# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_coden_ASTM ? _journal_coeditor_code ? _journal_coeditor_name ? _journal_coeditor_notes ; ? ; _journal_date_accepted ? _journal_date_from_coeditor ? _journal_date_printers_final ? _journal_date_printers_first ? _journal_date_proofs_in ? _journal_date_proofs_out ? #============================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_volume ? _journal_year ? loop_ _publ_author_name _publ_author_address A.Hill ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; R.D.Dewhurst ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; A.C.Willis ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; _publ_contact_author_address ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 0200, Australia ; _publ_contact_author_email willis@rsc.anu.edu.au _publ_contact_author_fax ' 61 2 6125 0750 ' _publ_contact_author_phone ' 61 2 6125 4109 ' #_publ_requested_category 'FM ' _publ_contact_author_name 'Anthony C. Willis' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? #============================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; Crystal structure of [{(C~9~H~10~BN~6~)W(CO)~2~C~3~}~2~Ir(HgCl)(CO){P(C~6~H~5~)~3~}~2~].2CH~2~Cl~2~ #-- rian19 ; data_rian19 _database_code_depnum_ccdc_archive 'CCDC 689223' _audit_creation_date 05-24-06 _audit_creation_method CRYSTALS_ver_12-03-99 # 5191230 rian19 _audit_update_record ; 2005-06-24 - Report on C67 H54 B2 Cl5 Hg Ir N12 O5 P2 W2 by Anthony C. Willis for Anthony F. Hill and Rian Dewhurst 2005-06-24- passes checkcif tests with minor warnings 2009-01-29 - modify cif for referee ; #============================================================================== # 4. TEXT _publ_section_abstract #Text of the abstract ; The crystal structure of [{(C~9~H~10~BN~6~)W(CO)~2~C~3~}~2~Ir(HgCl)(CO){P(C~6~H~5~)~3~}~2~].2CH~2~Cl~2~ is reported. ; _publ_section_comment #Text of the paper ; The unit cell contains one [{(C~9~H~10~BN~6~)W(CO)~2~C~3~}~2~Ir(HgCl)(CO){P(C~6~H~5~)~3~}~2~] molecule plus dichloromethane solvate molecules. The organometallic species is centred on a crystallographic inversion symmetry operation. The HgCl and CO groups on the Ir each have only one-half occupancy and are disordered with respect to each other. The Ir atom was initially at 1/2,1/2,1/2, but its anisotropic displacement ellipsoid was elongated in the direction of the Hg atom and the Hg---Ir distance was shorter than would have been expected. Ihe Ir atom was therefore displaced from the inversion centre in the direction away from the Hg atom. Initially a restraint was placed on the Ir---Hg distance, but later it was removed. Restraints were placed on the Ir---C and C---O distances and on the displacement parameters of C4 and O4 as they are in close proximity to the inversion image of the Hg atom. The dichloromethane molecule is disordered over two orientations, with Cl2 common to both. Restraints were placed on bonding distances and angles and on displacement parameters in this molecule. The biggest peaks in the final difference electron density map have no chemical significance. ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions #Captions to figures ; ? ; _publ_section_exptl_refinement # see also _refine_ls_hydrogen for refinement keywords. ; H atoms were included at idealized positions and ride on the atom to which they are attached. ; _publ_section_exptl_prep ; The compound was prepared by RDD and recrystallized from dichloromethane/ethanol The sample ID was RD-4,58. ; _refine_special_details #Text of the paper ; The unit cell contains one [{(C~9~H~10~BN~6~)W(CO)~2~C~3~}~2~Ir(HgCl)(CO){P(C~6~H~5~)~3~}~2~] molecule plus dichloromethane solvate molecules. The organometallic species is centred on a crystallographic inversion symmetry operation. The HgCl and CO groups on the Ir each have only one-half occupancy and are disordered with respect to each other. The Ir atom was initially at 1/2,1/2,1/2, but its anisotropic displacement ellipsoid was elongated in the direction of the Hg atom and the Hg---Ir distance was shorter than would have been expected. Ihe Ir atom was therefore displaced from the inversion centre in the direction away from the Hg atom. Initially a restraint was placed on the Ir---Hg distance, but later it was removed. Restraints were placed on the Ir---C and C---O distances and on the displacement parameters of C4 and O4 as they are in close proximity to the inversion image of the Hg atom. The dichloromethane molecule is disordered over two orientations, with Cl2 common to both. Restraints were placed on bonding distances and angles and on displacement parameters in this molecule. H atoms were included at idealized positions and ride on the atom to which they are attached. ; #========================================================================== _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point ? # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment noref #**************************************************************************** # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al 2003) ; _computing_publication_material ; CRYSTALS (Watkin et al 2003) ; _computing_molecular_graphics ; ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997) ; #============================================================= _cell_length_a 12.0420(4) _cell_angle_alpha 65.9070(17) _cell_length_b 12.6900(4) _cell_angle_beta 86.9260(19) _cell_length_c 14.3350(3) _cell_angle_gamma 66.3350(16) _cell_volume 1815.59(10) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z # choose from: rm (reference molecule of # known chirality), ad (anomolous # dispersion - ie. Flack param), rmad # (both rm and ad), syn (known from # synthetic pathway), unk (unknown) # or . (not applicable). _chemical_absolute_configuration . loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 International_Tables_Vol_IV_Table_2.2B 'B ' 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 International_Tables_Vol_IV_Table_2.2B 'Cl ' 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 International_Tables_Vol_IV_Table_2.2B 'Hg ' -2.3894 9.2266 20.6809 0.5450 19.0417 8.4484 21.6575 1.5729 5.9676 38.3246 12.6089 International_Tables_Vol_IV_Table_2.2B 'Ir ' -1.4442 7.9887 27.3049 1.5928 16.7296 8.8655 15.6115 0.4179 5.8338 45.0011 11.4722 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B 'P ' 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 International_Tables_Vol_IV_Table_2.2B 'W ' -0.8490 6.8722 29.0818 1.7203 15.4300 9.2259 14.4327 0.3217 5.1198 57.0560 9.8875 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 1 _chemical_formula_sum ' C67 H54 B2 Cl5 Hg Ir N12 O5 P2 W2 ' _chemical_formula_moiety ' C65 H50 B2 Cl Hg Ir N12 O5 P2 W2 , 2(C H2 Cl2)' _chemical_compound_source ; ? ; _chemical_formula_weight 2128.59 _cell_measurement_reflns_used 25429 _cell_measurement_theta_min 3 _cell_measurement_theta_max 25 _cell_measurement_temperature 200 _exptl_crystal_description ' plate ' _exptl_crystal_colour ' orange ' _exptl_crystal_size_min 0.03 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_max 0.06 _exptl_crystal_density_diffrn 1.947 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1010 _exptl_absorpt_coefficient_mu 7.376 _diffrn_measurement_device_type ; Nonius Kappa CCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; COLLECT (Nonius BV, 1997) ; _computing_data_reduction ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_structure_solution ; SIR92 (Altomare et al, 1994) ; _diffrn_measurement_method ' \f and \w scans with CCD ' _diffrn_special_details ; CCD data collecting conditions- phi and omega scans of width 2.0 deg at rate 1160 sec/frame, crystal-detector distance 28mm, multiple scan sets so over 95 percent of data collected with 2-fold redundancy or more. ; # Absorption correction loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 0 0.005 -1 0 0 0.030 0 1 1 0.010 0 -1 -1 0.015 0 -1 1 0.030 0 1 -1 0.030 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.677 _exptl_absorpt_correction_T_max 0.855 _exptl_absorpt_process_details ; via Gaussian method (Coppens, 1970) implemented in maXus (2000) ; # Sheldrick geometric definitions 0.74 0.80 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 200 _diffrn_reflns_number 31953 _reflns_number_total 6386 _diffrn_reflns_av_R_equivalents 0.05 # Number of reflections with Friedels Law is 6386 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 6442 _diffrn_reflns_theta_min 2.590 _diffrn_reflns_theta_max 25.0 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25. _diffrn_measured_fraction_theta_full 0.99 