#------------------------------------------------------------------------------ #$Date: 2021-09-06 14:11:24 +0300 (Mon, 06 Sep 2021) $ #$Revision: 268762 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/74/7707445.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7707445 loop_ _publ_author_name 'Szczepkowska, Anna M.' 'Janeta, Mateusz' 'Siczek, Mi\/losz' 'Tylus, W\/lodzimierz' 'Trzeciak, Anna M.' 'Bury, Wojciech' _publ_section_title ; Immobilization of Rh(I) precursor in a porphyrin metal-organic framework - turning on the catalytic activity. ; _journal_issue 26 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 9051 _journal_page_last 9058 _journal_paper_doi 10.1039/d1dt00518a _journal_volume 50 _journal_year 2021 _chemical_formula_moiety 'C97 H65 Cl N8 O38 Rh2 Zr6' _chemical_formula_sum 'C97 H53 Cl N8 O38 Rh2 Zr6' _chemical_formula_weight 2727.06 _space_group_crystal_system hexagonal _space_group_IT_number 191 _space_group_name_Hall '-P 6 2' _space_group_name_H-M_alt 'P 6/m m m' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2018/1 _audit_update_record ; 2021-04-13 deposited with the CCDC. 2021-05-04 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_formula_units_Z 3 _cell_length_a 42.262(8) _cell_length_b 42.262(8) _cell_length_c 16.951(2) _cell_measurement_reflns_used 17653 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 66.71 _cell_measurement_theta_min 2.08 _cell_volume 26220(8) _computing_cell_refinement 'CrysAlisPro 1.171.41.61a (Rigaku OD, 2020)' _computing_data_collection 'CrysAlisPro 1.171.41.61a (Rigaku OD, 2020)' _computing_data_reduction 'CrysAlisPro 1.171.41.61a (Rigaku OD, 2020)' _computing_structure_refinement 'SHELXL-2018/1 (Sheldrick, 2018)' _computing_structure_solution 'SHELXS(Sheldrick, 2018)' _diffrn_ambient_temperature 100(2) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_type 'HyPix-Arc 150' _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy R, DW system, HyPix-Arc 150' _diffrn_measurement_method /w _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.1078 _diffrn_reflns_av_unetI/netI 0.0498 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 50 _diffrn_reflns_limit_h_min -50 _diffrn_reflns_limit_k_max 50 _diffrn_reflns_limit_k_min -48 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 121519 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 67.159 _diffrn_reflns_theta_max 67.159 _diffrn_reflns_theta_min 2.414 _diffrn_source 'Rotating-anode X-ray tube' _diffrn_source_type 'Rigaku (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 2.452 _exptl_absorpt_correction_T_max 0.981 _exptl_absorpt_correction_T_min 0.795 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.41.61a (Rigaku Oxford Diffraction, 2020) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour PURPLE _exptl_crystal_density_diffrn 0.518 _exptl_crystal_description BLOCK _exptl_crystal_F_000 4026 _exptl_crystal_size_max 0.232 _exptl_crystal_size_mid 