# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry, 1999 # CCDC Number: 186/1534 #============================================================================== data_global #============================================================================== _audit_creation_date 18-02-99 _audit_creation_method from_MolEN_master_file_using_cif_in _audit_update_record ; ? ; # 1. SUBMISSION DETAILS _publ_contact_author ; Ulli Englert Institut fuer Anorganische Chemie RWTH Aachen Prof.-Pirlet-Str.1 52074 Aachen Germany ; _publ_contact_author_email 'ullrich.englert@ac.rwth-aachen.de' _publ_contact_author_fax '(0241) 8888288' _publ_contact_author_phone '(0241) 804666' _publ_requested_journal 'J. Chem. Soc. Dalton. Trans.' _publ_requested_coeditor_name ? _publ_contact_letter ; ?edit? ; # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? # 3. TITLE AND AUTHOR LIST _publ_section_title ; ? ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Braunstein, Pierre' #<--'Last name, first name' ; Laboratoire de Chimie de Coordination UMR 7513 CNRS Universite Louis Pasteur 67070 Strasbourg Cedex France ; 'Englert, Ulli' #<--'Last name, first name' ; Institut fuer Anorganische Chemie RWTH Aachen Prof.-Pirlet-Str.1 52074 Aachen Germany ; 'Herberich, Gerhard E.' #<--'Last name, first name' ; Institut fuer Anorganische Chemie RWTH Aachen Prof.-Pirlet-Str.1 52074 Aachen Germany ; 'Neuschuetz, Mark' #<--'Last name, first name' ; Institut fuer Anorganische Chemie RWTH Aachen Prof.-Pirlet-Str.1 52074 Aachen Germany ; 'Schmidt, Martin U.' #<--'Last name, first name' ; Institut fuer Anorganische Chemie RWTH Aachen Prof.-Pirlet-Str.1 52074 Aachen Germany ; # 4. TEXT _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_experimental ; Backgrounds were obtained from analysis of the scan profile (Blessing, Coppens _& Becker, 1974) ; _publ_section_references ; Blessing, R.H., Coppens, P. & Becker, P. (1974). J. Appl. Cryst., 7, 488-492. Enraf-Nonius, CAD4 Operations Manual, Delft, 1977. Fair, C.K. (1990). MolEN, An Interactive Intelligent System for Crystal Structure Analysis, User Manual, Enraf - Nonius, Delft, The Netherlands. International Tables for X-Ray Crystallography, T. Hahn E Vol. A, D. Reidel Publ. Comp., Dordrecht, (1983) Johnson, C.K. (1976). ORTEP. Report ORNL-5138. Oak Ridge National Laboratory, Tennessee, USA. Zachariasen, W.H. (1963). Acta Crystallogr., 16, 1139-1144. ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ?none? ?none? ; data_MN5 # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description 'translucent fragment' _exptl_crystal_colour green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _chemical_name_common ; complex 1 ; _chemical_formula_sum 'C26 H18 B2 Hg1 O6 Re2' _chemical_formula_weight 1021.04 _symmetry_cell_setting monoclinic _symmetry_space_group_name_h-m 'P21/n' _cell_length_a 10.911(4) _cell_length_b 8.467(3) _cell_length_c 