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _reflns_limit_h_min -14 _reflns_limit_h_max 14 _reflns_limit_k_min -13 _reflns_limit_k_max 15 _reflns_limit_l_min 0 _reflns_limit_l_max 17 _refine_diff_density_min -2.10 _refine_diff_density_max 1.97 _refine_ls_number_reflns 4285 _refine_ls_number_restraints 64 _refine_ls_number_parameters 478 #_refine_ls_R_factor_ref 0.0454 _refine_ls_wR_factor_ref 0.0377 _refine_ls_goodness_of_fit_ref 1.0179 #_reflns_number_all 6362 _refine_ls_R_factor_all 0.0738 _refine_ls_wR_factor_all 0.0410 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 4285 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_gt 0.0377 _refine_ls_shift/su_max 0.000980 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.18 -0.420 0.957 -0.0709 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 ## -------------------REFERENCES ----------------------## ## Insert your own references - in alphabetic order _publ_section_references ; Mackay, S., Gilmore, C. J.,Edwards, C., Stewart, N. & Shankland, K. (2000). maXus Computer Program for the Solution and Refinement of Crystal Structures. Nonius, The Netherlands, MacScience, Japan & The University of Glasgow. Coppens, P. (1970). The Evaluation of Absorption and Extinction in Single-Crystal Structure Analysis. Crystallographic Computing. F. R. Ahmed, S. R. Hall and C. P. Huber, eds., Munksgaard. Copenhagen. pp 255-270. Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius BV, COLLECT Software, 1997-2001) Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994), Acta Cryst, A50, 411-437 Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.8. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Johnson, C.K. (1976) ORTEP-II, A Fortran Thermal-Ellipsoid Plot Program, Report ORNL-5138, Oak Ridge National Laboratory, Oak Ridge, Tennessee, USA. ; # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Hg1 Hg 0.69223(12) 0.35546(16) 0.47776(10) 0.0374 0.5000 Uani . U . . . . Ir1 Ir 0.4815(2) 0.5107(5) 0.5001(4) 0.0281 0.5000 Uani D . . . . . W1 W 0.26830(3) 0.79760(3) 0.02036(3) 0.0295 1.0000 Uani . . . . . . Cl1 Cl 0.8838(5) 0.2134(7) 0.4528(5) 0.0715 0.5000 Uani . . . . . . Cl2 Cl 1.1151(5) 0.3375(6) 0.0869(5) 0.1500 1.0000 Uani D U . . . . Cl31 Cl 0.9382(13) 0.2902(17) 0.2049(9) 0.0883 0.5000 Uani D U . S 1 . Cl32 Cl 0.9425(18) 0.273(2) 0.2531(15) 0.1467 0.5000 Uani D U . S 2 . P1 P 0.4269(2) 0.3381(2) 0.55298(16) 0.0351 1.0000 Uani . . . . . . O4 O 0.2312(12) 0.7007(14) 0.5178(14) 0.0833 0.5000 Uani D U . . . . O5 O 0.1835(6) 1.0287(7) 0.0792(6) 0.0522 1.0000 Uani . . . . . . O6 O 0.0468(7) 0.7376(8) 0.1076(6) 0.0629 1.0000 Uani . . . . . . N11 N 0.1702(7) 0.9236(7) -0.1450(5) 0.0342 1.0000 Uani . . . . . . N12 N 0.2272(7) 0.9080(8) -0.2259(5) 0.0420 1.0000 Uani . . . . . . N21 N 0.3269(6) 0.6560(7) -0.0436(6) 0.0368 1.0000 Uani . . . . . . N22 N 0.3628(7) 0.6761(7) -0.1389(6) 0.0396 1.0000 Uani . . . . . . N31 N 0.4193(6) 0.8376(7) -0.0576(5) 0.0337 1.0000 Uani . . . . . . N32 N 0.4415(7) 0.8355(7) -0.1518(6) 0.0402 1.0000 Uani . . . . . . C1 C 0.3425(8) 0.7007(8) 0.1527(7) 0.0328 1.0000 Uani . . . . . . C2 C 0.3888(9) 0.6320(8) 0.2593(7) 0.0333 1.0000 Uani . . . . . . C3 C 0.4303(8) 0.5763(8) 0.3491(6) 0.0343 1.0000 Uani . . . . . . C4 C 0.319(2) 0.630(4) 0.504(3) 0.0387 0.5000 Uani D U . . . . C5 C 0.2135(8) 0.9430(9) 0.0574(6) 0.0373 1.0000 Uani . . . . . . C6 C 0.1286(9) 0.7605(9) 0.0745(7) 0.0427 1.0000 Uani . . . . . . C13 C 0.1481(11) 0.9919(11) -0.3134(7) 0.0580 1.0000 Uani . . . . . . C14 C 0.0425(10) 1.0595(10) -0.2879(8) 0.0582 1.0000 Uani . . . . . . C15 C 0.0588(9) 1.0168(9) -0.1837(7) 0.0454 1.0000 Uani . . . . . . C23 C 0.3953(9) 0.5723(10) -0.1560(8) 0.0505 1.0000 Uani . . . . . . C24 C 0.3832(9) 0.4773(10) -0.0719(9) 0.0496 1.0000 Uani . . . . . . C25 C 0.3405(11) 0.5386(11) -0.0073(9) 0.0651 1.0000 Uani . . . . . . C33 C 0.5398(9) 0.8619(10) -0.1795(8) 0.0540 1.0000 Uani . . . . . . C34 C 0.5840(9) 0.8786(10) -0.1035(9) 0.0536 1.0000 Uani . . . . . . C35 C 0.5036(9) 0.8657(9) -0.0287(8) 0.0434 1.0000 Uani . . . . . . C111 C 0.3076(9) 0.3692(8) 0.4593(7) 0.0435 1.0000 Uani . . . . . . C112 C 0.3344(12) 0.3751(10) 0.3614(8) 0.0560 1.0000 Uani . . . . . . C113 C 0.2430(12) 0.4020(11) 0.2884(8) 0.0584 1.0000 Uani . . . . . . C114 C 0.1276(14) 0.4218(14) 0.3154(11) 0.0787 1.0000 Uani . . . . . . C115 C 0.0977(13) 0.4148(19) 0.4123(14) 0.1046 1.0000 Uani . . . . . . C116 C 0.1931(11) 0.3876(14) 0.4840(10) 0.0748 1.0000 Uani . . . . . . C121 C 0.3580(8) 0.3037(9) 0.6726(7) 0.0372 1.0000 Uani . . . . . . C122 C 0.3148(10) 0.3868(10) 0.7183(7) 0.0477 1.0000 Uani . . . . . . C123 C 0.2483(9) 0.3639(10) 0.8014(7) 0.0485 1.0000 Uani . . . . . . C124 C 0.2279(10) 0.2557(10) 0.8393(8) 0.0522 1.0000 Uani . . . . . . C125 C 0.2738(11) 0.1692(10) 0.7974(9) 0.0599 1.0000 Uani . . . . . . C126 C 0.3399(10) 0.1937(10) 0.7142(8) 0.0539 1.0000 Uani . . . . . . C131 C 0.5473(9) 0.1812(9) 0.5762(7) 0.0393 1.0000 Uani . . . . . . C132 C 0.6441(10) 0.1262(9) 0.6574(8) 0.0493 1.0000 Uani . . . . . . C133 C 0.7395(11) 0.0110(9) 0.6767(8) 0.0508 1.0000 Uani . . . . . . C134 C 0.7456(10) -0.0529(11) 0.6158(9) 0.0562 1.0000 Uani . . . . . . C135 C 0.6543(10) -0.0001(10) 0.5383(9) 0.0556 1.0000 Uani . . . . . . C136 C 0.5542(10) 0.1169(10) 0.5172(8) 0.0514 1.0000 Uani . . . . . . C201 C 0.984(3) 0.313(6) 0.082(2) 0.1279 0.5000 Uani D U . S 1 . C202 C 0.985(4) 0.298(6) 0.123(2) 0.1404 0.5000 Uani D U . S 2 . B1 B 0.3594(10) 0.8085(10) -0.2096(7) 0.0365 1.0000 Uani . . . . . . H1 H 0.3877 0.8113 -0.2772 0.0419 1.0000 Uiso R . . . . . H131 H 0.1652 1.0020 -0.3849 0.0603 1.0000 Uiso R . . . . . H141 H -0.0330 1.1276 -0.3361 0.0565 1.0000 Uiso R . . . . . H151 H -0.0035 1.0503 -0.1422 0.0496 1.0000 Uiso R . . . . . H231 H 0.4242 0.5653 -0.2208 0.0655 1.0000 Uiso R . . . . . H241 H 0.4001 0.3886 -0.0600 0.0591 1.0000 Uiso R . . . . . H251 H 0.3214 0.4948 0.0631 0.0743 1.0000 Uiso R . . . . . H331 H 0.5746 0.8682 -0.2455 0.0609 1.0000 Uiso R . . . . . H341 H 0.6574 0.8963 -0.1013 0.0679 1.0000 Uiso R . . . . . H351 H 0.5089 0.8759 0.0363 0.0540 1.0000 Uiso R . . . . . H1121 H 0.4193 0.3600 0.3437 0.0778 1.0000 Uiso R . . . . . H1131 H 0.2612 0.4068 0.2182 0.0714 1.0000 Uiso R . . . . . H1141 H 0.0619 0.4421 0.2629 0.0973 1.0000 Uiso R . . . . . H1151 H 0.0132 0.4283 0.4304 0.1356 1.0000 Uiso R . . . . . H1161 H 0.1754 0.3818 0.5544 0.0912 1.0000 Uiso R . . . . . H1221 H 0.3312 0.4646 0.6916 0.0629 1.0000 Uiso R . . . . . H1231 H 0.2157 0.4257 0.8331 0.0665 1.0000 Uiso R . . . . . H1241 H 0.1791 0.2397 0.8981 0.0634 1.0000 Uiso R . . . . . H1251 H 0.2601 0.0898 0.8262 0.0687 1.0000 Uiso R . . . . . H1261 H 0.3748 0.1303 0.6841 0.0654 1.0000 Uiso R . . . . . H1321 H 0.6425 0.1716 0.7007 0.0595 1.0000 Uiso R . . . . . H1331 H 0.8056 -0.0276 0.7352 0.0573 1.0000 Uiso R . . . . . H1341 H 0.8160 -0.1359 0.6292 0.0700 1.0000 Uiso R . . . . . H1351 H 0.6578 -0.0456 0.4946 0.0724 1.0000 Uiso R . . . . . H1361 H 0.4881 0.1531 0.4592 0.0638 1.0000 Uiso R . . . . . H2011 H 0.919 0.390 0.027 0.1441 0.5000 Uiso R . . S 1 . H2012 H 1.002 0.237 0.069 0.1441 0.5000 Uiso R . . S 1 . H2021 H 0.912 0.368 0.072 0.1612 0.5000 Uiso R . . S 2 . H2022 H 1.003 0.217 0.116 0.1612 0.5000 Uiso R . . S 2 . 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 Hg1 0.0427(5) 0.0401(6) 0.0278(6) -0.0099(4) 0.0039(4) -0.0203(4) Ir1 0.0301(16) 0.0342(14) 0.0217(3) -0.0063(7) 0.0017(13) -0.0204(14) W1 0.0329(2) 0.0321(2) 0.02497(18) -0.01136(15) 0.00502(13) -0.01575(16) Cl1 0.049(3) 0.083(4) 0.061(3) -0.030(3) 0.018(3) -0.009(3) Cl2 0.111(4) 0.155(5) 0.172(5) -0.100(4) -0.036(4) -0.005(3) Cl31 0.056(4) 0.089(6) 0.111(8) -0.034(7) -0.023(6) -0.026(4) Cl32 0.092(7) 0.105(8) 0.219(15) -0.059(12) -0.059(10) -0.018(6) P1 0.0484(14) 0.0350(12) 0.0280(10) -0.0102(9) 0.0049(9) -0.0262(11) O4 0.064(9) 0.062(9) 0.067(9) 0.007(8) 0.007(8) -0.008(8) O5 0.055(4) 0.051(4) 0.063(5) -0.037(4) 0.010(3) -0.019(3) O6 0.050(4) 0.081(6) 0.071(5) -0.033(4) 0.026(4) -0.041(4) N11 0.035(4) 0.039(4) 0.031(4) -0.017(3) 0.007(3) -0.015(3) N12 0.047(5) 0.049(5) 0.025(4) -0.008(3) -0.002(3) -0.022(4) N21 0.035(4) 0.030(4) 0.039(4) -0.014(3) 0.000(3) -0.008(3) N22 0.036(4) 0.044(4) 0.041(4) -0.026(4) 0.004(3) -0.011(4) N31 0.033(4) 0.037(4) 0.031(4) -0.009(3) 0.004(3) -0.020(3) N32 0.036(4) 0.049(5) 0.036(4) -0.013(3) 0.012(3) -0.024(4) C1 0.038(5) 0.024(4) 0.036(5) -0.011(4) 0.002(4) -0.015(4) C2 0.048(5) 0.032(5) 0.034(5) -0.017(4) 0.009(4) -0.026(4) C3 0.044(5) 0.037(5) 0.027(5) -0.008(4) 0.006(4) -0.028(4) C4 0.036(8) 0.040(8) 0.035(9) -0.017(7) 0.015(7) -0.012(7) C5 0.036(5) 0.042(5) 0.030(4) -0.011(4) 0.010(4) -0.019(4) C6 0.045(6) 0.038(5) 