data_Global _audit_creation_method SHELXL-97 #------------------------------------------------------------------------------ _publ_contact_author ; Masood Parvez Department of Chemistry University of Calgary 2500 University Drive N.W. Calgary, Alberta, Canada T2N 1N4 ; #----------------------------------------------------------------------------- _publ_requested_journal ' ? ' _publ_requested_coeditor_name ' ? ' _publ_contact_author_phone ' (403)220-5348 ' _publ_contact_author_fax ' (403)289-9488 ' _publ_contact_author_email ' parvez@ucalgary.ca ' #------------------------------------------------------------------------------ _publ_section_title ; ? ; loop_ _publ_author_name _publ_author_address 'Parvez, Masood' ; Department of Chemistry The University of Calgary 2500 University Drive NW Calgary Alberta Canada T2N 1N4 ; #------------------------------------------------------------------------------ data_Compound_I #----------------------------------------------------------------------------- _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'HKL DENZO (Otwinowski & Minor, 1997)' _computing_data_reduction 'SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1991)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' #----------------------------------------------------------------------------- _vrf_PUBL012_GLOBAL ; PROBLEM: _publ_section_abstract is missing. RESPONSE: Will appear in the paper ; # end Validation Reply Form _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H72 Ir2 O P4' _chemical_formula_sum 'C50 H72 Ir2 O P4' _chemical_formula_weight 1197.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ir' 'Ir' -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Tetragonal' _symmetry_space_group_name_H-M 'I 41/a' _symmetry_space_group_name_Hall '-I 4ad' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z' '-y+3/4, x+1/4, z+1/4' 'y+1/4, -x+1/4, z+1/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1, z+1/2' '-y+5/4, x+3/4, z+3/4' 'y+3/4, -x+3/4, z+3/4' '-x, -y, -z' 'x, y-1/2, -z' 'y-3/4, -x-1/4, -z-1/4' '-y-1/4, x-1/4, -z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' '-y+1/4, x+1/4, -z+1/4' _cell_length_a 17.4249(4) _cell_length_b 17.4249(4) _cell_length_c 16.3359(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4960.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2711 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description 'Block' _exptl_crystal_colour 'Blue' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.603 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2376 _exptl_absorpt_coefficient_mu 5.524 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.4046 _exptl_absorpt_correction_T_max 0.5570 _exptl_absorpt_process_details 'SORTAV: (Blessing, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius APEX2 CCD' _diffrn_measurement_method ' \w and \f scans ' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4488 _diffrn_reflns_av_R_equivalents 0.0220 _diffrn_reflns_av_sigmaI/netI 0.0274 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.42 _diffrn_reflns_theta_max 27.47 _reflns_number_total 2818 _reflns_number_gt 2469 _reflns_threshold_expression >2sigma(I) _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0056P)^2^+35.4237P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2818 _refine_ls_number_parameters 134 