# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 1475 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Sardar, Kripa' 'Fisher, Janet' 'Thompsett, David' 'Lees, Martin' 'Clarkson, Guy' 'Sloan, Jeremy' 'Jalilikashtiban, Reza' 'Walton, Richard' _publ_contact_author_name 'Dr Richard Walton' _publ_contact_author_email r.i.walton@warwick.ac.uk _publ_section_title ; Structural Variety in Iridate Oxides and Hydroxides From Hydrothermal Synthesis ; # Attachment '- Ca-Ir-hydroxide.cif' data_ks2 _database_code_depnum_ccdc_archive 'CCDC 819218' #TrackingRef '- Ca-Ir-hydroxide.cif' _audit_creation_method SHELXL-97 _audit_creation_date 2011-02-25 _audit_update_record 2011-02-25 _chemical_formula_sum 'Ca2 F H7 Ir O7' _chemical_formula_weight 410.420 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2-y,x,1/2+z 3 1/2-x,1/2-y,z 4 y,1/2-x,1/2+z 5 1/2+x,-y,1/2-z 6 -x,1/2+y,1/2-z 7 1/2+y,1/2+x,-z 8 -y,-x,-z 9 -x,-y,-z 10 1/2+y,-x,1/2-z 11 1/2+x,1/2+y,-z 12 -y,1/2+x,1/2-z 13 1/2-x,y,1/2+z 14 x,1/2-y,1/2+z 15 1/2-y,1/2-x,z 16 y,x,z _cell_length_a 10.6331(4) _cell_length_b 10.6331(4) _cell_length_c 5.6597(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 639.90(5) _cell_formula_units_Z 4 _cell_measurement_temperature 566(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 3.67 _cell_measurement_theta_max 29.00 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.281 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 756 _exptl_absorpt_coefficient_mu 22.492 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'ABSPACK(CrysAlis, Oxford Diffraction)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 566(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 'Oxford Diffraction Gemini R' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 2757 _diffrn_reflns_av_R_equivalents 0.0303 _diffrn_reflns_av_sigmaI/netI 0.0231 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 2.71 _diffrn_reflns_theta_max 29.12 _reflns_number_total 429 _reflns_number_gt 275 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _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^)+(0.0283P)^2^+0.0000P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 429 _refine_ls_number_parameters 29 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0379 _refine_ls_R_factor_gt 0.0188 _refine_ls_wR_factor_ref 0.0478 _refine_ls_wR_factor_gt 0.0443 _refine_ls_goodness_of_fit_ref 0.910 _refine_ls_restrained_S_all 0.910 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_radius_bond Ir ? 