0.038(5) -0.014(4) 0.000(4) -0.011(4) C13 0.067(8) 0.068(7) 0.016(4) -0.007(5) 0.004(4) -0.017(6) C14 0.051(7) 0.050(6) 0.040(6) -0.002(5) -0.012(5) -0.005(5) C15 0.036(5) 0.046(6) 0.042(5) -0.012(4) 0.008(4) -0.013(5) C23 0.043(6) 0.060(6) 0.061(6) -0.041(6) 0.001(5) -0.017(5) C24 0.037(5) 0.034(5) 0.077(7) -0.031(5) -0.004(5) -0.005(4) C25 0.078(8) 0.061(7) 0.047(6) 0.006(5) -0.009(6) -0.048(7) C33 0.047(6) 0.060(7) 0.045(6) -0.011(5) 0.015(5) -0.025(5) C34 0.041(6) 0.062(7) 0.066(7) -0.025(6) 0.009(5) -0.033(5) C35 0.045(5) 0.037(5) 0.053(6) -0.020(4) 0.011(4) -0.022(4) C111 0.050(6) 0.030(5) 0.050(5) -0.012(4) -0.005(4) -0.020(4) C112 0.088(8) 0.064(7) 0.043(5) -0.022(5) 0.018(5) -0.058(6) C113 0.079(8) 0.063(7) 0.036(5) -0.015(5) -0.011(5) -0.037(6) C114 0.079(10) 0.085(9) 0.079(9) -0.044(8) -0.007(7) -0.030(8) C115 0.049(8) 0.175(18) 0.115(13) -0.096(13) 0.018(8) -0.036(9) C116 0.044(7) 0.112(11) 0.072(8) -0.056(8) -0.002(6) -0.017(7) C121 0.043(5) 0.040(5) 0.034(5) -0.012(4) 0.009(4) -0.027(4) C122 0.065(6) 0.056(6) 0.037(5) -0.013(4) 0.012(4) -0.046(5) C123 0.056(6) 0.069(7) 0.041(5) -0.026(5) 0.020(4) -0.045(6) C124 0.050(6) 0.057(6) 0.052(6) -0.015(5) 0.014(5) -0.033(5) C125 0.067(7) 0.043(6) 0.062(7) -0.009(5) 0.020(6) -0.030(6) C126 0.065(7) 0.044(6) 0.055(6) -0.016(5) 0.033(5) -0.032(5) C131 0.049(5) 0.046(5) 0.042(5) -0.023(4) 0.018(4) -0.035(5) C132 0.059(6) 0.040(5) 0.050(6) -0.013(4) -0.002(5) -0.026(5) C133 0.069(7) 0.032(5) 0.042(5) -0.006(4) 0.001(5) -0.022(5) C134 0.056(7) 0.058(7) 0.061(7) -0.031(6) 0.019(5) -0.025(6) C135 0.061(7) 0.054(6) 0.066(7) -0.037(6) 0.020(6) -0.027(6) C136 0.052(6) 0.060(7) 0.048(6) -0.031(5) 0.009(5) -0.021(5) C201 0.089(11) 0.130(11) 0.142(12) -0.071(11) -0.031(11) -0.004(10) C202 0.103(11) 0.130(11) 0.170(14) -0.089(12) -0.046(12) 0.002(10) B1 0.040(6) 0.040(6) 0.024(5) -0.012(4) 0.010(4) -0.015(5) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Hg1 . Ir1 . 2.615(3) yes Hg1 . Cl1 . 2.408(6) yes Hg1 . P1 . 3.380(3) yes Ir1 . P1 2_666 2.428(6) yes Ir1 . C3 2_666 2.092(10) yes Ir1 . P1 . 2.356(6) yes Ir1 . C3 . 2.004(10) yes Ir1 . C4 . 1.952(9) yes W1 . N11 . 2.294(7) yes W1 . N21 . 2.197(7) yes W1 . N31 . 2.207(7) yes W1 . C1 . 1.818(9) yes W1 . C5 . 1.976(10) yes W1 . C6 . 1.962(10) yes Cl1 . O4 2_666 1.544(10) yes Cl2 . C201 . 1.735(18) yes Cl2 . C202 . 1.820(18) yes Cl31 . C201 . 1.758(18) yes Cl32 . C202 . 1.845(18) yes P1 . C111 . 1.828(9) yes P1 . C121 . 1.829(9) yes P1 . C131 . 1.836(10) yes O4 . C4 . 1.149(9) yes O5 . C5 . 1.167(11) yes O6 . C6 . 1.161(11) yes N11 . N12 . 1.359(10) yes N11 . C15 . 1.332(12) yes N12 . C13 . 1.356(12) yes N12 . B1 . 1.539(13) yes N21 . N22 . 1.363(10) yes N21 . C25 . 1.303(13) yes N22 . C23 . 1.337(12) yes N22 . B1 . 1.553(13) yes N31 . N32 . 1.371(10) yes N31 . C35 . 1.336(11) yes N32 . C33 . 1.353(12) yes N32 . B1 . 1.542(13) yes C1 . C2 . 1.421(13) yes C2 . C3 . 1.205(12) yes C13 . C14 . 1.348(16) yes C13 . H131 . 1.000 no C14 . C15 . 1.360(14) yes C14 . H141 . 1.000 no C15 . H151 . 1.000 no C23 . C24 . 1.365(16) yes C23 . H231 . 1.000 no C24 . C25 . 1.394(17) yes C24 . H241 . 1.000 no C25 . H251 . 1.000 no C33 . C34 . 1.362(15) yes C33 . H331 . 1.000 no C34 . C35 . 1.409(14) yes C34 . H341 . 1.000 no C35 . H351 . 1.000 no C111 . C112 . 1.402(14) yes C111 . C116 . 1.356(16) yes C112 . C113 . 1.398(15) yes C112 . H1121 . 1.000 no C113 . C114 . 1.374(19) yes C113 . H1131 . 1.000 no C114 . C115 . 1.39(2) yes C114 . H1141 . 1.000 no C115 . C116 . 1.419(18) yes C115 . H1151 . 1.000 no C116 . H1161 . 1.000 no C121 . C122 . 1.378(14) yes C121 . C126 . 1.380(13) yes C122 . C123 . 1.395(13) yes C122 . H1221 . 1.000 no C123 . C124 . 1.374(14) yes C123 . H1231 . 1.000 no C124 . C125 . 1.373(16) yes C124 . H1241 . 1.000 no C125 . C126 . 1.396(14) yes C125 . H1251 . 1.000 no C126 . H1261 . 1.000 no C131 . C132 . 1.424(14) yes C131 . C136 . 1.376(13) yes C132 . C133 . 1.375(15) yes C132 . H1321 . 1.000 no C133 . C134 . 1.396(15) yes C133 . H1331 . 1.000 no C134 . C135 . 1.350(16) yes C134 . H1341 . 1.000 no C135 . C136 . 1.409(16) yes C135 . H1351 . 1.000 no C136 . H1361 . 1.000 no C201 . H2011 . 1.000 no C201 . H2012 . 1.000 no C202 . H2021 . 1.000 no C202 . H2022 . 1.000 no B1 . H1 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Ir1 . Hg1 . Cl1 . 178.4(2) yes C3 2_666 Ir1 . P1 2_666 91.6(3) yes C3 2_666 Ir1 . Hg1 . 80.6(3) yes P1 2_666 Ir1 . Hg1 . 84.73(12) yes C3 2_666 Ir1 . P1 . 85.2(3) yes P1 2_666 Ir1 . P1 . 170.11(14) yes Hg1 . Ir1 . P1 . 85.51(17) yes C3 2_666 Ir1 . C3 . 168.53(17) yes P1 2_666 Ir1 . C3 . 85.3(3) yes Hg1 . Ir1 . C3 . 88.2(3) yes C3 2_666 Ir1 . C4 . 104.7(13) yes P1 2_666 Ir1 . C4 . 95.9(18) yes Hg1 . Ir1 . C4 . 174.7(12) yes P1 . Ir1 . C3 . 96.0(3) yes P1 . Ir1 . C4 . 94.0(18) yes C3 . Ir1 . C4 . 86.6(13) yes N11 . W1 . N21 . 79.9(3) yes N11 . W1 . N31 . 80.2(2) yes N21 . W1 . N31 . 81.4(3) yes N11 . W1 . C1 . 178.3(3) yes N21 . W1 . C1 . 101.5(3) yes N31 . W1 . C1 . 100.7(3) yes N11 . W1 . C5 . 92.7(3) yes N21 . W1 . C5 . 171.8(3) yes N31 . W1 . C5 . 93.8(3) yes C1 . W1 . C5 . 85.9(4) yes N11 . W1 . C6 . 94.3(3) yes N21 . W1 . C6 . 93.4(3) yes N31 . W1 . C6 . 172.9(3) yes C1 . W1 . C6 . 84.9(4) yes C5 . W1 . C6 . 90.9(4) yes Ir1 . P1 . C111 . 110.8(3) yes Ir1 . P1 . C121 . 115.9(3) yes C111 . P1 . C121 . 102.5(4) yes Ir1 2_666 P1 . C111 . 115.8(3) yes Ir1 2_666 P1 . C121 . 120.8(3) yes Ir1 2_666 P1 . C131 . 108.3(3) yes Ir1 . P1 . C131 . 118.2(3) yes C111 . P1 . C131 . 106.0(4) yes C121 . P1 . C131 . 101.8(4) yes W1 . N11 . N12 . 120.4(5) yes W1 . N11 . C15 . 132.6(6) yes N12 . N11 . C15 . 107.1(7) yes N11 . N12 . C13 . 108.0(8) yes N11 . N12 . B1 . 121.3(7) yes C13 . N12 . B1 . 130.7(8) yes W1 . N21 . N22 . 124.5(6) yes W1 . N21 . C25 . 133.3(8) yes N22 . N21 . C25 . 102.3(8) yes N21 . N22 . C23 . 111.1(8) yes N21 . N22 . B1 . 118.8(7) yes C23 . N22 . B1 . 130.1(8) yes W1 . N31 . N32 . 122.0(5) yes W1 . N31 . C35 . 131.0(6) yes N32 . N31 . C35 . 107.0(7) yes N31 . N32 . C33 . 108.8(8) yes N31 . N32 . B1 . 121.2(7) yes C33 . N32 . B1 . 130.0(8) yes W1 . C1 . C2 . 173.9(7) yes C1 . C2 . C3 . 177.6(9) yes Ir1 2_666 C3 . C2 . 172.8(7) yes Ir1 . C3 . C2 . 170.5(8) yes Ir1 . C4 . O4 . 170(4) yes W1 . C5 . O5 . 178.7(7) yes W1 . C6 . O6 . 179.2(8) yes N12 . C13 . C14 . 108.5(9) yes N12 . C13 . H131 . 125.750 no C14 . C13 . H131 . 125.728 no C13 . C14 . C15 . 106.5(9) yes C13 . C14 . H141 . 126.776 no C15 . C14 . H141 . 126.765 no C14 . C15 . N11 . 109.9(9) yes C14 . C15 . H151 . 125.040 no N11 . C15 . H151 . 125.033 no N22 . C23 . C24 . 109.9(9) yes N22 . C23 . H231 . 125.016 no C24 . C23 . H231 . 125.038 no C23 . C24 . C25 . 100.4(9) yes C23 . C24 . H241 . 129.788 no C25 . C24 . H241 . 129.810 no C24 . C25 . N21 . 116.3(10) yes C24 . C25 . H251 . 121.836 no N21 . C25 . H251 . 121.830 no N32 . C33 . C34 . 109.4(9) yes N32 . C33 . H331 . 125.315 no C34 . C33 . H331 . 125.308 no C33 . C34 . C35 . 104.9(8) yes C33 . C34 . H341 . 127.527 no C35 . C34 . H341 . 127.539 no C34 . C35 . N31 . 109.8(9) yes C34 . C35 . H351 . 125.098 no N31 . C35 . H351 . 125.090 no P1 . C111 . C112 . 119.9(8) yes P1 . C111 . C116 . 120.2(8) yes C112 . C111 . C116 . 119.9(10) yes C111 . C112 . C113 . 120.3(11) yes C111 . C112 . H1121 . 119.864 no C113 . C112 . H1121 . 119.854 no C112 . C113 . C114 . 118.3(11) yes C112 . C113 . H1131 . 120.827 no C114 . C113 . H1131 . 120.827 no C113 . C114 . C115 . 123.1(12) yes C113 . C114 . H1141 . 118.428 no C115 . C114 . H1141 . 118.430 no C114 . C115 . C116 . 116.7(13) yes C114 . C115 . H1151 . 121.663 no C116 . C115 . H1151 . 121.678 no C115 . C116 . C111 . 121.6(12) yes C115 . C116 . H1161 . 119.178 no C111 . C116 . H1161 . 119.180 no P1 . C121 . C122 . 123.2(6) yes P1 . C121 . C126 . 118.0(7) yes C122 . C121 . C126 . 118.6(8) yes C121 . C122 . C123 . 120.9(8) yes C121 . C122 . H1221 . 119.572 no C123 . C122 . H1221 . 119.560 no C122 . C123 . C124 . 119.4(10) yes C122 . C123 . H1231 . 120.297 no C124 . C123 . H1231 . 120.290 no C123 . C124 . C125 . 120.8(10) yes C123 . C124 . H1241 . 119.597 no C125 . C124 . H1241 . 119.596 no C124 . C125 . C126 . 119.1(9) yes C124 . C125 . H1251 . 120.456 no C126 . C125 . H1251 . 120.453 no C125 . C126 . C121 . 121.1(10) yes C125 . C126 . H1261 . 119.436 no C121 . C126 . H1261 . 119.433 no P1 . C131 . C132 . 117.3(7) yes P1 . C131 . C136 . 124.6(8) yes C132 . C131 . C136 . 117.9(9) yes C131 . C132 . C133 . 120.4(9) yes C131 . C132 . H1321 . 119.802 no C133 . C132 . H1321 . 119.796 no C132 . C133 . C134 . 121.0(10) yes C132 . C133 . H1331 . 119.484 no C134 . C133 . H1331 . 119.497 no C133 . C134 . C135 . 118.5(11) yes C133 . C134 . H1341 . 