15.374(6) _cell_angle_alpha 90.00 _cell_angle_beta 110.13(3) _cell_angle_gamma 90.00 _cell_volume 1333.6(9) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8 _cell_measurement_theta_max 12 _cell_formula_units_z 2.00 _exptl_crystal_density_diffrn 2.54 _exptl_crystal_density_meas none _diffrn_radiation_type Mo-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 14.960 _cell_measurement_temperature 253 _exptl_crystal_F_000 924 # 6. DATA COLLECTION _diffrn_ambient_temperature 253 _diffrn_measurement_device Enraf_Nonius_CAD4 _diffrn_measurement_method \w _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.090 _exptl_absorpt_correction_T_max 0.107 _diffrn_reflns_number 1532 _reflns_number_total 1427 _reflns_number_observed 1191 _reflns_observed_criterion >1.0\s(I) _diffrn_reflns_av_R_equivalents 0.068 _diffrn_reflns_theta_min 3.1 _diffrn_reflns_theta_max 23.0 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_max 15 _diffrn_standards_number 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0.00 # 7. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_R_factor_obs 0.059 _refine_ls_wR_factor_obs 0.059 _refine_ls_hydrogen_treatment 'riding' _refine_ls_number_reflns 1191 _refine_ls_number_parameters 100 _refine_ls_number_restraints 39 _refine_ls_goodness_of_fit_obs 1.648 _refine_ls_weighting_scheme '4Fo^2^/ (\s^2^(Fo^2^) + 0.0009 Fo^4^)' _refine_ls_shift/esd_max 0.005 _refine_diff_density_max 1.6161 _refine_diff_density_min -2.1453 _refine_ls_extinction_method isotropic_(Zachariasen,_1963) _refine_ls_extinction_coef 0.23E-07 _atom_type_scat_source International_Tables_for_Xray_Crystallography # 8. COMPUTING DATA _computing_data_collection CAD4_(Enraf-Nonius,_1977) _computing_cell_refinement CAD4_(Enraf-Nonius,_1977) _computing_data_reduction PROCESS_MolEN_(Fair,_1990) _computing_structure_solution isotropic_(Zachariasen,_1963) _computing_structure_refinement LSFM_MolEN_(Fair,_1990) _computing_molecular_graphics ORTEP_(Johnson,_1976) _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag Hg 0.0000 0.0000 0.0000 0.0376(4) Ueq calc Re -0.0457(1) 0.0621(1) 0.16162(6) 0.0363(3) Ueq . O1 -0.294(2) 0.167(2) 0.004(1) 0.072(7) Ueq . O2 -0.231(2) -0.027(3) 0.266(1) 0.119(9) Ueq . O3 0.000(2) -0.293(2) 0.160(1) 0.10(1) Ueq . C1 -0.204(3) 0.121(4) 0.058(2) 0.064(8) Uiso . C2 -0.160(3) 0.014(4) 0.227(2) 0.072(9) Uiso . C3 -0.023(3) -0.160(3) 0.157(2) 0.049(7) Uiso . C10 0.173(3) 0.099(3) 0.241(2) 0.054(7) Uiso . C11 0.095(2) 0.146(3) 0.296(1) 0.043(6) Uiso . C12 0.015(3) 0.272(3) 0.251(2) 0.051(7) Uiso . C13 0.029(2) 0.312(3) 0.169(1) 0.044(7) Uiso . C14 0.235(2) 0.244(3) 0.098(1) 0.028(5) Uiso . C15 0.345(3) 0.157(3) 0.110(2) 0.054(7) Uiso . C16 0.425(3) 0.187(3) 0.062(2) 0.073(9) Uiso . C17 0.397(3) 0.308(3) -0.001(2) 0.071(9) Uiso . C18 0.291(3) 0.396(3) -0.015(2) 0.062(8) Uiso . C19 0.209(3) 0.368(3) 0.035(1) 0.050(7) Uiso . B 0.151(3) 