1.200 Ca ? 1.200 F ? 1.200 O ? 0.660 H ? 1.200 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_Wyckoff_symbol _atom_site_attached_hydrogens _atom_site_calc_flag _atom_site_thermal_displace_type _atom_site_u_iso_or_equiv Ir1 Ir 0.5000 1.0000 0.5000 1.000 4 d ? d Uani 0.00495(12) Ca1 Ca 0.3708(1) 0.8708(1) 0.0000 1.000 8 g ? d Uani 0.0081(2) F1 F 0.2500 0.7500 0.2500 1.000 4 b ? d Uani 0.009(1) O1 O 0.4874(3) 0.8256(3) 0.3681(5) 1.000 16 j ? d Uani 0.0092(7) H1 H 0.5594(19) 0.800(4) 0.328(7) 1.000 16 j ? d Uiso 0.01400 O2 O 0.5634(3) 0.9366(3) 0.8101(6) 1.000 8 i ? d Uani 0.0081(9) H2 H 0.6199(7) 0.8801(7) 0.801(10) 1.000 8 i ? d Uiso 0.01200 O3 O 0.7500 0.7500 0.2754(9) 1.000 4 e ? d Uani 0.0185(15) H3 H 0.7500 0.7500 0.125(4) 1.000 4 e ? d Uiso 0.02800 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ir1 0.00550(14) 0.00550(14) 0.00385(16) -0.00073(12) 0.00012(12) -0.00012(12) Ca1 0.0093(4) 0.0093(4) 0.0056(4) -0.0025(6) -0.0004(4) 0.0004(4) F1 0.0092(14) 0.0092(14) 0.0085(19) 0.00000 0.00000 0.00000 O1 0.0115(18) 0.0073(17) 0.0087(14) 0.0027(14) 0.0022(13) -0.0006(14) O2 0.0087(14) 0.0087(14) 0.0070(18) 0.002(2) -0.0013(14) 0.0013(14) O3 0.023(2) 0.023(2) 0.010(3) -0.002(4) 0.00000 0.00000 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ir1 O2 . 9_676 1.998(4) no Ir1 O2 . . 1.998(4) no Ir1 O1 . 9_676 2.003(3) no Ir1 O1 . . 2.003(3) no Ir1 O1 . 15_665 2.003(3) no Ir1 O1 . 7_456 2.003(3) no Ir1 Ca1 . 9_676 3.4323(7) no Ir1 Ca1 . . 3.4323(7) no Ir1 Ca1 . 9_675 3.4323(7) no Ir1 Ca1 . 1_556 3.4323(7) no Ca1 F1 . 13_554 2.3030(9) no Ca1 F1 . . 2.3030(9) no Ca1 O2 . 9_676 2.416(2) no Ca1 O2 . 1_554 2.416(2) no Ca1 O1 . . 2.471(3) no Ca1 O1 . 7_455 2.471(3) no Ca1 O1 . 14_564 2.541(3) no Ca1 O1 . 12_655 2.541(3) no Ca1 Ir1 . 1_554 3.4323(7) no F1 Ca1 . 3_565 2.3030(9) no F1 Ca1 . 12_655 2.3030(9) no F1 Ca1 . 10_465 2.3030(9) no O1 Ca1 . 10_465 2.541(3) no O1 H1 . . 0.845(9) no O2 Ca1 . 9_676 2.416(2) no O2 Ca1 . 1_556 2.416(2) no O2 H2 . . 0.851(9) no O3 H3 . . 0.85(2) no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O2 Ir1 O2 9_676 . . 180.0() no O2 Ir1 O1 9_676 . 9_676 92.14(12) no O2 Ir1 O1 . . 9_676 87.86(12) no O2 Ir1 O1 9_676 . . 87.86(12) no O2 Ir1 O1 . . . 92.14(12) no O1 Ir1 O1 9_676 . . 