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0321 _refine_ls_R_factor_gt 0.0255 _refine_ls_wR_factor_ref 0.0586 _refine_ls_wR_factor_gt 0.0539 _refine_ls_goodness_of_fit_ref 1.115 _refine_ls_restrained_S_all 1.115 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.5000 0.2500 0.493953(11) 0.01906(7) Uani 1 2 d S . . P1 P 0.36948(5) 0.24701(6) 0.51394(6) 0.02130(19) Uani 1 1 d . . . O1 O 0.5000 0.2500 0.3750 0.0213(10) Uani 1 4 d S . . C1 C 0.5000 0.2500 0.6125(3) 0.0242(11) Uani 1 2 d S . . C2 C 0.4346(2) 0.2171(2) 0.6592(2) 0.0253(8) Uani 1 1 d . . . C3 C 0.3637(2) 0.2126(2) 0.6190(2) 0.0254(8) Uani 1 1 d . . . C4 C 0.3002(3) 0.1802(3) 0.6571(3) 0.0344(9) Uani 1 1 d . . . H4 H 0.2523 0.1788 0.6293 0.041 Uiso 1 1 calc R . . C5 C 0.3063(3) 0.1498(3) 0.7355(3) 0.0394(11) Uani 1 1 d . . . H5 H 0.2629 0.1278 0.7615 0.047 Uiso 1 1 calc R . . C6 C 0.3765(3) 0.1521(3) 0.7750(3) 0.0367(10) Uani 1 1 d . . . H6 H 0.3813 0.1307 0.8283 0.044 Uiso 1 1 calc R . . C7 C 0.4398(3) 0.1853(2) 0.7380(3) 0.0325(9) Uani 1 1 d . . . H7 H 0.4874 0.1865 0.7663 0.039 Uiso 1 1 calc R . . C8 C 0.3225(2) 0.3427(2) 0.5171(3) 0.0286(8) Uani 1 1 d . . . H8 H 0.3294 0.3666 0.4619 0.034 Uiso 1 1 calc R . . C9 C 0.3644(3) 0.3938(3) 0.5788(3) 0.0386(10) Uani 1 1 d . . . H9A H 0.3438 0.4460 0.5759 0.046 Uiso 1 1 calc R . . H9B H 0.4193 0.3947 0.5658 0.046 Uiso 1 1 calc R . . H9C H 0.3570 0.3733 0.6341 0.046 Uiso 1 1 calc R . . C10 C 0.2364(2) 0.3410(3) 0.5346(3) 0.0354(10) Uani 1 1 d . . . H10A H 0.2166 0.3936 0.5368 0.042 Uiso 1 1 calc R . . H10B H 0.2273 0.3155 0.5872 0.042 Uiso 1 1 calc R . . H10C H 0.2101 0.3126 0.4911 0.042 Uiso 1 1 calc R . . C11 C 0.3016(2) 0.1860(2) 0.4567(3) 0.0278(8) Uani 1 1 d . . . H11 H 0.2501 0.1900 0.4834 0.033 Uiso 1 1 calc R . . C12 C 0.3272(3) 0.1021(2) 0.4600(3) 0.0367(10) Uani 1 1 d . . . H12A H 0.2908 0.0703 0.4294 0.044 Uiso 1 1 calc R . . H12B H 0.3290 0.0850 0.5171 0.044 Uiso 1 1 calc R . . H12C H 0.3784 0.0973 0.4355 0.044 Uiso 1 1 calc R . . C13 C 0.2943(2) 0.2146(3) 0.3684(3) 0.0329(9) Uani 1 1 d . . . H13A H 0.2590 0.1812 0.3382 0.039 Uiso 1 1 calc R . . H13B H 0.3449 0.2136 0.3420 0.039 Uiso 1 1 calc R . . H13C H 0.2745 0.2672 0.3684 0.039 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.01864(11) 0.02068(11) 0.01788(10) 0.000 0.000 -0.00043(8) P1 0.0194(5) 0.0216(5) 0.0228(4) -0.0010(4) 0.0015(4) 0.0001(4) O1 0.020(3) 0.025 0.019(2) 0.000 0.000 0.000 C1 0.024(3) 0.023(3) 0.026(3) 0.000 0.000 0.000(2) C2 0.028(2) 0.026(2) 0.0218(18) 0.0000(15) 0.0040(15) 0.0043(15) C3 0.0262(19) 0.0257(19) 0.0243(18) -0.0020(16) 0.0044(16) 0.0012(15) C4 0.032(2) 0.037(2) 0.035(2) -0.0001(19) 0.0055(18) -0.0002(19) C5 0.044(3) 0.039(3) 0.035(2) 0.007(2) 0.019(2) -0.002(2) C6 0.045(3) 0.037(2) 0.028(2) 0.0103(18) 0.0139(19) 0.008(2) C7 0.032(2) 0.037(2) 0.028(2) 0.0027(17) 0.0043(17) 0.0088(18) C8 0.031(2) 0.026(2) 0.029(2) 0.0003(16) 0.0021(17) 0.0035(16) C9 0.045(3) 0.027(2) 0.044(3) -0.0089(19) -0.001(2) 0.0023(19) C10 0.031(2) 0.037(2) 0.038(2) -0.0009(19) 0.0034(19) 0.0130(18) C11 0.0236(19) 0.028(2) 0.031(2) -0.0063(17) -0.0010(16) -0.0023(16) C12 0.042(3) 0.025(2) 0.044(3) -0.0023(19) 0.000(2) -0.0016(18) C13 0.030(2) 0.038(2) 0.031(2) -0.0051(18) -0.0072(18) -0.0055(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 C1 1.936(5) . ? Ir1 O1 1.94321(19) . ? Ir1 P1 2.2982(9) . ? Ir1 P1 2.2982(9) 2_655 ? P1 