0.219(4) 0.163(2) 0.043(8) Uiso . H10 0.2285 0.0054 0.2505 0.0659 Uiso calc H11 0.0988 0.0992 0.3551 0.0517 Uiso calc H12 -0.0469 0.3243 0.2754 0.0616 Uiso calc H13 -0.0260 0.3840 0.1216 0.0528 Uiso calc H15 0.3630 0.0671 0.1526 0.0660 Uiso calc H16 0.5063 0.1265 0.0737 0.0905 Uiso calc H17 0.4540 0.3313 -0.0372 0.0874 Uiso calc H18 0.2701 0.4804 -0.0613 0.0759 Uiso calc H19 0.1321 0.4353 0.0263 0.0609 Uiso calc 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 Hg 0.0345(7) 0.0434(9) 0.0350(5) 0.0029(6) 0.0120(5) -0.0030(6) Re 0.0322(5) 0.0438(7) 0.0330(4) -0.0040(5) 0.0112(3) -0.0038(4) O1 0.04(1) 0.10(2) 0.07(1) 0.02(1) 0.003(9) -0.00(1) O2 0.09(1) 0.20(2) 0.09(1) -0.06(2) 0.055(9) -0.04(1) O3 0.13(2) 0.04(1) 0.08(1) -0.01(1) -0.02(1) -0.01(1) # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Hg Re 2.7483 ? Hg Re 2.7483 ? Re C1 1.97(3) ? Re C2 1.89(3) ? Re C3 1.90(3) ? Re C10 2.29(2) ? Re C11 2.22(2) ? Re C12 2.20(2) ? Re C13 2.26(2) ? O1 C1 1.12(3) ? O2 C2 1.18(3) ? O3 C3 1.16(2) ? C10 C11 1.44(3) ? C10 B 1.53(3) ? C10 H10 0.9800 ? C11 C12 1.40(3) ? C11 H11 0.9800 ? C12 C13 1.37(3) ? C12 H12 0.9800 ? C13 B 1.58(3) ? C13 H13 0.9800 ? C14 C15 1.36(3) ? C14 C19 1.39(3) ? C14 B 1.58(3) ? C15 C16 1.35(3) ? C15 H15 0.9800 ? C16 C17 1.38(3) ? C16 H16 0.9800 ? C17 C18 1.33(3) ? C17 H17 0.9800 ? C18 C19 1.39(3) ? C18 H18 0.9800 ? C19 H19 0.9800 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag Re Hg Re 180.00 ? Hg Re C1 72.52 ? Hg Re C2 142.70 ? Hg Re C3 73.08 ? Hg Re C10 91.64 ? Hg Re C11 128.20 ? Hg Re C12 127.66 ? Hg Re C13 92.99 ? C1 Re C2 86(1) ? C1 Re C3 1071(1) ? C1 Re C10 149.0(9) ? C1 Re C11 143.4(9) ? C1 Re C12 106.9(9) ? C1 Re C13 90.2(9) ? C2 Re C3 86(1) ? C2 Re C10 119.9(9) ? C2 Re C11 86.9(9) ? C2 Re C12 87.(1) ? C2 Re C13 117.7(9) ? C3 Re C10 91.8(9) ? C3 Re C11 107.2(8) ? C3 Re C12 143.7(8) ? C3 Re C13 151.8(9) ? C10 Re C11 37.2(7) ? C10 Re C12 61.6(8) ? C10 Re C13 63.6(8) ? C11 Re C12 36.9(7) ? C11 Re C13 62.0(7) ? C12 Re C13 35.6(7) ? Re C1 O1 174(2) ? Re C2 O2 175(2) ? Re C3 O3 174(2) ? Re C10 C11 69(1) ? Re C10 B 80(1) ? Re C10 H10 116.67 ? C11 C10 B 108(2) ? C11 C10 H10 126.64 ? B C10 H10 124.88 ? Re C11 C10 74(1) ? Re C11 C12 71(1) ? Re C11 H11 121.88 ? C10 C11 C12 108(2) ? C10 C11 H11 125.95 ? C12 C11 H11 125.57 ? Re C12 C11 72(1) ? Re C12 C13 74(1) ? Re C12 H12 120.38 ? C11 C12 C13 113(2) ? C11 C12 H12 123.76 ? C13 C12 H12 122.99 ? Re C13 C12 70(1) ? Re C13 B 80(1) ? Re C13 H13 115.16 ? C12 C13 B 107(2) ? C12 C13 H13 127.71 ? B C13 H13 124.98 ? C15 C14 C19 117(2) ? C15 C14 B 121(2) ? C19 C14 B 121(2) ? C14 C15 C16 123(2) ? C14 C15 H15 118.01 ? C16 C15 H15 119.40 ? C15 C16 C17 120(3) ? C15 C16 H16 121.20 ? C17 C16 H16 118.95 ? C16 C17 C18 120(3) ? C16 C17 H17 121.34 ? C18 C17 H17 118.86 ? C17 C18 C19 121(2) ? C17 C18 H18 119.48 ? C19 C18 H18 119.67 ? C14 C19 C18 120(2) ? C14 C19 H19 119.87 ? C18 C19 H19 120.48 ? C10 B C13 101(2) ? C10 B C14 128(2) ? C13 B C14 131(2) ? # #=END # data_MN1_240592 # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description parallelepiped _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _chemical_name_common ; complex 6b ; _chemical_formula_sum 'C36 H34 B2 Fe2 N2 O4 Pt1' _chemical_formula_weight 887.09 _symmetry_cell_setting triclinic _symmetry_space_group_name_h-m 'P-1' _cell_length_a 8.532(2) _cell_length_b 10.445(3) _cell_length_c 10.430(3) _cell_angle_alpha 100.75(2) _cell_angle_beta 101.13(2) _cell_angle_gamma 101.15(2) _cell_volume 870.3(4) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 13 _cell_measurement_theta_max 17 _cell_formula_units_z 1.00 _exptl_crystal_density_diffrn 1.69 _exptl_crystal_density_meas none _diffrn_radiation_type Mo-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 4.913 _cell_measurement_temperature 248 _exptl_crystal_F_000 436 # 6. DATA COLLECTION _diffrn_ambient_temperature 248 _diffrn_measurement_device Enraf_Nonius_CAD4 _diffrn_measurement_method \w _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.770 _exptl_absorpt_correction_T_max 0.992 _diffrn_reflns_number 3248 _reflns_number_total 2477 _reflns_number_observed 2477 _reflns_observed_criterion >1.0\s(I) _diffrn_reflns_av_R_equivalents 0.018 _diffrn_reflns_theta_min 3.2 _diffrn_reflns_theta_max 27.0 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_max 7 _diffrn_standards_number 3 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0.00 # 7. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0667P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2477 _refine_ls_number_parameters 220 _refine_ls_number_restraints 45 _refine_ls_R_factor_all 0.0304 _refine_ls_R_factor_obs 0.0301 _refine_ls_wR_factor_all 0.0893 _refine_ls_wR_factor_obs 0.0890 _refine_ls_goodness_of_fit_all 1.155 _refine_ls_goodness_of_fit_obs 1.152 _refine_ls_restrained_S_all 1.149 _refine_ls_restrained_S_obs 1.146 _refine_ls_shift/esd_max 0.004 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pt Pt 0.0000 0.0000 0.0000 0.03058(13) Uani 1 d S . Fe Fe 0.02331(10) -0.2030(4) -0.2037(4) 0.0384(2) Uani 1 d . . O1 O 0.3250(8) -0.0003(9) -0.1473(7) 0.062(2) Uani 1 d . . O2 O 0.1709(9) -0.3666(7) -0.0243(8) 0.054(2) Uani 1 d . . N N -0.1163(8) -0.1438(6) 0.0777(7) 0.0355(13) Uani 1 d . . C1 C 0.2017(11) -0.0812(10) -0.1693(8) 0.045(2) Uani 1 d . . C2 C 0.1080(11) -0.3033(10) -0.0927(9) 0.045(2) Uani 1 d . . C11 C -0.0268(12) -0.2051(9) 0.1612(10) 0.044(2) Uani 1 d . . H11 H 0.0935(12) -0.1801(9) 0.1797(10) 0.057 Uiso 1 calc R . C12 C -0.1002(11) -0.2997(9) 0.2193(9) 0.044(2) Uani 1 d . . H12 H -0.0323(11) -0.3415(9) 0.2780(9) 0.057 Uiso 1 calc R . C13 C -0.2705(12) -0.3372(8) 0.1957(9) 0.044(2) Uani 1 d . . C14 C -0.3591(10) -0.2776(9) 0.1101(10) 0.044(2) Uani 1 d . . H14 H -0.4795(10) -0.3036(9) 0.0889(10) 0.057 Uiso 1 calc R . C15 C -0.2822(9) -0.1821(8) 0.0536(9) 0.040(2) Uani 1 d . . H15 H -0.3493(9) -0.1406(8) -0.0059(9) 0.052 Uiso 1 calc R . C16 C -0.3515(21) -0.4438(15) 0.2604(15) 0.066(4) Uani 1 d . . H16A H -0.3408(116) -0.4045(32) 0.3556(30) 0.086 Uiso 1 calc R . H16B H -0.2974(91) -0.5186(51) 0.2525(97) 0.086 Uiso 1 calc R . H16C H -0.4683(38) -0.4766(80) 0.2148(72) 0.086 Uiso 1 calc R . C21 C 0.0011(11) -0.3673(16) -0.3593(18) 0.050(2) Uani 1 d . . H21 H 0.0694(11) -0.4326(16) -0.3564(18) 0.065 Uiso 1 calc R . C22 C -0.1448(14) -0.3781(11) -0.3199(11) 0.061(3) Uani 1 d . . H22 H -0.1984(14) -0.4546(11) -0.2893(11) 0.080 Uiso 1 calc R . C23 C -0.2070(11) -0.2623(11) -0.3298(10) 0.054(2) Uani 1 d . . H23 H -0.3088(11) -0.2473(11) -0.3061(10) 0.071 Uiso 1 calc R . C24 C -0.1002(11) -0.1716(10) -0.3791(10) 0.047(2) Uani 1 d . . H24 H -0.1135(11) -0.0834(10) -0.3920(10) 0.061 Uiso 1 calc R . C31 C 0.1851(10) -0.1779(10) -0.4724(8) 0.047(2) Uani 1 d DU . C32 C 0.1941(12) -0.0622(12) -0.5203(10) 0.060(2) Uani 1 d DU . H32 H 0.1138(12) -0.0089(12) -0.5052(10) 0.077 Uiso 1 calc R . C33 C 0.3096(13) -0.0180(16) -0.5878(11) 0.080(4) Uani 1 d DU . H33 H 0.3102(13) 0.0640(16) -0.6206(11) 0.104 Uiso 1 calc R . C34 C 0.4245(14) -0.0913(17) -0.6085(13) 0.088(5) Uani 1 d DU . H34 H 0.5114(14) -0.0605(17) -0.6527(13) 0.114 Uiso 1 calc R . C35 C 0.4140(23) -0.2078(22) -0.5657(18) 0.099(6) Uani 1 d DU . H35 H 0.4884(23) -0.2642(22) -0.5890(18) 0.128 Uiso 1 calc R . C36 C 0.3051(16) -0.2512(18) -0.4918(14) 0.080(4) Uani 1 d DU . H36 H 0.3108(16) -0.3299(18) -0.4541(14) 0.104 Uiso 1 calc R . B B 0.0413(12) -0.2371(11) -0.4089(9) 0.045(2) Uani 1 d . . H H -0.0771(93) -0.0900(88) -0.1610(83) 0.024(19) Uiso 1 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 Pt 0.0280(2) 0.0331(10) 0.0268(9) -0.00040(11) 0.0060(6) 0.0058(7) Fe 0.0357(4) 0.030(2) 0.042(2) -0.0063(3) 0.0092(15) 0.0058(14) O1 0.046(3) 0.079(6) 0.049(4) 0.002(3) 0.018(3) -0.007(3) O2 0.063(4) 0.049(4) 0.061(4) 0.021(3) 0.018(3) 0.030(3) N 0.036(3) 0.021(3) 0.046(4) 0.003(3) 0.008(3) 0.004(2) C1 0.048(4) 0.052(6) 0.033(4) 0.001(4) 0.011(3) 0.012(4) C2 0.049(4) 0.039(5) 0.042(4) -0.004(3) 0.013(3) 0.011(4) C11 0.042(7) 0.039(6) 0.050(6) 0.009(5) 0.006(4) 0.017(5) C12 0.045(4) 0.041(5) 0.046(5) 0.010(4) 0.005(3) 0.016(4) C13 0.056(5) 0.023(4) 0.046(5) 0.002(3) 0.011(4) 0.003(3) C14 0.034(4) 0.031(4) 0.062(5) 0.005(4) 0.013(3) 0.003(3) C15 0.032(3) 0.029(4) 0.058(5) 0.010(3) 0.005(3) 0.010(3) C16 0.098(10) 0.046(7) 0.064(7) 0.026(6) 0.033(7) 0.015(7) C21 0.071(4) 0.021(7) 0.048(9) -0.011(3) 0.004(7) 0.019(6) C22 0.069(6) 0.042(5) 0.054(5) -0.014(4) 0.010(4) -0.004(4) C23 0.040(4) 0.057(6) 0.051(5) -0.005(4) 0.004(4) -0.004(4) C24 0.043(4) 0.045(5) 0.046(5) -0.006(4) 0.006(3) 0.014(4) C31 0.048(4) 0.055(6) 0.029(4) -0.011(3) 0.002(3) 0.013(4) C32 0.047(5) 0.069(7) 0.053(5) 0.008(5) 0.001(4) 0.007(4) C33 0.059(6) 0.105(10) 0.054(6) 