180.00 no O2 Ir1 O1 9_676 . 15_665 87.86(12) no O2 Ir1 O1 . . 15_665 92.14(12) no O1 Ir1 O1 9_676 . 15_665 90.86(16) no O1 Ir1 O1 . . 15_665 89.14(16) no O2 Ir1 O1 9_676 . 7_456 92.14(12) no O2 Ir1 O1 . . 7_456 87.86(12) no O1 Ir1 O1 9_676 . 7_456 89.14(16) no O1 Ir1 O1 . . 7_456 90.86(16) no O1 Ir1 O1 15_665 . 7_456 180.00 no O2 Ir1 Ca1 9_676 . 9_676 136.42(7) no O2 Ir1 Ca1 . . 9_676 43.58(7) no O1 Ir1 Ca1 9_676 . 9_676 45.23(9) no O1 Ir1 Ca1 . . 9_676 134.77(9) no O1 Ir1 Ca1 15_665 . 9_676 84.84(8) no O1 Ir1 Ca1 7_456 . 9_676 95.16(8) no O2 Ir1 Ca1 9_676 . . 43.58(7) no O2 Ir1 Ca1 . . . 136.42(7) no O1 Ir1 Ca1 9_676 . . 134.77(9) no O1 Ir1 Ca1 . . . 45.23(9) no O1 Ir1 Ca1 15_665 . . 95.16(8) no O1 Ir1 Ca1 7_456 . . 84.84(8) no Ca1 Ir1 Ca1 9_676 . . 180.00 no O2 Ir1 Ca1 9_676 . 9_675 43.58(7) no O2 Ir1 Ca1 . . 9_675 136.42(7) no O1 Ir1 Ca1 9_676 . 9_675 84.84(8) no O1 Ir1 Ca1 . . 9_675 95.16(8) no O1 Ir1 Ca1 15_665 . 9_675 45.23(9) no O1 Ir1 Ca1 7_456 . 9_675 134.77(9) no Ca1 Ir1 Ca1 9_676 . 9_675 111.07(3) no Ca1 Ir1 Ca1 . . 9_675 68.93(3) no O2 Ir1 Ca1 9_676 . 1_556 136.42(7) no O2 Ir1 Ca1 . . 1_556 43.58(7) no O1 Ir1 Ca1 9_676 . 1_556 95.16(8) no O1 Ir1 Ca1 . . 1_556 84.84(8) no O1 Ir1 Ca1 15_665 . 1_556 134.77(9) no O1 Ir1 Ca1 7_456 . 1_556 45.23(9) no Ca1 Ir1 Ca1 9_676 . 1_556 68.93(3) no Ca1 Ir1 Ca1 . . 1_556 111.07(3) no Ca1 Ir1 Ca1 9_675 . 1_556 180.00(3) no F1 Ca1 F1 13_554 . . 75.81(4) no F1 Ca1 O2 13_554 . 9_676 155.17(9) no F1 Ca1 O2 . . 9_676 111.16(7) no F1 Ca1 O2 13_554 . 1_554 111.16(7) no F1 Ca1 O2 . . 1_554 155.17(9) no O2 Ca1 O2 9_676 . 1_554 73.00(15) no F1 Ca1 O1 13_554 . . 133.56(8) no F1 Ca1 O1 . . . 69.71(7) no O2 Ca1 O1 9_676 . . 69.20(12) no O2 Ca1 O1 1_554 . . 90.36(11) no F1 Ca1 O1 13_554 . 7_455 69.71(7) no F1 Ca1 O1 . . 7_455 133.56(8) no O2 Ca1 O1 9_676 . 7_455 90.36(11) no O2 Ca1 O1 1_554 . 7_455 69.20(12) no O1 Ca1 O1 . . 7_455 154.94(16) no F1 Ca1 O1 13_554 . 14_564 68.47(7) no F1 Ca1 O1 . . 14_564 89.65(7) no O2 Ca1 O1 9_676 . 14_564 133.35(11) no O2 Ca1 O1 1_554 . 14_564 72.16(11) no O1 Ca1 O1 . . 14_564 80.97(8) no O1 Ca1 O1 7_455 . 14_564 105.04(6) no F1 Ca1 O1 13_554 . 12_655 89.65(7) no F1 Ca1 O1 . . 12_655 68.47(7) no O2 Ca1 O1 9_676 . 12_655 72.16(11) no O2 Ca1 O1 1_554 . 12_655 133.35(11) no O1 Ca1 O1 . . 12_655 105.04(6) no O1 Ca1 O1 7_455 . 12_655 80.97(8) no O1 Ca1 O1 14_564 . 