120.753 no C135 . C134 . H1341 . 120.766 no C134 . C135 . C136 . 122.1(10) yes C134 . C135 . H1351 . 118.947 no C136 . C135 . H1351 . 118.936 no C135 . C136 . C131 . 120.0(10) yes C135 . C136 . H1361 . 119.986 no C131 . C136 . H1361 . 119.991 no Cl31 . C201 . Cl2 . 103.9(11) yes Cl31 . C201 . H2011 . 110.679 no Cl2 . C201 . H2011 . 110.673 no Cl31 . C201 . H2012 . 111.015 no Cl2 . C201 . H2012 . 111.022 no H2011 . C201 . H2012 . 109.467 no Cl32 . C202 . Cl2 . 118.4(14) yes Cl32 . C202 . H2021 . 107.253 no Cl2 . C202 . H2021 . 107.261 no Cl32 . C202 . H2022 . 107.128 no Cl2 . C202 . H2022 . 107.114 no H2021 . C202 . H2022 . 109.467 no N22 . B1 . N32 . 107.7(7) yes N22 . B1 . N12 . 107.9(7) yes N32 . B1 . N12 . 108.2(8) yes N22 . B1 . H1 . 111.230 no N32 . B1 . H1 . 110.967 no N12 . B1 . H1 . 110.791 no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cl1 Cl32 2.78(2) . . no Cl1 Cl31 3.38(1) . . no Cl2 C34 3.51(1) . 2_765 no O5 C15 3.36(1) . 2_575 no O5 O6 3.372(9) . 2_575 no O5 C201 3.46(6) . 1_465 no O5 C34 3.53(2) . 2_675 no O5 C202 3.58(6) . 1_465 no O6 C201 3.11(6) . 2_665 no O6 C124 3.33(2) . 2_566 no O6 C15 3.46(2) . 2_575 no O6 C202 3.57(5) . 2_665 no N11 C125 3.59(2) . 1_564 no N21 C24 3.37(1) . 2_665 no N22 C25 3.59(1) . 2_665 no N31 C24 3.44(1) . 2_665 no N31 C125 3.53(1) . 1_564 no C6 C201 3.29(6) . 2_665 no C23 C25 3.48(2) . 2_665 no C24 C25 3.48(2) . 2_665 no C24 C123 3.51(2) . 1_554 no C25 C25 3.56(3) . 2_665 no C25 C201 3.59(3) . 2_665 no C33 C126 3.59(1) . 1_564 no #------------------------------------------------------------------------------ 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag HG1 Ir1 P1 C111 . . . . -112.7(4) no HG1 Ir1 P1 C121 . . . . 131.1(3) no HG1 Ir1 P1 C131 . . . . 9.9(4) no Ir1 P1 C111 C112 . . . . 68.3(9) no Ir1 P1 C111 C116 . . . . -111(1) no Ir1 P1 C121 C122 . . . . 14.0(9) no Ir1 P1 C121 C126 . . . . -171.3(7) no Ir1 P1 C131 C132 . . . . 63.5(9) no Ir1 P1 C131 C136 . . . . -113(1) no W1 N11 N12 C13 . . . . 178.6(9) no W1 N11 N12 B1 . . . . -2(2) no W1 N11 C15 C14 . . . . -177.9(9) no W1 N21 N22 C23 . . . . 178.9(7) no W1 N21 N22 B1 . . . . -2(1) no W1 N21 C25 C24 . . . . -178.5(7) no W1 N31 N32 C33 . . . . -179.3(5) no W1 N31 N32 B1 . . . . 1.7(9) no W1 N31 C35 C34 . . . . 177.8(6) no P1 C111 C112 C113 . . . . -178.4(9) no P1 C111 C116 C115 . . . . 179(1) no P1 C121 C122 C123 . . . . 171.2(7) no P1 C121 C126 C125 . . . . -171.6(9) no P1 C131 C132 C133 . . . . -177.7(9) no P1 C131 C136 C135 . . . . 176.5(9) no N11 W1 N21 N22 . . . . 42.4(7) no N11 W1 N21 C25 . . . . -140(1) no N11 W1 N31 N32 . . . . -42.5(6) no N11 W1 N31 C35 . . . . 138.1(8) no N11 N12 C13 C14 . . . . -0(2) no N11 N12 B1 N22 . . . . 60(1) no N11 N12 B1 N32 . . . . -57(1) no N11 C15 C14 C13 . . . . -1(2) no N12 N11 W1 N21 . . . . -40.3(9) no N12 N11 W1 N31 . . . . 42.6(9) no N12 N11 W1 C5 . . . . 136.0(9) no N12 N11 W1 C6 . . . . -132.9(9) no N12 N11 C15 C14 . . . . 1(2) no N12 C13 C14 C15 . . . . 1(2) no N12 B1 N22 N21 . . . . -58(1) no N12 B1 N22 C23 . . . . 121(1) no N12 B1 N32 N31 . . . . 57.7(9) no N12 B1 N32 C33 . . . . -121.1(9) no N21 W1 N11 C15 . . . . 139(1) no N21 W1 N31 N32 . . . . 38.7(5) no N21 W1 N31 C35 . . . . -140.7(7) no N21 N22 C23 C24 . . . . -0(1) no N21 N22 B1 N32 . . . . 58(1) no N21 C25 C24 C23 . . . . -0(1) no N22 N21 W1 N31 . . . . -39.2(7) no N22 N21 W1 C1 . . . . -138.5(7) no N22 N21 W1 C6 . . . . 136.1(7) no N22 N21 C25 C24 . . . . -0(1) no N22 C23 C24 C25 . . . . 0(1) no N22 B1 N12 C13 . . . . -121(1) no N22 B1 N32 N31 . . . . -59(1) no N22 B1 N32 C33 . . . . 122.5(9) no N31 W1 N11 C15 . . . . -138(1) no N31 W1 N21 C25 . . . . 139(1) no N31 N32 C33 C34 . . . . 1(1) no N31 C35 C34 C33 . . . . 2(1) no N32 N31 W1 C1 . . . . 138.9(6) no N32 N31 W1 C5 . . . . -134.6(6) no N32 N31 C35 C34 . . . . -1.7(9) no N32 C33 C34 C35 . . . . -2(1) no N32 B1 N12 C13 . . . . 123(1) no N32 B1 N22 C23 . . . . -123(1) no C1 W1 N21 C25 . . . . 40(1) no C1 W1 N31 C35 . . . . -40.5(8) no C3 Ir1 P1 C111 . . . . -25.1(5) no C3 Ir1 P1 C121 . . . . -141.2(4) no C3 Ir1 P1 C131 . . . . 97.5(5) no C3 Ir1 P1 C111 . . 2_666 2_666 -159.6(4) no C3 Ir1 P1 C121 . . 2_666 2_666 -35.0(4) no C3 Ir1 P1 C131 . . 2_666 2_666 81.6(5) no C4 Ir1 P1 C111 . . . . 62(1) no C4 Ir1 P1 C121 . . . . -54(1) no C4 Ir1 P1 C131 . . . . -175(1) no C4 Ir1 P1 C111 . . 2_666 2_666 114(1) no C4 Ir1 P1 C121 . . 2_666 2_666 -121(1) no C4 Ir1 P1 C131 . . 2_666 2_666 -5(1) no C5 W1 N11 C15 . . . . -45(1) no C5 W1 N31 C35 . . . . 46.0(7) no C6 W1 N11 C15 . . . . 46(1) no C6 W1 N21 C25 . . . . -46(1) no C13 N12 N11 C15 . . . . -1(1) no C14 C13 N12 B1 . . . . -180(1) no C15 N11 N12 B1 . . . . 179(1) no C23 N22 N21 C25 . . . . 0(1) no C24 C23 N22 B1 . . . . -180(1) no C25 N21 N22 B1 . . . . 179.6(9) no C33 N32 N31 C35 . . . . 0.3(9) no C34 C33 N32 B1 . . . . -179.8(8) no C35 N31 N32 B1 . . . . -178.8(7) no C111 P1 C121 C122 . . . . -106.8(9) no C111 P1 C121 C126 . . . . 67.9(8) no C111 P1 C131 C132 . . . . -171.5(8) no C111 P1 C131 C136 . . . . 12(1) no C111 C112 C113 C114 . . . . -0(2) no C111 C116 C115 C114 . . . . -0(3) no C112 C111 P1 C121 . . . . -167.4(9) no C112 C111 P1 C131 . . . . -61.1(9) no C112 C111 C116 C115 . . . . -1(2) no C112 C113 C114 C115 . . . . -1(2) no C113 C112 C111 C116 . . . . 1(2) no C113 C114 C115 C116 . . . . 1(3) no C116 C111 P1 C121 . . . . 13(1) no C116 C111 P1 C131 . . . . 119(1) no C121 P1 C131 C132 . . . . -65(1) no C121 P1 C131 C136 . . . . 119(1) no C121 C122 C123 C124 . . . . 1(2) no C121 C126 C125 C124 . . . . -1(2) no C122 C121 P1 C131 . . . . 143.7(9) no C122 C121 C126 C125 . . . . 3(2) no C122 C123 C124 C125 . . . . 1(2) no C123 C122 C121 C126 . . . . -3(1) no C123 C124 C125 C126 . . . . -1(2) no C126 C121 P1 C131 . . . . -41.6(9) no C131 C132 C133 C134 . . . . 2(2) no C131 C136 C135 C134 . . . . 0(2) no C132 C131 C136 C135 . . . . 0(2) no C132 C133 C134 C135 . . . . -1(2) no C133 C132 C131 C136 . . . . -1(2) no C133 C134 C135 C136 . . . . 0(2) no #------------------------------------------------------------------------------ # start Validation Reply Form _vrf_PLAT431_rian19 ; PROBLEM: Short Inter HL..A Contact Cl1 .. Cl32 .. 2.78 Ang. RESPONSE: ... This comes from the disorder - each of these sites has half-occupancy. ; # end Validation Reply Form #===END= # Attachment 'New Compound 8b.cif' data_rian20a _database_code_depnum_ccdc_archive 'CCDC 689224' _audit_creation_date 05-17-05 _audit_creation_method CRYSTALS_ver_12-03-99 # 7220937 rian20a _audit_update_record ; 2005-05-17 - Report on C87 H98 B2 Cl Hg Ir N12 O5 P2 W2 by Anthony C. Willis for Anthony F. Hill and Rian Dewhurst 2005-05-17- passes checkcif tests with minor warnings 2009-01-29 - modify cif for referee ; #============================================================================== # 4. TEXT _publ_section_abstract #Text of the abstract ; The crystal structure of [{(C~15~H~22~BN~6~)W(CO)~2~C~3~}~2~Ir(HgCl)(CO){P(C~6~H~5~)~3~}~2~].solvate is reported. ; _publ_section_comment #Text of the paper ; The unit cell contains one [{(C~15~H~22~BN~6~)W(CO)~2~C~3~}~2~Ir(HgCl)(CO){P(C~6~H~5~)~3~}~2~] molecule plus solvate molecules. The organometallic species is centred on a crystallographic inversion symmetry operation. The HgCl and CO groups on the Ir each have only one-half occupancy and are disordered with respect to each other. The Ir atom was initially at 1/2,1/2,1/2, but its anisotropic displacement ellipsoid was elongated in the direction of the Hg atom and the Hg---Ir distance was shorter than would have been expected. Ihe Ir atom was therefore displaced from the inversion centre in the direction away from the Hg atom. Initially a restraint was placed on the Ir---Hg distance, but later it was removed. Restraints were placed on the Ir---C and C---O distances and on the displacement parameters of C4 and O4 as they are in close proximity to the inversion image of the Hg atom. A region of electron density was observed away from the principal species, presumably indicating the presence of molecules of solvation. It exhibited 5 adjacent peaks of almost equal intensity. The crystals had been produced from CH~2~Cl~2~, with ethanol and hexane having been used during synthesis. Attempts to model the electron density as disordered dichloromethane molecules was not successful. A fair fit can be obtained for a n-pentane molecule. Possibly it represents disordered hexane with multiple terminal sites of low occupancy not being observed. Restraints were placed on distances, angles and displacement parameters in this molecule. The biggest peaks in the final difference electron density map are near to W or Ir atoms and have no chemical significance. ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions #Captions to figures ; ? ; _publ_section_exptl_refinement # see also _refine_ls_hydrogen for refinement keywords. ; H atoms were included at idealized positions and ride on the atom to which they are attached. The methyl hydrogens of the C~15~H~22~BN~6~ groups have been oriented to match peaks in difference electron density maps. ; _publ_section_exptl_prep ; The compound was prepared by RDD and recrystallized from dichloromethane, tetrahydrofuran, ethanol and hexane being present in earlier synthetic steps. The sample ID was RD-4,88. ; _refine_special_details #Text of the paper ; The unit cell contains one [{(C~15~H~22~BN~6~)W(CO)~2~C~3~}~2~Ir(HgCl)(CO){P(C~6~H~5~)~3~}~2~] molecule plus solvate molecules. The organometallic species is centred on a crystallographic inversion symmetry operation. The HgCl and CO groups on the Ir each have only one-half occupancy and are disordered with respect to each other. The Ir atom was initially at 1/2,1/2,1/2, but its anisotropic displacement ellipsoid was elongated in the direction of the Hg atom and the Hg---Ir distance was shorter than would have been expected. Ihe Ir atom was therefore displaced from the inversion centre in the direction away from the Hg atom. Initially a restraint was placed on the Ir---Hg distance, but later it was removed. Restraints were placed on the Ir---C and C---O distances and on the displacement parameters of C4 and O4 as they are in close proximity to the inversion image of the Hg atom. A region of electron density was observed away from the principal species, presumably indicating the presence of molecules of solvation. It exhibited 5 adjacent peaks of almost equal intensity. The crystals had been produced from CH~2~Cl~2~, with ethanol and hexane having been used during synthesis. Attempts to model the electron density as disordered dichloromethane molecules was not successful. A fair fit can be obtained for a n-pentane molecule. Possibly it represents disordered hexane with multiple terminal sites of low occupancy not being observed. Restraints were placed on distances, angles and displacement parameters in this molecule. H atoms were included at idealized positions and ride on the atom to which they are attached. The methyl hydrogens of the C~15~H~22~BN~6~ groups have been oriented to match peaks in difference electron density maps. ; #========================================================================== _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point ? # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment noref #**************************************************************************** # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al 2003) ; _computing_publication_material ; CRYSTALS (Watkin et al 2003) ; _computing_molecular_graphics ; ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997) ; #============================================================= _cell_length_a 11.4118(4) _cell_angle_alpha 81.4328(17) _cell_length_b 13.3666(4) _cell_angle_beta 72.8924(16) _cell_length_c 15.9096(3) _cell_angle_gamma 69.1166(12) _cell_volume 2164.41(11) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z # choose from: rm (reference molecule of # known chirality), ad (anomolous # dispersion - ie. Flack param), rmad # (both rm and ad), syn (known from # synthetic pathway), unk (unknown) # or . (not applicable). _chemical_absolute_configuration . loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 International_Tables_Vol_IV_Table_2.2B 'B ' 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 International_Tables_Vol_IV_Table_2.2B 'Cl ' 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 International_Tables_Vol_IV_Table_2.2B 'Hg ' -2.3894 9.2266 20.6809 0.5450 19.0417 8.4484 21.6575 1.5729 5.9676 38.3246 12.6089 International_Tables_Vol_IV_Table_2.2B 'Ir ' -1.4442 7.9887 27.3049 1.5928 16.7296 8.8655 15.6115 0.4179 5.8338 45.0011 11.4722 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B 'P ' 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 International_Tables_Vol_IV_Table_2.2B 'W ' -0.8490 6.8722 29.0818 1.7203 15.4300 9.2259 14.4327 0.3217 5.1198 57.0560 9.8875 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 1 _chemical_formula_sum ' C87 H98 B2 Cl Hg Ir N12 O5 P2 W2 ' _chemical_formula_moiety ' C77 H74 B2 Cl Hg Ir N12 O5 P2 W2 , 2(C5 H12)' _chemical_compound_source ; ? ; _chemical_formula_weight 2271.35 _cell_measurement_reflns_used 70955 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27 _cell_measurement_temperature 200 _exptl_crystal_description ' plate ' _exptl_crystal_colour ' red ' _exptl_crystal_size_min 0.08 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.40 _exptl_crystal_density_diffrn 1.742 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1106 _exptl_absorpt_coefficient_mu 6.074 _diffrn_measurement_device_type ; Nonius Kappa CCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; COLLECT (Nonius BV, 1997) ; _computing_data_reduction ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_structure_solution ; SIR92 (Altomare et al, 1994) ; _diffrn_measurement_method ' \f and \w scans with CCD ' _diffrn_special_details ; CCD data collecting conditions- phi and omega scans of width 1.1 deg at rate 22 sec/frame, crystal-detector distance 28mm, multiple scan sets so over 95 percent of data collected with 2-fold redundancy or more. ; # Absorption correction loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 1 0 0.060 0 -1 0 0.030 6 3 -1 0.068 -6 -3 1 0.134 -1 -1 4 0.149 1 0 1 0.101 -1 1 -4 0.151 3 3 -12 0.127 3 -1 -1 0.038 -16 5 -4 0.147 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.230 _exptl_absorpt_correction_T_max 0.601 _exptl_absorpt_process_details ; via Gaussian method (Coppens, 1970) implemented in maXus (2000) ; #_diffrn_reflns_av_R_equivalents 0.054 # Sheldrick geometric definitions 0.30 0.62 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 200 _diffrn_reflns_number 45949 _reflns_number_total 9962 _diffrn_reflns_av_R_equivalents 0.07 # Number of reflections with Friedels Law is 9962 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 9992 _diffrn_reflns_theta_min 1.341 _diffrn_reflns_theta_max 27.5 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.547 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _reflns_limit_h_min -13 _reflns_limit_h_max 14 _reflns_limit_k_min -17 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 20 _refine_diff_density_min -1.56 _refine_diff_density_max 1.57 _refine_ls_number_reflns 6453 _refine_ls_number_restraints 40 _refine_ls_number_parameters 526 #_refine_ls_R_factor_ref 0.0325 _refine_ls_wR_factor_ref 0.0369 _refine_ls_goodness_of_fit_ref 1.0852 #_reflns_number_all 9925 _refine_ls_R_factor_all 0.0568 _refine_ls_wR_factor_all 0.0444 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 6453 _refine_ls_R_factor_gt 0.0325 _refine_ls_wR_factor_gt 0.0369 _refine_ls_shift/su_max 0.017 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.33 -0.0617 1.07 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 ## -------------------REFERENCES ----------------------## ## Insert your own references - in alphabetic order _publ_section_references ; Mackay, S., Gilmore, C. J.,Edwards, C., Stewart, N. & Shankland, K. (2000). maXus Computer Program for the Solution and Refinement of Crystal Structures. Nonius, The Netherlands, MacScience, Japan & The University of Glasgow. Coppens, P. (1970). The Evaluation of Absorption and Extinction in Single-Crystal Structure Analysis. Crystallographic Computing. F. R. Ahmed, S. R. Hall and C. P. Huber, eds., Munksgaard. Copenhagen. pp 255-270. Larson, A.C. (1970). The Inclusion of Secondary Extinction in Least-Squares Refinement in Crystal Structures. Crystallographic Computing. F. R. Ahmed, S. R. Hall and C. P. Huber, eds., Munksgaard. Copenhagen. pp 291-294 Altomare, A., Cascarano, G., Giacovazzo C., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius BV, COLLECT Software, 1997-2001) Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994), Acta Cryst, A50, 411-437 Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.8. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Johnson, C.K. (1976) ORTEP-II, A Fortran Thermal-Ellipsoid Plot Program, Report ORNL-5138, Oak Ridge National Laboratory, Oak Ridge, Tennessee, USA. ; # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Hg1 Hg 0.29378(8) 0.63951(5) 0.51354(6) 0.0408 0.5000 Uani . U . . . . Ir1 Ir 0.51740(18) 0.4902(2) 0.4994(2) 0.0293 0.5000 Uani D . . . . . W1 W 0.63645(2) 0.655772(16) 0.090252(12) 0.0294 1.0000 Uani . . . . . . Cl1 Cl 0.0908(5) 0.7783(4) 0.5291(4) 0.0935 0.5000 Uani . . . . . . P1 P 0.57522(14) 0.62233(11) 0.54425(8) 0.0339 1.0000 Uani . . . . . . O4 O 0.7937(11) 0.3232(9) 0.4778(9) 0.0745 0.5000 Uani D U . . . . O5 O 0.3491(4) 0.6732(4) 0.1068(3) 0.0548 1.0000 Uani . . . . . . O6 O 0.6998(5) 0.4123(3) 0.0612(3) 0.0527 1.0000 Uani . . . . . . N11 N 0.6879(4) 0.7090(3) -0.0546(3) 0.0323 1.0000 Uani . . . . . . N12 N 0.7667(4) 0.7715(3) -0.0820(3) 0.0331 1.0000 Uani . . . . . . N21 N 0.8385(4) 0.6484(4) 0.0747(3) 0.0340 1.0000 Uani . . . . . . N22 N 0.8791(4) 0.7343(4) 0.0387(3) 0.0340 1.0000 Uani . . . . . . N31 N 0.5919(4) 0.8288(3) 0.1046(3) 0.0339 1.0000 Uani . . . . . . N32 N 0.6675(4) 0.8847(3) 0.0496(3) 0.0331 1.0000 Uani . . . . . . C1 C 0.5993(5) 0.6130(4) 0.2075(4) 0.0350 1.0000 Uani . . . . . . C2 C 0.5687(5) 0.5807(5) 0.2951(4) 0.0379 1.0000 Uani . . . . . . C3 C 0.5456(6) 0.5523(5) 0.3722(3) 0.0392 1.0000 Uani . . . . . . C4 C 0.690(2) 0.3842(19) 0.488(2) 0.0408 0.5000 Uani D . . . . . C5 C 0.4537(6) 0.6702(5) 0.0986(3) 0.0390 1.0000 Uani . . . . . . C6 C 0.6803(5) 0.5011(5) 0.0684(4) 0.0409 1.0000 Uani . . . . . . C13 C 0.8019(5) 0.7812(5) -0.1718(3) 0.0379 1.0000 Uani . . . . . . C14 C 0.7445(6) 0.7238(5) -0.2023(3) 0.0409 1.0000 Uani . . . . . . C15 C 0.6747(5) 0.6799(4) -0.1283(4) 0.0379 1.0000 Uani . . . . . . C16 C 0.8889(7) 0.8427(6) -0.2225(5) 0.0570 1.0000 Uani . . . . . . C17 C 0.5948(7) 0.6114(5) -0.1237(4) 0.0481 1.0000 Uani . . . . . . C23 C 0.9965(5) 0.7199(5) 0.0517(4) 0.0406 1.0000 Uani . . . . . . C24 C 1.0328(5) 0.6221(5) 0.0961(4) 0.0382 1.0000 Uani . . . . . . C25 C 0.9342(5) 0.5794(4) 0.1092(3) 0.0362 1.0000 Uani . . . . . . C26 C 1.0653(6) 0.8001(6) 0.0208(5) 0.0527 1.0000 Uani . . . . . . C27 C 0.9281(6) 0.4731(5) 0.1519(4) 0.0484 1.0000 Uani . . . . . . C33 C 0.6117(6) 0.9905(4) 0.0651(4) 0.0400 1.0000 Uani . . . . . . C34 C 0.4997(6) 1.0033(5) 0.1304(4) 0.0451 1.0000 Uani . . . . . . C35 C 0.4897(5) 0.9007(5) 0.1554(4) 0.0396 1.0000 Uani . . . . . . C36 C 0.6693(8) 1.0716(5) 0.0160(5) 0.0534 1.0000 Uani . . . . . . C37 C 0.3858(7) 0.8702(6) 0.2240(5) 0.0532 1.0000 Uani . . . . . . C111 C 0.6128(6) 0.7166(5) 0.4543(4) 0.0394 1.0000 Uani . . . . . . C112 C 0.7217(6) 0.6788(5) 0.3839(4) 0.0459 1.0000 Uani . . . . . . C113 C 0.7505(7) 0.7446(6) 0.3109(4) 0.0544 1.0000 Uani . . . . . . C114 C 0.6670(8) 0.8491(6) 0.3072(5) 0.0634 1.0000 Uani . . . . . . C115 C 0.5577(8) 0.8859(6) 0.3753(6) 0.0687 1.0000 Uani . . . . . . C116 C 0.5306(7) 0.8198(6) 0.4487(5) 0.0529 1.0000 Uani . . . . . . C121 C 0.7208(6) 0.5629(5) 0.5855(4) 0.0410 1.0000 Uani . . . . . . C122 C 0.7270(6) 0.4772(6) 0.6472(4) 0.0501 1.0000 Uani . . . . . . C123 C 0.8299(7) 0.4378(7) 0.6850(5) 0.0616 1.0000 Uani . . . . . . C124 C 0.9263(7) 0.4813(7) 0.6629(5) 0.0642 1.0000 Uani . . . . . . C125 C 0.9228(7) 0.5675(7) 0.6012(5) 0.0602 1.0000 Uani . . . . . . C126 C 0.8196(6) 0.6080(6) 0.5628(5) 0.0508 1.0000 Uani . . . . . . C131 C 0.4654(5) 0.7061(4) 0.6353(4) 0.0375 1.0000 Uani . . . . . . C132 C 0.3506(6) 0.6919(5) 0.6871(4) 0.0440 1.0000 Uani . . . . . . C133 C 0.2753(7) 0.7547(6) 0.7576(4) 0.0574 1.0000 Uani . . . . . . C134 C 0.3120(8) 0.8348(6) 0.7761(4) 0.0599 1.0000 Uani . . . . . . C135 C 0.4267(8) 0.8494(6) 0.7269(5) 0.0590 1.0000 Uani . . . . . . C136 C 0.5058(7) 0.7845(5) 0.6573(4) 0.0492 1.0000 Uani . . . . . . C501 C 0.7873(17) 0.9236(13) 0.5445(13) 0.1505 1.0000 Uani D U . . . . C502 C 0.789(2) 0.9422(17) 0.4560(15) 0.1935 1.0000 Uani D U . . . . C503 C 0.870(2) 1.0085(16) 0.3985(14) 0.1885 1.0000 Uani D U . . . . C504 C 0.983(2) 0.9074(18) 0.3548(15) 0.2123 1.0000 Uani D U . . . . C505 C 0.9868(15) 0.9083(13) 0.2622(13) 0.1556 1.0000 Uani D U . . . . B1 B 0.7962(6) 0.8240(5) -0.0138(4) 0.0341 1.0000 Uani . . . . . . H1 H 0.8439 0.8748 -0.0441 0.0430 1.0000 Uiso R . . . . . H141 H 0.7517 0.7154 -0.2652 0.0466 1.0000 Uiso R . . . . . H161 H 0.9013 0.8389 -0.2870 0.0651 1.0000 Uiso R . . . . . H162 H 0.8487 0.9193 -0.2061 0.0651 1.0000 Uiso R . . . . . H163 H 0.9750 0.8112 -0.2084 0.0651 1.0000 Uiso R . . . . . H171 H 0.5972 0.5989 -0.1847 0.0613 1.0000 Uiso R . . . . . H172 H 0.5031 0.6482 -0.0908 0.0613 1.0000 Uiso R . . . . . H173 H 0.6305 0.5411 -0.0927 0.0613 1.0000 Uiso R . . . . . H241 H 1.1150 0.5882 0.1152 0.0454 1.0000 Uiso R . . . . . H261 H 1.1497 0.7731 0.0374 0.0674 1.0000 Uiso R . . . . . H262 H 1.0101 0.8696 0.0489 0.0674 1.0000 Uiso R . . . . . H263 H 1.0824 0.8113 -0.0446 0.0674 1.0000 Uiso R . . . . . H271 H 1.0079 0.4346 0.1730 0.0580 1.0000 Uiso R . . . . . H272 H 0.8495 0.4843 0.2031 0.0580 1.0000 Uiso R . . . . . H273 H 0.9228 0.4293 0.1082 0.0580 1.0000 Uiso R . . . . . H341 H 0.4368 1.0725 0.1557 0.0544 1.0000 Uiso R . . . . . H361 H 0.6126 1.1442 0.0379 0.0688 1.0000 Uiso R . . . . . H362 H 0.7575 1.0549 0.0250 0.0688 1.0000 Uiso R . . . . . H363 H 0.6767 1.0708 -0.0481 0.0688 1.0000 Uiso R . . . . . H371 H 0.3198 0.9357 0.2536 0.0614 1.0000 Uiso R . . . . . H372 H 0.4248 0.8185 0.2686 0.0614 1.0000 Uiso R . . . . . H373 H 0.3429 0.8358 0.1959 0.0614 1.0000 Uiso R . . . . . H1121 H 0.7799 0.6027 0.3865 0.0553 1.0000 Uiso R . . . . . H1131 H 0.8300 0.7174 0.2617 0.0689 1.0000 Uiso R . . . . . H1141 H 0.6862 0.8979 0.2549 0.0762 1.0000 Uiso R . . . . . H1151 H 0.4975 0.9612 0.3717 0.0783 1.0000 Uiso R . . . . . H1161 H 0.4509 0.8473 0.4977 0.0614 1.0000 Uiso R . . . . . H1221 H 0.6568 0.4441 0.6641 0.0620 1.0000 Uiso R . . . . . H1231 H 0.8336 0.3762 0.7294 0.0726 1.0000 Uiso R . . . . . H1241 H 1.0003 0.4515 0.6910 0.0751 1.0000 Uiso R . . . . . H1251 H 0.9938 0.5996 0.5848 0.0747 1.0000 Uiso R . . . . . H1261 H 0.8160 0.6699 0.5186 0.0634 1.0000 Uiso R . . . . . H1321 H 0.3221 0.6351 0.6731 0.0546 1.0000 Uiso R . . . . . H1331 H 0.1941 0.7421 0.7952 0.0664 1.0000 Uiso R . . . . . H1341 H 0.2552 0.8825 0.8256 0.0686 1.0000 Uiso R . . . . . H1351 H 0.4533 0.9072 0.7413 0.0725 1.0000 Uiso R . . . . . H1361 H 0.5907 0.7933 0.6232 0.0597 1.0000 Uiso R . . . . . H5011 H 0.7306 0.8793 0.5736 0.1941 1.0000 Uiso R . . . . . H5012 H 0.7525 0.9936 0.5734 0.1941 1.0000 Uiso R . . . . . H5013 H 0.8776 0.8845 0.5503 0.1941 1.0000 Uiso R . . . . . H5021 H 0.697 0.9798 0.4529 0.2351 1.0000 Uiso R . . . . . H5022 H 0.823 0.8707 0.4298 0.2351 1.0000 Uiso R . . . . . H5031 H 0.898 1.0483 0.4330 0.2245 1.0000 Uiso R . . . . . H5032 H 0.827 1.0595 0.3555 0.2245 1.0000 Uiso R . . . . . H5041 H 1.067 0.9087 0.3596 0.2501 1.0000 Uiso R . . . . . H5042 H 0.967 0.8409 0.3860 0.2501 1.0000 Uiso R . . . . . H5051 H 1.0584 0.8438 0.2349 0.2018 1.0000 Uiso R . . . . . H5052 H 1.0028 0.9747 0.2309 0.2018 1.0000 Uiso R . . . . . H5053 H 0.9020 0.9069 0.2573 0.2018 1.0000 Uiso 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 Hg1 0.0418(4) 0.0405(4) 0.0407(2) -0.0034(3) -0.0116(2) -0.0132(3) Ir1 0.0372(9) 0.0319(8) 0.02217(16) 0.0006(5) -0.0073(7) -0.0165(7) W1 0.03302(11) 0.03191(11) 0.02435(10) 0.00144(7) -0.00799(7) -0.01267(8) Cl1 0.064(2) 0.077(3) 0.120(4) -0.017(3) -0.031(3) 0.011(2) P1 0.0420(7) 0.0376(7) 0.0267(6) -0.0025(5) -0.0064(5) -0.0203(6) O4 0.041(6) 0.068(7) 0.105(8) -0.021(6) -0.027(5) 0.006(5) O5 0.042(2) 0.056(3) 0.071(3) 0.006(2) -0.022(2) -0.020(2) O6 0.063(3) 0.031(2) 0.065(3) -0.0059(19) -0.009(2) -0.021(2) N11 0.040(2) 0.036(2) 0.024(2) 0.0023(16) -0.0088(17) -0.0174(18) N12 0.038(2) 0.035(2) 0.026(2) 0.0025(16) -0.0082(17) -0.0138(18) N21 0.032(2) 0.038(2) 0.031(2) 0.0031(17) -0.0082(17) -0.0113(18) N22 0.034(2) 0.036(2) 0.035(2) 0.0021(17) -0.0099(17) -0.0150(18) N31 0.036(2) 0.031(2) 0.037(2) -0.0014(17) -0.0134(18) -0.0115(18) N32 0.039(2) 0.031(2) 0.032(2) 0.0060(17) -0.0164(18) -0.0108(18) C1 0.035(3) 0.034(3) 0.039(3) 0.002(2) -0.011(2) -0.014(2) C2 0.046(3) 0.040(3) 0.032(3) -0.001(2) -0.008(2) -0.023(2) C3 0.048(3) 0.049(3) 0.023(2) -0.001(2) -0.002(2) -0.025(3) C4 0.0418(4) 0.0405(4) 0.0407(2) -0.0034(3) -0.0116(2) -0.0132(3) C5 0.045(3) 0.044(3) 0.029(3) 0.001(2) -0.013(2) -0.014(2) C6 0.035(3) 0.051(4) 0.035(3) 0.000(2) -0.003(2) -0.017(2) C13 0.035(3) 0.046(3) 0.025(2) 0.005(2) -0.009(2) -0.006(2) C14 0.044(3) 0.050(3) 0.023(2) -0.001(2) -0.008(2) -0.009(2) C15 0.036(3) 0.038(3) 0.038(3) -0.006(2) -0.011(2) -0.006(2) C16 0.050(4) 0.065(4) 0.047(4) 0.010(3) -0.003(3) -0.022(3) C17 0.061(4) 0.051(3) 0.042(3) -0.010(3) -0.019(3) -0.021(3) C23 0.037(3) 0.049(3) 0.043(3) 0.000(2) -0.013(2) -0.021(2) C24 0.031(3) 0.042(3) 0.040(3) 0.000(2) -0.013(2) -0.008(2) C25 0.034(3) 0.040(3) 0.031(2) -0.004(2) -0.010(2) -0.006(2) C26 0.046(3) 0.053(4) 0.069(4) 0.005(3) -0.021(3) -0.027(3) C27 0.049(3) 0.042(3) 0.053(4) 0.011(3) -0.023(3) -0.012(3) C33 0.050(3) 0.028(3) 0.049(3) 