0.023 _exptl_crystal_size_min 0.022 _refine_diff_density_max 1.586 _refine_diff_density_min -3.044 _refine_diff_density_rms 0.202 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.165 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 200 _refine_ls_number_reflns 8665 _refine_ls_number_restraints 4 _refine_ls_restrained_S_all 1.165 _refine_ls_R_factor_all 0.1356 _refine_ls_R_factor_gt 0.0964 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2784 _refine_ls_wR_factor_ref 0.3173 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5711 _reflns_number_total 8665 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt00518a2.cif _cod_data_source_block aw523a _cod_depositor_comments 'Adding full bibliography for 7707445--7707447.cif.' _cod_original_cell_volume 26220(10) _cod_database_code 7707445 _shelx_shelxl_version_number 2018/1 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_res_file ; TITL aw523_cu_100k_a.res in P6/mmm aw523a.res created by SHELXL-2018/1 at 10:35:04 on 12-Apr-2021 CELL 1.54184 42.262 42.262 16.951 90 90 120 ZERR 3 0.008 0.008 0.002 0 0 0 LATT 1 SYMM -Y,+X-Y,+Z SYMM +Y-X,-X,+Z SYMM -X,-Y,+Z SYMM +Y,-X+Y,+Z SYMM -Y+X,+X,+Z SYMM +Y,+X,-Z SYMM -Y+X,-Y,-Z SYMM -X,-X+Y,-Z SYMM -Y,-X,-Z SYMM +Y-X,+Y,-Z SYMM +X,+X-Y,-Z SFAC C H Cl N O Rh Zr UNIT 291 159 3 24 114 6 18 DFIX 1.8 Rh1 C12 DFIX 1.2 C12 O12 DFIX 1.2 C11 O11 DFIX 1.8 Rh1 C11 EADP C11 Cl2 L.S. 20 PLAN 20 TEMP -173 CONF list 4 MORE -1 BOND $H fmap 2 acta OMIT -2 4 0 OMIT -1 7 2 OMIT -1 3 0 OMIT 0 0 2 OMIT -4 12 2 OMIT 0 1 2 OMIT -2 6 2 OMIT 0 9 0 OMIT -4 11 2 OMIT -3 9 0 OMIT 0 6 4 OMIT -1 2 5 OMIT -1 2 0 OMIT -1 5 1 WGHT 0.200000 FVAR 0.11075 ZR1 7 0.466316 0.533684 0.500000 10.25000 0.05008 0.05008 = 0.01976 0.00000 0.00000 0.03812 ZR2 7 0.541823 0.541823 0.603425 10.50000 0.05678 0.05678 = 0.02998 -0.01084 -0.01084 0.04207 RH1 6 0.500539 0.750270 1.000000 10.25000 0.18100 0.07677 = 0.04050 0.00000 0.00000 0.09050 PART 1 CL1 3 0.438151 0.719075 1.000000 10.06250 0.06946 C12 1 0.451681 0.725841 1.000000 10.06250 0.03951 PART 0 PART 2 CL2 3 0.561286 0.780643 1.000000 10.06250 0.07088 C11 1 0.549491 0.774746 1.000000 10.06250 0.07088 O11 5 0.581850 0.790925 1.000000 10.06250 0.13030 PART 0 N1 4 0.499353 0.701937 1.000000 10.50000 0.19242 0.06200 = 0.02504 0.00000 0.00000 0.09555 N2 4 0.500872 0.750436 0.880440 10.50000 0.16092 0.06382 = 0.02525 -0.00181 -0.00363 0.08046 C1 1 0.498832 0.682210 0.935353 11.00000 0.19989 0.07268 = 0.03462 -0.00862 -0.00864 0.10258 C2 1 0.497041 0.648661 0.960504 11.00000 0.30180 0.09542 = 0.04479 -0.01015 -0.01361 0.15067 AFIX 43 H2 2 0.496049 0.630099 0.927225 11.00000 -1.20000 AFIX 0 C5 1 0.501210 0.693466 0.856804 11.00000 0.17868 0.07828 = 0.03710 -0.00219 -0.00609 0.09642 C6 1 0.502963 0.725565 0.832458 11.00000 0.17223 0.06881 = 0.02727 -0.00494 -0.00445 0.08830 C7 1 0.506506 0.736994 0.752061 11.00000 0.18075 0.07525 = 0.03546 -0.00085 0.00395 0.08776 AFIX 