12_655 152.65(14) no F1 Ca1 Ir1 13_554 . . 162.37(3) no F1 Ca1 Ir1 . . . 86.56(0) no O2 Ca1 Ir1 9_676 . . 34.75(8) no O2 Ca1 Ir1 1_554 . . 84.94(8) no O1 Ca1 Ir1 . . . 35.13(8) no O1 Ca1 Ir1 7_455 . . 124.91(8) no O1 Ca1 Ir1 14_564 . . 112.08(7) no O1 Ca1 Ir1 12_655 . . 83.78(7) no F1 Ca1 Ir1 13_554 . 1_554 86.56(0) no F1 Ca1 Ir1 . . 1_554 162.37(3) no O2 Ca1 Ir1 9_676 . 1_554 84.94(8) no O2 Ca1 Ir1 1_554 . 1_554 34.75(9) no O1 Ca1 Ir1 . . 1_554 124.91(8) no O1 Ca1 Ir1 7_455 . 1_554 35.13(8) no O1 Ca1 Ir1 14_564 . 1_554 83.78(7) no O1 Ca1 Ir1 12_655 . 1_554 112.08(7) no Ir1 Ca1 Ir1 . . 1_554 111.07(3) no F1 Ca1 Ca1 13_554 . 3_565 37.91(2) no F1 Ca1 Ca1 . . 3_565 37.91(2) no O2 Ca1 Ca1 9_676 . 3_565 143.50(7) no O2 Ca1 Ca1 1_554 . 3_565 143.50(7) no O1 Ca1 Ca1 . . 3_565 102.53(8) no O1 Ca1 Ca1 7_455 . 3_565 102.53(8) no O1 Ca1 Ca1 14_564 . 3_565 76.33(7) no O1 Ca1 Ca1 12_655 . 3_565 76.33(7) no Ir1 Ca1 Ca1 . . 3_565 124.46(2) no Ir1 Ca1 Ca1 1_554 . 3_565 124.46(2) no F1 Ca1 Ca1 13_554 . 10_464 33.91(1) no F1 Ca1 Ca1 . . 10_464 94.57(3) no O2 Ca1 Ca1 9_676 . 10_464 154.05(8) no O2 Ca1 Ca1 1_554 . 10_464 82.25(7) no O1 Ca1 Ca1 . . 10_464 119.55(8) no O1 Ca1 Ca1 7_455 . 10_464 73.32(6) no O1 Ca1 Ca1 14_564 . 10_464 39.64(7) no O1 Ca1 Ca1 12_655 . 10_464 123.05(7) no Ir1 Ca1 Ca1 . . 10_464 151.57(1) no Ir1 Ca1 Ca1 1_554 . 10_464 70.04(0) no Ca1 Ca1 Ca1 3_565 . 10_464 61.62(1) no Ca1 F1 Ca1 3_565 . . 104.19(4) no Ca1 F1 Ca1 3_565 . 12_655 112.18(2) no Ca1 F1 Ca1 . . 12_655 112.18(2) no Ca1 F1 Ca1 3_565 . 10_465 112.18(2) no Ca1 F1 Ca1 . . 10_465 112.18(2) no Ca1 F1 Ca1 12_655 . 10_465 104.19(4) no Ir1 O1 Ca1 . . . 99.64(13) no Ir1 O1 Ca1 . . 10_465 133.16(13) no Ca1 O1 Ca1 . . 10_465 99.38(11) no Ir1 O1 H1 . . . 110.(3) no Ca1 O1 H1 . . . 107.(3) no Ca1 O1 H1 10_465 . . 105.(3) no Ir1 O2 Ca1 . . 9_676 101.67(12) no Ir1 O2 Ca1 . . 1_556 101.67(12) no Ca1 O2 Ca1 9_676 . 1_556 107.00(15) no Ir1 O2 H2 . . . 115.(4) no Ca1 O2 H2 9_676 . . 115.0(18) no Ca1 O2 H2 1_556 . . 115.0(18) no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O1 H1 O3 . . . 0.845(9) 2.115(11) 2.953(3) 171.(4) no O2 H2 O3 . . 2_655 0.851(9) 1.961(10) 2.812(4) 179.(5) no O3 H3 O3 . . 2_654 0.85(2) 1.98(2) 2.830(8) 180.0(3) no _diffrn_measured_fraction_theta_max 0.921 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.750 _refine_diff_density_min -1.314 _refine_diff_density_rms 0.212 # Attachment '- Sr-Ir-hydroxide.cif' data_ks1 _database_code_depnum_ccdc_archive 'CCDC 819219' #TrackingRef '- Sr-Ir-hydroxide.