0.001(2) -0.030(3) -0.009(2) C34 0.053(3) 0.033(3) 0.049(3) -0.011(2) -0.023(3) -0.003(2) C35 0.040(3) 0.039(3) 0.037(3) -0.012(2) -0.014(2) -0.001(2) C36 0.079(5) 0.034(3) 0.059(4) 0.004(3) -0.036(3) -0.021(3) C37 0.052(4) 0.052(4) 0.049(4) -0.016(3) -0.006(3) -0.011(3) C111 0.046(3) 0.043(3) 0.036(3) 0.000(2) -0.009(2) -0.024(3) C112 0.056(3) 0.043(3) 0.039(3) -0.001(2) -0.002(3) -0.026(3) C113 0.065(4) 0.070(4) 0.038(3) 0.000(3) -0.006(3) -0.041(4) C114 0.071(5) 0.069(5) 0.051(4) 0.022(3) -0.017(3) -0.032(4) C115 0.068(5) 0.053(4) 0.075(5) 0.019(4) -0.022(4) -0.014(4) C116 0.051(4) 0.052(4) 0.050(4) 0.012(3) -0.016(3) -0.015(3) C121 0.045(3) 0.044(3) 0.034(3) -0.009(2) -0.008(2) -0.015(2) C122 0.053(4) 0.061(4) 0.040(3) 0.003(3) -0.017(3) -0.023(3) C123 0.060(4) 0.078(5) 0.043(4) 0.003(3) -0.024(3) -0.013(4) C124 0.046(4) 0.094(6) 0.047(4) -0.015(4) -0.018(3) -0.008(4) C125 0.044(3) 0.091(5) 0.052(4) -0.015(4) -0.009(3) -0.027(4) C126 0.045(3) 0.061(4) 0.052(4) -0.011(3) -0.011(3) -0.022(3) C131 0.045(3) 0.037(3) 0.036(3) -0.004(2) -0.012(2) -0.017(2) C132 0.050(3) 0.047(3) 0.039(3) -0.006(2) -0.010(2) -0.021(3) C133 0.062(4) 0.059(4) 0.045(4) -0.012(3) -0.002(3) -0.019(3) C134 0.080(5) 0.053(4) 0.039(3) -0.015(3) -0.009(3) -0.013(3) C135 0.077(5) 0.046(4) 0.059(4) -0.020(3) -0.023(4) -0.014(3) C136 0.062(4) 0.041(3) 0.046(3) -0.008(3) -0.012(3) -0.018(3) C501 0.154(11) 0.120(10) 0.211(17) 0.009(11) -0.086(12) -0.061(9) C502 0.185(13) 0.159(12) 0.244(17) -0.017(13) -0.078(14) -0.045(10) C503 0.176(13) 0.180(14) 0.205(16) 0.021(12) -0.061(12) -0.058(11) C504 0.178(13) 0.197(14) 0.250(17) 0.006(14) -0.048(14) -0.062(11) C505 0.120(9) 0.145(11) 0.240(18) 0.030(12) -0.079(12) -0.078(9) B1 0.037(3) 0.038(3) 0.033(3) 0.007(2) -0.015(2) -0.017(2) _refine_ls_extinction_coef 90(10) _refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eq 22' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Hg1 . Ir1 . 2.5905(16) yes Hg1 . Cl1 . 2.367(4) yes Ir1 . P1 2_666 2.395(3) yes Ir1 . C3 2_666 2.024(6) yes Ir1 . P1 . 2.356(3) yes Ir1 . C3 . 2.047(6) yes Ir1 . C4 . 1.945(19) yes W1 . N11 . 2.275(4) yes W1 . N21 . 2.213(4) yes W1 . N31 . 2.216(4) yes W1 . C1 . 1.838(5) yes W1 . C5 . 1.990(6) yes W1 . C6 . 2.005(6) yes P1 . C111 . 1.819(6) yes P1 . C121 . 1.834(6) yes P1 . C131 . 1.827(6) yes O4 . C4 . 1.156(18) yes O5 . C5 . 1.148(7) yes O6 . C6 . 1.144(7) yes N11 . N12 . 1.376(6) yes N11 . C15 . 1.353(7) yes N12 . C13 . 1.365(6) yes N12 . B1 . 1.546(7) yes N21 . N22 . 1.374(6) yes N21 . C25 . 1.352(7) yes N22 . C23 . 1.357(7) yes N22 . B1 . 1.546(7) yes N31 . N32 . 1.375(6) yes N31 . C35 . 1.347(7) yes N32 . C33 . 1.355(7) yes N32 . B1 . 1.535(8) yes C1 . C2 . 1.375(8) yes C2 . C3 . 1.209(7) yes C13 . C14 . 1.382(8) yes C13 . C16 . 1.492(8) yes C14 . C15 . 1.393(8) yes C14 . H141 . 1.000 no C15 . C17 . 1.487(8) yes C16 . H161 . 1.000 no C16 . H162 . 1.000 no C16 . H163 . 1.000 no C17 . H171 . 1.000 no C17 . H172 . 1.000 no C17 . H173 . 1.000 no C23 . C24 . 1.374(8) yes C23 . C26 . 1.492(8) yes C24 . C25 . 1.386(8) yes C24 . H241 . 1.000 no C25 . C27 . 1.497(8) yes C26 . H261 . 1.000 no C26 . H262 . 1.000 no C26 . H263 . 1.000 no C27 . H271 . 1.000 no C27 . H272 . 1.000 no C27 . H273 . 1.000 no C33 . C34 . 1.362(9) yes C33 . C36 . 1.473(9) yes C34 . C35 . 1.405(9) yes C34 . H341 . 1.000 no C35 . C37 . 1.488(9) yes C36 . H361 . 1.000 no C36 . H362 . 1.000 no C36 . H363 . 1.000 no C37 . H371 . 1.000 no C37 . H372 . 1.000 no C37 . H373 . 1.000 no C111 . C112 . 1.398(8) yes C111 . C116 . 1.372(9) yes C112 . C113 . 1.381(9) yes C112 . H1121 . 1.000 no C113 . C114 . 1.386(11) yes C113 . H1131 . 1.000 no C114 . C115 . 1.378(11) yes C114 . H1141 . 1.000 no C115 . C116 . 1.383(10) yes C115 . H1151 . 1.000 no C116 . H1161 . 1.000 no C121 . C122 . 1.389(9) yes C121 . C126 . 1.395(8) yes C122 . C123 . 1.378(9) yes C122 . H1221 . 1.000 no C123 . C124 . 1.357(11) yes C123 . H1231 . 1.000 no C124 . C125 . 1.395(12) yes C124 . H1241 . 1.000 no C125 . C126 . 1.387(10) yes C125 . H1251 . 1.000 no C126 . H1261 . 1.000 no C131 . C132 . 1.388(8) yes C131 . C136 . 1.407(8) yes C132 . C133 . 1.378(9) yes C132 . H1321 . 1.000 no C133 . C134 . 1.376(10) yes C133 . H1331 . 1.000 no C134 . C135 . 1.378(11) yes C134 . H1341 . 1.000 no C135 . C136 . 1.391(9) yes C135 . H1351 . 1.000 no C136 . H1361 . 1.000 no C501 . C502 . 1.388(19) yes C501 . H5011 . 1.000 no C501 . H5012 . 1.000 no C501 . H5013 . 1.000 no C502 . C503 . 1.52(2) yes C502 . H5021 . 1.000 no C502 . H5022 . 1.000 no C503 . C504 . 1.57(2) yes C503 . H5031 . 1.000 no C503 . H5032 . 1.000 no C504 . C505 . 1.46(2) yes C504 . H5041 . 1.000 no C504 . H5042 . 1.000 no C505 . H5051 . 1.000 no C505 . H5052 . 1.000 no C505 . H5053 . 1.000 no B1 . H1 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Ir1 . Hg1 . Cl1 . 178.46(16) yes P1 2_666 Ir1 . C3 2_666 91.0(2) yes P1 2_666 Ir1 . Hg1 . 86.78(8) yes C3 2_666 Ir1 . Hg1 . 88.09(19) yes P1 2_666 Ir1 . P1 . 170.71(7) yes C3 2_666 Ir1 . P1 . 88.6(2) yes Hg1 . Ir1 . P1 . 83.94(9) yes P1 2_666 Ir1 . C3 . 86.99(19) yes C3 2_666 Ir1 . C3 . 169.12(9) yes Hg1 . Ir1 . C3 . 81.12(18) yes P1 2_666 Ir1 . C4 . 96.1(9) yes C3 2_666 Ir1 . C4 . 93.2(9) yes Hg1 . Ir1 . C4 . 176.8(9) yes P1 . Ir1 . C3 . 91.6(2) yes P1 . Ir1 . C4 . 93.2(9) yes C3 . Ir1 . C4 . 97.6(9) yes N11 . W1 . N21 . 80.63(15) yes N11 . W1 . N31 . 80.96(16) yes N21 . W1 . N31 . 83.40(16) yes N11 . W1 . C1 . 178.33(19) yes N21 . W1 . C1 . 97.72(19) yes N31 . W1 . C1 . 98.6(2) yes N11 . W1 . C5 . 96.31(18) yes N21 . W1 . C5 . 176.36(19) yes N31 . W1 . C5 . 94.2(2) yes C1 . W1 . C5 . 85.3(2) yes N11 . W1 . C6 . 95.12(19) yes N21 . W1 . C6 . 96.0(2) yes N31 . W1 . C6 . 176.08(19) yes C1 . W1 . C6 . 85.3(2) yes C5 . W1 . C6 . 86.2(2) yes Ir1 . P1 . C111 . 112.2(2) yes Ir1 . P1 . C121 . 111.5(2) yes C111 . P1 . C121 . 106.1(3) yes Ir1 . P1 . C131 . 120.42(19) yes C111 . P1 . C131 . 104.8(3) yes C121 . P1 . C131 . 100.3(3) yes W1 . N11 . N12 . 118.9(3) yes W1 . N11 . C15 . 133.7(4) yes N12 . N11 . C15 . 106.6(4) yes N11 . N12 . C13 . 109.9(4) yes N11 . N12 . B1 . 120.3(4) yes C13 . N12 . B1 . 129.7(5) yes W1 . N21 . N22 . 121.0(3) yes W1 . N21 . C25 . 131.8(4) yes N22 . N21 . C25 . 106.0(4) yes N21 . N22 . C23 . 110.4(4) yes N21 . N22 . B1 . 119.0(4) yes C23 . N22 . B1 . 130.4(4) yes W1 . N31 . N32 . 121.2(3) yes W1 . N31 . C35 . 131.5(4) yes N32 . N31 . C35 . 107.0(4) yes N31 . N32 . C33 . 109.6(5) yes N31 . N32 . B1 . 119.7(4) yes C33 . N32 . B1 . 130.7(5) yes W1 . C1 . C2 . 178.5(4) yes C1 . C2 . C3 . 177.8(6) yes Ir1 . C3 . C2 . 174.6(5) yes Ir1 . C4 . O4 . 178(2) yes W1 . C5 . O5 . 175.9(5) yes W1 . C6 . O6 . 175.4(5) yes N12 . C13 . C14 . 107.4(5) yes N12 . C13 . C16 . 123.3(6) yes C14 . C13 . C16 . 129.3(5) yes C13 . C14 . C15 . 106.6(5) yes C13 . C14 . H141 . 126.708 no C15 . C14 . H141 . 126.707 no C14 . C15 . N11 . 109.7(5) yes C14 . C15 . C17 . 128.8(5) yes N11 . C15 . C17 . 121.5(5) yes C13 . C16 . H161 . 109.466 no C13 . C16 . H162 . 109.467 no H161 . C16 . H162 . 109.476 no C13 . C16 . H163 . 109.467 no H161 . C16 . H163 . 109.476 no H162 . C16 . H163 . 109.476 no C15 . C17 . H171 . 109.467 no C15 . C17 . H172 . 109.466 no H171 . C17 . H172 . 109.476 no C15 . C17 . H173 . 109.467 no H171 . C17 . H173 . 109.476 no H172 . C17 . H173 . 109.476 no N22 . C23 . C24 . 107.0(5) yes N22 . C23 . C26 . 123.0(5) yes C24 . C23 . C26 . 130.0(5) yes C23 . C24 . C25 . 107.0(5) yes C23 . C24 . H241 . 126.487 no C25 . C24 . H241 . 126.487 no C24 . C25 . N21 . 109.6(5) yes C24 . C25 . C27 . 128.2(5) yes N21 . C25 . C27 . 122.1(5) yes C23 . C26 . H261 . 109.467 no C23 . C26 . H262 . 109.467 no H261 . C26 . H262 . 109.475 no C23 . C26 . H263 . 109.466 no H261 . C26 . H263 . 109.476 no H262 . C26 . H263 . 109.476 no C25 . C27 . H271 . 109.467 no C25 . C27 . H272 . 109.466 no H271 . C27 . H272 . 109.476 no C25 . C27 . H273 . 109.467 no H271 . C27 . H273 . 109.475 no H272 . C27 . H273 . 109.476 no N32 . C33 . C34 . 107.9(5) yes N32 . C33 . C36 . 122.6(6) yes C34 . C33 . C36 . 129.5(6) yes C33 . C34 . C35 . 106.9(5) yes C33 . C34 . H341 . 126.561 no C35 . C34 . H341 . 126.562 no C34 . C35 . N31 . 108.6(5) yes C34 . C35 . C37 . 128.6(5) yes N31 . C35 . C37 . 122.8(5) yes C33 . C36 . H361 . 109.467 no C33 . C36 . H362 . 109.466 no H361 . C36 . H362 . 109.476 no C33 . C36 . H363 . 109.466 no H361 . C36 . H363 . 109.476 no H362 . C36 . H363 . 109.476 no C35 . C37 . H371 . 109.467 no C35 . C37 . H372 . 109.467 no H371 . C37 . H372 . 109.476 no C35 . C37 . H373 . 109.467 no H371 . C37 . H373 . 109.476 no H372 . C37 . H373 . 109.476 no P1 . C111 . C112 . 118.5(5) yes P1 . C111 . C116 . 