0.013(6) -0.003(5) -0.008(6) C34 0.053(6) 0.139(13) 0.052(6) -0.005(7) 0.019(5) -0.004(7) C35 0.104(10) 0.140(16) 0.069(9) 0.007(10) 0.040(8) 0.065(11) C36 0.070(7) 0.116(11) 0.058(7) -0.007(7) 0.016(5) 0.058(7) B 0.046(5) 0.053(6) 0.033(4) -0.005(4) 0.006(3) 0.025(4) _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 Pt N 2.022(7) . ? Pt N 2.022(7) 2 ? Pt Fe 2.7735(11) 2 ? Pt Fe 2.7736(11) . ? Fe C1 1.713(10) . ? Fe C2 1.838(11) . ? Fe C24 2.044(11) . ? Fe C23 2.050(9) . ? Fe C21 2.082(7) . ? Fe C22 2.088(10) . ? Fe B 2.144(10) . ? O1 C1 1.168(12) . ? O2 C2 1.184(13) . ? N C15 1.353(10) . ? N C11 1.376(11) . ? C11 C12 1.366(13) . ? C12 C13 1.389(13) . ? C13 C14 1.373(14) . ? C13 C16 1.528(14) . ? C14 C15 1.374(12) . ? C21 C22 1.38(2) . ? C21 B 1.54(3) . ? C22 C23 1.42(2) . ? C23 C24 1.421(15) . ? C24 B 1.551(12) . ? C31 C32 1.385(15) . ? C31 C36 1.414(13) . ? C31 B 1.582(14) . ? C32 C33 1.38(2) . ? C33 C34 1.38(2) . ? C34 C35 1.36(2) . ? C35 C36 1.38(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 N Pt N 180.0 . 2 ? N Pt Fe 92.1(2) . 2 ? N Pt Fe 87.9(2) 2 2 ? N Pt Fe 87.9(2) . . ? N Pt Fe 92.1(2) 2 . ? Fe Pt Fe 180.0 2 . ? C1 Fe C2 95.2(5) . . ? C1 Fe C24 100.8(5) . . ? C2 Fe C24 155.5(4) . . ? C1 Fe C23 140.4(6) . . ? C2 Fe C23 124.0(5) . . ? C24 Fe C23 40.6(4) . . ? C1 Fe C21 115.1(5) . . ? C2 Fe C21 85.4(7) . . ? C24 Fe C21 71.0(7) . . ? C23 Fe C21 67.6(4) . . ? C1 Fe C22 153.0(4) . . ? C2 Fe C22 88.7(5) . . ? C24 Fe C22 68.8(5) . . ? C23 Fe C22 40.3(5) . . ? C21 Fe C22 38.5(5) . . ? C1 Fe B 86.4(4) . . ? C2 Fe B 120.3(4) . . ? C24 Fe B 43.4(3) . . ? C23 Fe B 69.9(4) . . ? C21 Fe B 42.8(8) . . ? C22 Fe B 68.8(4) . . ? C1 Fe Pt 73.8(3) . . ? C2 Fe Pt 96.0(3) . . ? C24 Fe Pt 106.2(3) . . ? C23 Fe Pt 104.4(3) . . ? C21 Fe Pt 170.9(3) . . ? C22 Fe Pt 132.4(3) . . ? B Fe Pt 140.2(4) . . ? C15 N C11 117.2(8) . . ? C15 N Pt 122.7(6) . . ? C11 N Pt 120.2(6) . . ? O1 C1 Fe 178.4(8) . . ? O2 C2 Fe 175.9(8) . . ? C12 C11 N 122.1(9) . . ? C11 C12 C13 120.5(8) . . ? C14 C13 C12 117.1(8) . . ? C14 C13 C16 122.8(10) . . ? C12 C13 C16 120.1(10) . . ? C13 C14 C15 121.3(7) . . ? N C15 C14 121.9(8) . . ? C22 C21 B 109.9(12) . . ? C22 C21 Fe 71.0(5) . . ? B C21 Fe 70.7(6) . . ? C21 C22 C23 110.4(13) . . ? C21 C22 Fe 70.5(5) . . ? C23 C22 Fe 68.5(5) . . ? C24 C23 C22 110.2(9) . . ? C24 C23 Fe 69.5(5) . . ? C22 C23 Fe 71.3(6) . . ? C23 C24 B 107.9(9) . . ? C23 C24 Fe 69.9(6) . . ? B C24 Fe 71.7(5) . . ? C32 C31 C36 117.3(11) . . ? C32 C31 B 123.6(8) . . ? C36 C31 B 118.9(11) . . ? C33 C32 C31 123.6(11) . . ? C32 C33 C34 118.8(14) . . ? C35 C34 C33 118.2(12) . . ? C34 C35 C36 124.2(14) . . ? C35 C36 C31 117.5(15) . . ? C21 B C24 101.4(8) . . ? C21 B C31 132.0(8) . . ? C24 B C31 126.5(9) . . ? C21 B Fe 66.4(6) . . ? C24 B Fe 64.9(5) . . ? C31 B Fe 130.1(6) . . ? _refine_diff_density_max 1.072 _refine_diff_density_min -0.962 _refine_diff_density_rms 0.118