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H8 Ir O8 Sr2' _chemical_formula_weight 503.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' Sr Sr -1.5307 3.2498 '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 monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 5.9657(3) _cell_length_b 10.9919(4) _cell_length_c 6.0097(3) _cell_angle_alpha 90.00 _cell_angle_beta 112.903(6) _cell_angle_gamma 90.00 _cell_volume 363.01(3) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1379 _cell_measurement_theta_min 3.67 _cell_measurement_theta_max 29.00 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.606 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 450 _exptl_absorpt_coefficient_mu 32.927 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.21 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'ABSPACK(CrysAlis, Oxford Diffraction)' _exptl_special_details ; A crystal was glued to a glass fibre and the data recorded at 296K. The data collection nominally covered over a hemisphere of Reciprocal space, by a combination of four sets of exposures with different \f angles for the crystal; each 10 s exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.5 cm. Crystal decay was found to be negligible by by repeating the initial frames at the end of data collection and analyzing the duplicate reflections. Hydrogen atoms were located in a difference map and refined with a distance retraint. Anisotropic displacement parameters were used for all non-H atoms; H-atoms were given isotropic displacement parameter equal to 1.5 times the equivalent isotropic displacement parameter of the atom to which they are attached. ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 10.2833 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 1848 _diffrn_reflns_av_R_equivalents 0.0248 _diffrn_reflns_av_sigmaI/netI 0.0330 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 3.71 _diffrn_reflns_theta_max 29.07 _reflns_number_total 844 _reflns_number_gt 729 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _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^)+(0.0329P)^2^+0.0000P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0175(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 