122.1(5) yes C112 . C111 . C116 . 119.0(6) yes C111 . C112 . C113 . 121.3(6) yes C111 . C112 . H1121 . 119.354 no C113 . C112 . H1121 . 119.354 no C112 . C113 . C114 . 118.7(7) yes C112 . C113 . H1131 . 120.659 no C114 . C113 . H1131 . 120.658 no C113 . C114 . C115 . 120.3(6) yes C113 . C114 . H1141 . 119.853 no C115 . C114 . H1141 . 119.852 no C114 . C115 . C116 . 120.6(7) yes C114 . C115 . H1151 . 119.713 no C116 . C115 . H1151 . 119.712 no C115 . C116 . C111 . 120.1(7) yes C115 . C116 . H1161 . 119.945 no C111 . C116 . H1161 . 119.944 no P1 . C121 . C122 . 119.0(5) yes P1 . C121 . C126 . 121.6(5) yes C122 . C121 . C126 . 119.1(6) yes C121 . C122 . C123 . 119.9(7) yes C121 . C122 . H1221 . 120.026 no C123 . C122 . H1221 . 120.025 no C122 . C123 . C124 . 121.1(7) yes C122 . C123 . H1231 . 119.461 no C124 . C123 . H1231 . 119.459 no C123 . C124 . C125 . 120.3(6) yes C123 . C124 . H1241 . 119.862 no C125 . C124 . H1241 . 119.862 no C124 . C125 . C126 . 119.2(7) yes C124 . C125 . H1251 . 120.397 no C126 . C125 . H1251 . 120.397 no C121 . C126 . C125 . 120.4(7) yes C121 . C126 . H1261 . 119.814 no C125 . C126 . H1261 . 119.813 no P1 . C131 . C132 . 124.0(4) yes P1 . C131 . C136 . 117.1(4) yes C132 . C131 . C136 . 118.7(5) yes C131 . C132 . C133 . 121.1(6) yes C131 . C132 . H1321 . 119.463 no C133 . C132 . H1321 . 119.463 no C132 . C133 . C134 . 119.9(7) yes C132 . C133 . H1331 . 120.034 no C134 . C133 . H1331 . 120.034 no C133 . C134 . C135 . 120.3(6) yes C133 . C134 . H1341 . 119.859 no C135 . C134 . H1341 . 119.861 no C134 . C135 . C136 . 120.4(6) yes C134 . C135 . H1351 . 119.792 no C136 . C135 . H1351 . 119.792 no C131 . C136 . C135 . 119.4(6) yes C131 . C136 . H1361 . 120.278 no C135 . C136 . H1361 . 120.279 no C502 . C501 . H5011 . 109.468 no C502 . C501 . H5012 . 109.450 no H5011 . C501 . H5012 . 109.477 no C502 . C501 . H5013 . 109.482 no H5011 . C501 . H5013 . 109.475 no H5012 . C501 . H5013 . 109.476 no C501 . C502 . C503 . 118.5(15) yes C501 . C502 . H5021 . 107.176 no C503 . C502 . H5021 . 107.169 no C501 . C502 . H5022 . 107.144 no C503 . C502 . H5022 . 107.159 no H5021 . C502 . H5022 . 109.467 no C502 . C503 . C504 . 93.4(13) yes C502 . C503 . H5031 . 113.333 no C504 . C503 . H5031 . 113.325 no C502 . C503 . H5032 . 113.321 no C504 . C503 . H5032 . 113.329 no H5031 . C503 . H5032 . 109.467 no C503 . C504 . C505 . 109.9(15) yes C503 . C504 . H5041 . 109.378 no C505 . C504 . H5041 . 109.380 no C503 . C504 . H5042 . 109.362 no C505 . C504 . H5042 . 109.362 no H5041 . C504 . H5042 . 109.466 no C504 . C505 . H5051 . 109.467 no C504 . C505 . H5052 . 109.457 no H5051 . C505 . H5052 . 109.476 no C504 . C505 . H5053 . 109.476 no H5051 . C505 . H5053 . 109.476 no H5052 . C505 . H5053 . 109.476 no N12 . B1 . N22 . 108.3(4) yes N12 . B1 . N32 . 108.9(4) yes N22 . B1 . N32 . 109.1(4) yes N12 . B1 . H1 . 110.505 no N22 . B1 . H1 . 110.231 no N32 . B1 . H1 . 109.734 no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cl1 C501 3.27(2) . 1_455 no Cl1 C504 3.35(2) . 1_455 no Cl1 C503 3.44(3) . 2_676 no O5 O6 3.317(8) . 2_665 no O6 C26 3.251(7) . 2_765 no O6 C24 3.261(7) . 2_765 no O6 C17 3.33(1) . 2_665 no O6 C23 3.358(6) . 2_765 no C6 C24 3.561(7) . 2_765 no C13 C34 3.569(7) . 2_675 no C115 C502 3.59(3) . . no C125 C125 3.59(2) . 2_766 no #------------------------------------------------------------------------------ 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Hg1 Ir1 P1 C111 . . . . -79.5(2) no Hg1 Ir1 P1 C121 . . . . 161.5(2) no Hg1 Ir1 P1 C131 . . . . 44.5(2) no Ir1 P1 C111 C112 . . . . -65.6(7) no Ir1 P1 C111 C116 . . . . 107.1(7) no Ir1 P1 C121 C122 . . . . -49.1(6) no Ir1 P1 C121 C126 . . . . 137.1(5) no Ir1 P1 C131 C132 . . . . 5.7(6) no Ir1 P1 C131 C136 . . . . -179.0(4) no W1 N11 N12 C13 . . . . 170.9(3) no W1 N11 N12 B1 . . . . -12.6(5) no W1 N11 C15 C14 . . . . -168.9(3) no W1 N11 C15 C17 . . . . 11.3(7) no W1 N21 N22 C23 . . . . 167.9(4) no W1 N21 N22 B1 . . . . -16.6(6) no W1 N21 C25 C24 . . . . -166.3(4) no W1 N21 C25 C27 . . . . 15.2(8) no W1 N31 N32 C33 . . . . 172.9(4) no W1 N31 N32 B1 . . . . -9.2(7) no W1 N31 C35 C34 . . . . -171.5(5) no W1 N31 C35 C37 . . . . 7(1) no P1 C111 C112 C113 . . . . 175.6(7) no P1 C111 C116 C115 . . . . -174.4(8) no P1 C121 C122 C123 . . . . -174.0(5) no P1 C121 C126 C125 . . . . 174.0(6) no P1 C131 C132 C133 . . . . 176.8(5) no P1 C131 C136 C135 . . . . -179.1(5) no N11 W1 N21 N22 . . . . 51.7(4) no N11 W1 N21 C25 . . . . -142.8(5) no N11 W1 N31 N32 . . . . -37.7(4) no N11 W1 N31 C35 . . . . 134.5(6) no N11 N12 C13 C14 . . . . -0.0(5) no N11 N12 C13 C16 . . . . -179.1(5) no N11 N12 B1 N22 . . . . 67.2(5) no N11 N12 B1 N32 . . . . -51.4(5) no N11 C15 C14 C13 . . . . 0.1(6) no N12 N11 W1 N21 . . . . -36.0(3) no N12 N11 W1 N31 . . . . 48.8(3) no N12 N11 W1 C5 . . . . 142.1(3) no N12 N11 W1 C6 . . . . -131.2(3) no N12 N11 C15 C14 . . . . -0.1(5) no N12 N11 C15 C17 . . . . -179.9(4) no N12 C13 C14 C15 . . . . -0.1(6) no N12 B1 N22 N21 . . . . -50.0(6) no N12 B1 N22 C23 . . . . 124.6(6) no N12 B1 N32 N31 . . . . 65.4(6) no N12 B1 N32 C33 . . . . -117.3(7) no N21 W1 N11 C15 . . . . 131.8(4) no N21 W1 N31 N32 . . . . 43.9(4) no N21 W1 N31 C35 . . . . -144.0(6) no N21 N22 C23 C24 . . . . 0.7(6) no N21 N22 C23 C26 . . . . -179.4(6) no N21 N22 B1 N32 . . . . 68.5(7) no N21 C25 C24 C23 . . . . -0.4(6) no N22 N21 W1 N31 . . . . -30.2(4) no N22 N21 W1 C1 . . . . -128.0(4) no N22 N21 W1 C6 . . . . 146.0(4) no N22 N21 C25 C24 . . . . 0.8(6) no N22 N21 C25 C27 . . . . -177.7(5) no N22 C23 C24 C25 . . . . -0.2(7) no N22 B1 N12 C13 . . . . -117.0(5) no N22 B1 N32 N31 . . . . -52.8(8) no N22 B1 N32 C33 . . . . 124.6(7) no N31 W1 N11 C15 . . . . -143.5(4) no N31 W1 N21 C25 . . . . 135.3(5) no N31 N32 C33 C34 . . . . 0.1(8) no N31 N32 C33 C36 . . . . -179.6(7) no N31 C35 C34 C33 . . . . -1.4(8) no N32 N31 W1 C1 . . . . 140.7(4) no N32 N31 W1 C5 . . . . -133.4(4) no N32 N31 C35 C34 . . . . 1.5(7) no N32 N31 C35 C37 . . . . -179.7(7) no N32 C33 C34 C35 . . . . 0.8(8) no N32 B1 N12 C13 . . . . 124.4(5) no N32 B1 N22 C23 . . . . -117.0(6) no C1 W1 N21 C25 . . . . 37.5(5) no C1 W1 N31 C35 . . . . -47.1(6) no C3 Ir1 P1 C111 . . . . 1.4(3) no C3 Ir1 P1 C121 . . . . -117.6(3) no C3 Ir1 P1 C131 . . . . 125.4(3) no C3 Ir1 P1 C111 . . 2_666 2_666 174.7(2) no C3 Ir1 P1 C121 . . 2_666 2_666 -61.3(3) no C3 Ir1 P1 C131 . . 2_666 2_666 57.4(3) no C5 W1 N11 C15 . . . . -50.2(4) no C5 W1 N31 C35 . . . . 38.8(6) no C6 W1 N11 C15 . . . . 36.5(4) no C6 W1 N21 C25 . . . . -48.5(5) no C13 N12 N11 C15 . . . . 0.1(5) no C13 C14 C15 C17 . . . . 179.8(5) no C14 C13 N12 B1 . . . . -176.2(4) no C15 N11 N12 B1 . . . . 176.6(4) no C15 C14 C13 C16 . . . . 178.9(5) no C16 C13 N12 B1 . . . . 4.8(8) no C23 N22 N21 C25 . . . . -0.9(6) no C23 C24 C25 C27 . . . . 178.0(5) no C24 C23 N22 B1 . . . . -174.2(5) no C25 N21 N22 B1 . . . . 174.6(4) no C25 C24 C23 C26 . . . . 179.9(6) no C26 C23 N22 B1 . . . . 6(1) no C33 N32 N31 C35 . . . . -1.0(7) no C33 C34 C35 C37 . . . . 179.9(8) no C34 C33 N32 B1 . . . . -177.5(6) no C35 N31 N32 B1 . . . . 176.9(6) no C35 C34 C33 C36 . . . . -179.5(8) no C36 C33 N32 B1 . . . . 3(1) no C111 P1 C121 C122 . . . . -171.6(5) no C111 P1 C121 C126 . . . . 14.5(6) no C111 P1 C131 C132 . . . . 133.3(5) no C111 P1 C131 C136 . . . . -51.4(6) no C111 C112 C113 C114 . . . . -2(1) no C111 C116 C115 C114 . . . . 0(2) no C112 C111 P1 C121 . . . . 56.5(7) no C112 C111 P1 C131 . . . . 162.1(6) no C112 C111 C116 C115 . . . . -2(1) no C112 C113 C114 C115 . . . . 0(2) no C113 C112 C111 C116 . . . . 3(1) no C113 C114 C115 C116 . . . . 1(2) no C116 C111 P1 C121 . . . . -130.8(7) no C116 C111 P1 C131 . . . . -25.2(8) no C121 P1 C131 C132 . . . . -116.8(6) no C121 P1 C131 C136 . . . . 58.4(5) no C121 C122 C123 C124 . . . . -0(1) no C121 C126 C125 C124 . . . . -0(1) no C122 C121 P1 C131 . . . . 79.6(6) no C122 C121 C126 C125 . . . . 0(1) no C122 C123 C124 C125 . . . . 0(1) no C123 C122 C121 C126 . . . . -0(1) no C123 C124 C125 C126 . . . . -0(1) no C126 C121 P1 C131 . . . . -94.3(6) no C131 C132 C133 C134 . . . . 2(1) no C131 C136 C135 C134 . . . . 2(1) no C132 C131 C136 C135 . . . . -3.5(9) no C132 C133 C134 C135 . . . . -3(1) no C133 C132 C131 C136 . . . . 1.5(9) no C133 C134 C135 C136 . . . . 1(1) no C501 C502 C503 C504 . . . . 103(2) no C502 C503 C504 C505 . . . . 111(2) no #------------------------------------------------------------------------------ # start Validation Reply Form _vrf_PLAT410_rian20a ; PROBLEM: Short Intra H...H Contact H5022 .. H5042 .. 1.51 Ang. RESPONSE: ... The solvate is ill-defined so these calculated H positions are not well defined either. ; # end Validation Reply Form #===END