C3 1.821(4) . ? P1 C11 1.844(4) . ? P1 C8 1.859(4) . ? O1 Ir1 1.94321(19) 11_666 ? C1 C2 1.486(5) 2_655 ? C1 C2 1.486(5) . ? C2 C3 1.401(6) . ? C2 C7 1.405(6) . ? C3 C4 1.390(6) . ? C4 C5 1.390(6) . ? C4 H4 0.9500 . ? C5 C6 1.384(7) . ? C5 H5 0.9500 . ? C6 C7 1.384(6) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C10 1.528(6) . ? C8 C9 1.530(6) . ? C8 H8 1.0000 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.529(6) . ? C11 C13 1.532(6) . ? C11 H11 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ir1 O1 180.000(1) . . ? C1 Ir1 P1 81.83(2) . . ? O1 Ir1 P1 98.17(2) . . ? C1 Ir1 P1 81.83(2) . 2_655 ? O1 Ir1 P1 98.17(2) . 2_655 ? P1 Ir1 P1 163.67(5) . 2_655 ? C3 P1 C11 104.65(19) . . ? C3 P1 C8 104.19(18) . . ? C11 P1 C8 104.40(19) . . ? C3 P1 Ir1 101.30(13) . . ? C11 P1 Ir1 125.13(14) . . ? C8 P1 Ir1 114.79(14) . . ? Ir1 O1 Ir1 180.0 . 11_666 ? C2 C1 C2 118.2(5) 2_655 . ? C2 C1 Ir1 120.9(2) 2_655 . ? C2 C1 Ir1 120.9(2) . . ? C3 C2 C7 117.6(4) . . ? C3 C2 C1 117.2(3) . . ? C7 C2 C1 125.0(4) . . ? C4 C3 C2 121.1(4) . . ? C4 C3 P1 126.8(3) . . ? C2 C3 P1 112.0(3) . . ? C5 C4 C3 120.4(4) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C6 C5 C4 119.2(4) . . ? C6 C5 H5 120.4 . . ? C4 C5 H5 120.4 . . ? C5 C6 C7 120.8(4) . . ? C5 C6 H6 119.6 . . ? C7 C6 H6 119.6 . . ? C6 C7 C2 120.9(4) . . ? C6 C7 H7 119.5 . . ? C2 C7 H7 119.5 . . ? C10 C8 C9 110.9(4) . . ? C10 C8 P1 114.8(3) . . ? C9 C8 P1 109.2(3) . . ? C10 C8 H8 107.2 . . ? C9 C8 H8 107.2 . . ? P1 C8 H8 107.2 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C13 111.6(4) . . ? C12 C11 P1 110.2(3) . . ? C13 C11 P1 110.1(3) . . ? C12 C11 H11 108.3 . . ? C13 C11 H11 108.3 . . ? P1 C11 H11 108.3 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Ir1 P1 C3 -19.52(13) . . . . ? O1 Ir1 P1 C3 160.48(13) . . . . ? P1 Ir1 P1 C3 -19.52(13) 2_655 . . . ? C1 Ir1 P1 C11 -136.65(17) . . . . ? O1 Ir1 P1 C11 43.35(17) . . . . ? P1 Ir1 P1 C11 -136.65(17) 2_655 . . . ? C1 Ir1 P1 C8 92.05(15) . . . . ? O1 Ir1 P1 C8 -87.95(15) . . . . ? P1 Ir1 P1 C8 92.05(15) 2_655 . . . ? P1 Ir1 C1 C2 -154.58(18) . . . 2_655 ? P1 Ir1 C1 C2 25.42(18) 2_655 . . 2_655 ? P1 Ir1 C1 C2 25.42(18) . . . . ? P1 Ir1 C1 C2 -154.58(18) 2_655 . . . ? C2 C1 C2 C3 157.0(4) 2_655 . . . ? Ir1 C1 C2 C3 -23.0(4) . . . . ? C2 C1 C2 C7 -27.7(3) 2_655 . . . ? Ir1 C1 C2 C7 152.3(3) . . . . ? C7 C2 C3 C4 2.2(6) . . . . ? C1 C2 C3 C4 177.7(3) . . . . ? C7 C2 C3 P1 -173.8(3) . . . . ? C1 C2 C3 P1 1.8(4) . . . . ? C11 P1 C3 C4 -30.1(4) . . . . ? C8 P1 C3 C4 79.2(4) . . . . ? Ir1 P1 C3 C4 -161.3(3) . . . . ? C11 P1 C3 C2 145.6(3) . . . . ? C8 P1 C3 C2 -105.1(3) . . . . ? Ir1 P1 C3 C2 14.4(3) . . . . ? C2 C3 C4 C5 -1.5(6) . . . . ? P1 C3 C4 C5 173.9(4) . . . . ? C3 C4 C5 C6 -0.1(7) . . . . ? C4 C5 C6 C7 1.1(7) . . . . ? C5 C6 C7 C2 -0.4(7) . . . . ? C3 C2 C7 C6 -1.2(6) . . . . ? C1 C2 C7 C6 -176.5(4) . . . . ? C3 P1 C8 C10 -67.2(3) . . . . ? C11 P1 C8 C10 42.3(4) . . . . ? Ir1 P1 C8 C10 -177.1(3) . . . . ? C3 P1 C8 C9 58.1(3) . . . . ? C11 P1 C8 C9 167.6(3) . . . . ? Ir1 P1 C8 C9 -51.8(3) . . . . ? C3 P1 C11 C12 -62.5(3) . . . . ? C8 P1 C11 C12 -171.7(3) . . . . ? Ir1 P1 C11 C12 53.0(4) . . . . ? C3 P1 C11 C13 174.0(3) . . . . ? C8 P1 C11 C13 64.8(3) . . . . ? Ir1 P1 C11 C13 -70.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.548 _refine_diff_density_min -0.669 _refine_diff_density_rms 0.104