844 _refine_ls_number_parameters 65 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0290 _refine_ls_R_factor_gt 0.0234 _refine_ls_wR_factor_ref 0.0546 _refine_ls_wR_factor_gt 0.0533 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.001 _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 0.0000 0.0000 0.0000 0.00583(14) Uani 1 2 d S . . Sr1 Sr 0.27359(11) 0.37242(5) 0.10489(9) 0.00896(17) Uani 1 1 d . . . O1 O 0.0195(9) 0.1686(4) -0.1256(7) 0.0098(9) Uani 1 1 d D . . H1 H -0.120(6) 0.199(6) -0.176(12) 0.015 Uiso 1 1 d D . . O2 O -0.1163(9) 0.0620(3) 0.2495(7) 0.0094(9) Uani 1 1 d D . . H2 H -0.225(11) 0.112(6) 0.173(11) 0.014 Uiso 1 1 d D . . O3 O 0.3458(9) 0.0250(4) 0.2378(8) 0.0107(9) Uani 1 1 d D . . H3 H 0.422(13) 0.073(5) 0.183(13) 0.016 Uiso 1 1 d D . . O4 O 0.5540(9) 0.2289(4) 0.0196(7) 0.0149(10) Uani 1 1 d D . . H4 H 0.633(13) 0.265(6) -0.052(12) 0.022 Uiso 1 1 d D . . 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 0.0033(2) 0.00728(19) 0.0071(2) -0.00006(11) 0.00221(14) -0.00053(12) Sr1 0.0070(3) 0.0106(3) 0.0103(3) 0.0009(2) 0.0044(2) 0.0016(2) O1 0.003(2) 0.0095(19) 0.015(2) 0.0010(16) 0.002(2) 0.0017(16) O2 0.007(3) 0.011(2) 0.010(2) -0.0005(16) 0.0025(18) 0.0013(17) O3 0.006(3) 0.0129(19) 0.013(2) -0.0015(17) 0.0037(19) -0.0023(17) O4 0.011(3) 0.019(2) 0.015(2) 0.0004(17) 0.005(2) 0.0038(19) _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 O2 2.001(4) 3 ? Ir1 O2 2.001(4) . ? Ir1 O3 2.020(5) 3 ? Ir1 O3 2.020(5) . ? Ir1 O1 2.021(4) . ? Ir1 O1 2.021(4) 3 ? Ir1 Sr1 3.6369(6) 2_544 ? Ir1 Sr1 3.6369(6) 4_566 ? Ir1 Sr1 3.6449(5) 4_565 ? Ir1 Sr1 3.6449(5) 2_545 ? Sr1 O4 2.493(5) . ? Sr1 O2 2.574(5) 4_565 ? Sr1 O2 2.575(4) 2 ? Sr1 O4 2.647(4) 4_566 ? Sr1 O1 2.652(4) 4_566 ? Sr1 O3 2.658(4) 4_565 ? Sr1 O3 2.681(5) 2_655 ? Sr1 O1 2.757(4) . ? Sr1 Ir1 3.6369(6) 2_554 ? Sr1 Ir1 3.6449(5) 2 ? Sr1 Sr1 4.0339(7) 4_565 ? Sr1 Sr1 4.0339(7) 4_566 ? Sr1 H4 2.91(6) . ? O1 Sr1 2.652(4) 4_565 ? O1 H1 0.84(2) . ? O2 Sr1 2.574(5) 4_566 ? O2 Sr1 2.575(4) 2_545 ? O2 H2 0.84(2) . ? O3 Sr1 2.658(4) 4_566 ? O3 Sr1 2.681(5) 2_645 ? O3 H3 0.84(2) . ? O4 Sr1 2.647(4) 4_565 ? O4 H4 0.85(2) . ? 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 O2 Ir1 O2 180.0(2) 3 . ? O2 Ir1 O3 88.85(19) 3 3 ? O2 Ir1 O3 91.15(19) . 