'
_chemical_formula_weight         1674.50
_space_group_IT_number           9
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 114.34(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.603(6)
_cell_length_b                   12.948(3)
_cell_length_c                   24.642(5)
_cell_measurement_temperature    150(2)
_cell_volume                     8024(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_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  0.0592
_diffrn_reflns_av_sigmaI/netI    0.0769
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            25680
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.95
_exptl_absorpt_coefficient_mu    3.639
_exptl_absorpt_correction_T_max  0.364
_exptl_absorpt_correction_T_min  0.283
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav (Blessing, 1995)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3332
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.729
_refine_diff_density_min         '-0.774 (near Ir1)'
_refine_diff_density_rms         0.178
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.002(8)
_refine_ls_extinction_coef       0.00000(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     792
_refine_ls_number_reflns         14523
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0665
_refine_ls_R_factor_gt           0.0544
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0715P)^2^+81.6980P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1324
_refine_ls_wR_factor_ref         0.1409
_reflns_number_gt                12672
_reflns_number_total             14523
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048532usi20041027_113733_3.cif
_cod_data_source_block           compound_3
_cod_original_cell_volume        8025(3)
_cod_original_formula_sum        'C77.50 H77 Au F3 Ir O4 P4 S'
_cod_database_code               4308829