3 ? O2 Ir1 O3 91.15(19) 3 . ? O2 Ir1 O3 88.85(19) . . ? O3 Ir1 O3 180.0(2) 3 . ? O2 Ir1 O1 86.86(17) 3 . ? O2 Ir1 O1 93.14(17) . . ? O3 Ir1 O1 92.98(18) 3 . ? O3 Ir1 O1 87.02(18) . . ? O2 Ir1 O1 93.14(17) 3 3 ? O2 Ir1 O1 86.86(17) . 3 ? O3 Ir1 O1 87.02(18) 3 3 ? O3 Ir1 O1 92.98(18) . 3 ? O1 Ir1 O1 180.00(9) . 3 ? O2 Ir1 Sr1 43.21(14) 3 2_544 ? O2 Ir1 Sr1 136.79(14) . 2_544 ? O3 Ir1 Sr1 45.80(13) 3 2_544 ? O3 Ir1 Sr1 134.20(13) . 2_544 ? O1 Ir1 Sr1 92.80(12) . 2_544 ? O1 Ir1 Sr1 87.20(12) 3 2_544 ? O2 Ir1 Sr1 136.79(14) 3 4_566 ? O2 Ir1 Sr1 43.21(14) . 4_566 ? O3 Ir1 Sr1 134.20(13) 3 4_566 ? O3 Ir1 Sr1 45.80(13) . 4_566 ? O1 Ir1 Sr1 87.20(12) . 4_566 ? O1 Ir1 Sr1 92.80(12) 3 4_566 ? Sr1 Ir1 Sr1 180.000(18) 2_544 4_566 ? O2 Ir1 Sr1 43.05(11) 3 4_565 ? O2 Ir1 Sr1 136.95(11) . 4_565 ? O3 Ir1 Sr1 100.63(12) 3 4_565 ? O3 Ir1 Sr1 79.37(12) . 4_565 ? O1 Ir1 Sr1 45.45(12) . 4_565 ? O1 Ir1 Sr1 134.55(12) 3 4_565 ? Sr1 Ir1 Sr1 68.761(15) 2_544 4_565 ? Sr1 Ir1 Sr1 111.239(15) 4_566 4_565 ? O2 Ir1 Sr1 136.95(11) 3 2_545 ? O2 Ir1 Sr1 43.05(11) . 2_545 ? O3 Ir1 Sr1 79.37(12) 3 2_545 ? O3 Ir1 Sr1 100.63(12) . 2_545 ? O1 Ir1 Sr1 134.55(12) . 2_545 ? O1 Ir1 Sr1 45.45(12) 3 2_545 ? Sr1 Ir1 Sr1 111.239(15) 2_544 2_545 ? Sr1 Ir1 Sr1 68.761(15) 4_566 2_545 ? Sr1 Ir1 Sr1 180.000(18) 4_565 2_545 ? O4 Sr1 O2 117.94(14) . 4_565 ? O4 Sr1 O2 160.81(16) . 2 ? O2 Sr1 O2 73.99(15) 4_565 2 ? O4 Sr1 O4 72.46(11) . 4_566 ? O2 Sr1 O4 159.24(14) 4_565 4_566 ? O2 Sr1 O4 101.60(14) 2 4_566 ? O4 Sr1 O1 127.34(14) . 4_566 ? O2 Sr1 O1 90.44(14) 4_565 4_566 ? O2 Sr1 O1 63.86(13) 2 4_566 ? O4 Sr1 O1 69.84(14) 4_566 4_566 ? O4 Sr1 O3 76.08(14) . 4_565 ? O2 Sr1 O3 65.07(14) 4_565 4_565 ? O2 Sr1 O3 97.87(13) 2 4_565 ? O4 Sr1 O3 135.47(15) 4_566 4_565 ? O1 Sr1 O3 153.48(14) 4_566 4_565 ? O4 Sr1 O3 85.66(15) . 2_655 ? O2 Sr1 O3 119.03(13) 4_565 2_655 ? O2 Sr1 O3 75.20(14) 2 2_655 ? O4 Sr1 O3 78.06(14) 4_566 2_655 ? O1 Sr1 O3 119.85(13) 4_566 2_655 ? O3 Sr1 O3 68.82(16) 4_565 2_655 ? O4 Sr1 O1 70.37(15) . . ? O2 Sr1 O1 70.62(13) 4_565 . ? O2 Sr1 O1 128.81(14) 2 . ? O4 Sr1 O1 98.83(14) 4_566 . ? O1 Sr1 O1 80.55(12) 4_566 . ? O3 Sr1 O1 99.37(13) 4_565 . ? O3 Sr1 O1 155.48(14) 2_655 . ? O4 Sr1 Ir1 96.58(9) . 2_554 ? O2 Sr1 Ir1 32.17(10) 4_565 2_554 ? O2 Sr1 Ir1 86.93(9) 2 2_554 ? O4 Sr1 Ir1 167.63(10) 4_566 2_554 ? O1 Sr1 Ir1 122.35(10) 4_566 2_554 ? O3 Sr1 Ir1 33.01(10) 4_565 2_554 ? O3 Sr1 Ir1 95.75(10) 2_655 2_554 ? O1 Sr1 Ir1 82.30(9) . 2_554 ? O4 Sr1 Ir1 152.08(9) . 2 ? O2 Sr1 Ir1 86.77(9) 4_565 2 ? O2 Sr1 Ir1 32.04(9) 2 2 ? O4 Sr1 Ir1 80.07(10) 4_566 2 ? O1 Sr1 Ir1 32.89(9) 4_566 2 ? O3 Sr1 Ir1 129.49(10) 4_565 2 ? O3 Sr1 Ir1 93.56(9) 2_655 2 ? O1 Sr1 Ir1 110.00(9) . 2 ? Ir1 Sr1 Ir1 111.239(15) 2_554 2 ? O4 Sr1 Sr1 39.67(11) . 4_565 ? O2 Sr1 Sr1 80.25(9) 4_565 4_565 ? O2 Sr1 Sr1 154.01(10) 2 4_565 ? O4 Sr1 Sr1 103.74(10) 4_566 4_565 ? O1 Sr1 Sr1 120.48(9) 4_566 4_565 ? O3 Sr1 Sr1 67.53(9) 4_565 4_565 ? O3 Sr1 Sr1 115.75(9) 2_655 4_565 ? O1 Sr1 Sr1 40.79(9) . 4_565 ? Ir1 Sr1 Sr1 69.071(6) 2_554 4_565 ? Ir1 Sr1 Sr1 150.665(14) 2 4_565 ? O4 Sr1 Sr1 85.72(10) . 4_566 ? O2 Sr1 Sr1 122.88(9) 4_565 4_566 ? O2 Sr1 Sr1 100.44(9) 2 4_566 ? O4 Sr1 Sr1 36.97(11) 4_566 4_566 ? O1 Sr1 Sr1 42.79(9) 4_566 4_566 ? O3 Sr1 Sr1 161.50(10) 4_565 4_566 ? O3 Sr1 Sr1 113.59(10) 2_655 4_566 ? O1 Sr1 Sr1 70.89(9) . 4_566 ? Ir1 Sr1 Sr1 150.657(14) 2_554 4_566 ? Ir1 Sr1 Sr1 68.998(6) 2 4_566 ? Sr1 Sr1 Sr1 96.30(2) 4_565 4_566 ? O4 Sr1 H4 15.8(10) . . ? O2 Sr1 H4 112.8(15) 4_565 . ? O2 Sr1 H4 148.3(11) 2 . ? O4 Sr1 H4 81.9(14) 4_566 . ? O1 Sr1 H4 142.9(10) 4_566 . ? O3 Sr1 H4 61.7(11) 4_565 . ? O3 Sr1 H4 74.8(13) 2_655 . ? O1 Sr1 H4 80.7(12) . . ? Ir1 Sr1 H4 86.2(13) 2_554 . ? Ir1 Sr1 H4 160.2(15) 2 . ? Sr1 Sr1 H4 43.5(14) 4_565 . ? Sr1 Sr1 H4 100.6(11) 4_566 . ? Ir1 O1 Sr1 101.66(16) . 4_565 ? Ir1 O1 Sr1 131.12(19) . . ? Sr1 O1 Sr1 96.42(15) 4_565 . ? Ir1 O1 H1 108(5) . . ? Sr1 O1 H1 125(5) 4_565 . ? Sr1 O1 H1 97(5) . . ? Ir1 O2 Sr1 104.62(19) . 4_566 ? Ir1 O2 Sr1 104.91(16) . 2_545 ? Sr1 O2 Sr1 106.01(15) 4_566 2_545 ? Ir1 O2 H2 103(5) . . ? Sr1 O2 H2 122(5) 4_566 . ? Sr1 O2 H2 114(5) 2_545 . ? Ir1 O3 Sr1 101.19(18) . 4_566 ? Ir1 O3 Sr1 131.0(2) . 2_645 ? Sr1 O3 Sr1 111.18(16) 4_566 2_645 ? Ir1 O3 H3 111(6) . . ? Sr1 O3 H3 110(5) 4_566 . ? Sr1 O3 H3 91(5) 2_645 . ? Sr1 O4 Sr1 103.36(18) . 4_565 ? Sr1 O4 H4 111(5) . . ? Sr1 O4 H4 90(5) 4_565 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3 O4 0.84(2) 2.26(3) 3.091(6) 167(7) . O1 H1 O4 0.84(2) 2.23(4) 2.987(7) 150(6) 4_465 O4 H4 O4 0.85(2) 2.43(6) 3.0404(15) 129(6) 4_565 O1 H1 O4 0.84(2) 2.66(5) 3.287(6) 133(6) 1_455 O2 H2 O4 0.84(2) 1.81(2) 2.651(6) 176(8) 1_455 O3 H3 O2 0.84(2) 2.63(7) 3.208(7) 127(7) 1_655 _diffrn_measured_fraction_theta_max 0.870 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.658 _refine_diff_density_min -1.804 _refine_diff_density_rms 0.323