43 H7 2 0.508478 0.724546 0.707328 11.00000 -1.20000 AFIX 0 C51 1 0.502633 0.668724 0.796187 11.00000 0.14930 0.07950 = 0.03103 -0.01434 -0.01166 0.08843 C52 1 0.474950 0.649953 0.744304 11.00000 0.13271 0.09043 = 0.06069 -0.00355 0.00849 0.08718 AFIX 43 H52 2 0.454189 0.653050 0.745843 11.00000 -1.20000 AFIX 0 C53 1 0.476216 0.626074 0.688415 11.00000 0.11528 0.08199 = 0.04430 -0.01763 -0.00917 0.07648 AFIX 43 H53 2 0.456554 0.613289 0.652576 11.00000 -1.20000 AFIX 0 C54 1 0.506328 0.621287 0.685897 11.00000 0.09565 0.06584 = 0.04131 -0.00772 -0.00096 0.05933 C55 1 0.534654 0.640178 0.738621 11.00000 0.10987 0.10258 = 0.07834 -0.04613 -0.03142 0.07833 AFIX 43 H55 2 0.555435 0.637099 0.738208 11.00000 -1.20000 AFIX 0 C56 1 0.532198 0.663614 0.791919 11.00000 0.17948 0.10441 = 0.05474 -0.04369 -0.05074 0.09435 AFIX 43 H56 2 0.551945 0.676828 0.827326 11.00000 -1.20000 AFIX 0 C57 1 0.506780 0.594228 0.632962 11.00000 0.07832 0.06025 = 0.04075 -0.01504 -0.00992 0.05339 O51 5 0.482895 0.580881 0.580007 11.00000 0.07211 0.05493 = 0.03558 -0.01082 -0.00718 0.04632 O52 5 0.531184 0.585719 0.646018 11.00000 0.09088 0.07837 = 0.05863 -0.03653 -0.02741 0.06593 O6 5 0.557371 0.524492 0.500000 10.50000 0.16261 0.09522 = 0.02931 0.00000 0.00000 0.10058 AFIX 13 H6 2 0.584565 0.535800 0.499998 10.50000 -1.20000 AFIX 0 O5 5 0.483800 0.516200 0.602761 10.50000 0.06783 0.06783 = 0.11622 0.03186 -0.03186 0.03548 AFIX 13 H5 2 0.475922 0.524078 0.650958 10.12500 -1.20000 AFIX 0 O4 5 0.538204 0.538204 0.734053 10.50000 0.14228 0.14228 = 0.03390 -0.02705 -0.02705 0.11388 O3 5 0.593985 0.593985 0.582052 10.50000 0.05920 0.05920 = 0.17232 -0.01469 -0.01469 0.03714 PART 1 O12 5 0.419488 0.709744 1.000000 10.06250 0.10479 PART 2 O1W 5 0.464275 0.535725 0.785041 10.25000 0.15592 0.15592 = 0.08966 -0.00282 0.00282 0.07436 PART 3 O3W 5 0.471065 0.528935 0.939617 10.25000 0.24611 PART 4 O2W 5 0.569285 0.664021 0.500000 10.12500 0.20346 HKLF 4 REM aw523_cu_100k_a.res in P6/mmm REM R1 = 0.0964 for 5711 Fo > 4sig(Fo) and 0.1356 for all 8665 data REM 200 parameters refined using 4 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 1.586, deepest hole -3.044, 1-sigma level 0.202 Q1 1 0.6065 0.6065 0.5000 10.25000 0.05 1.59 Q2 1 0.4906 0.5094 0.8152 10.50000 0.05 1.17 Q3 1 0.5483 0.6938 0.5000 10.50000 0.05 1.08 Q4 1 0.4768 0.5232 1.0000 10.25000 0.05 0.89 Q5 1 0.6432 0.6432 0.5000 10.25000 0.05 0.88 Q6 1 0.4109 0.6082 0.5000 10.50000 0.05 0.84 Q7 1 0.6002 0.6415 0.5000 10.50000 0.05 0.81 Q8 1 0.4947 0.7252 0.5000 10.50000 0.05 0.79 Q9 1 0.3805 0.7610 1.0000 10.25000 0.05 0.79 Q10 1 0.4802 0.5198 0.9390 10.50000 0.05 0.78 Q11 1 0.4978 0.7068 0.5000 10.50000 0.05 0.76 Q12 1 0.4834 0.6970 0.5000 10.50000 0.05 0.76 Q13 1 0.5272 0.7112 0.5000 10.50000 0.05 0.74 Q14 1 0.3840 0.6304 0.8821 11.00000 0.05 0.73 Q15 1 0.4324 0.4843 0.8731 11.00000 0.05 0.73 Q16 1 0.4448 0.5552 0.8486 10.50000 0.05 0.73 Q17 1 0.3796 0.7592 0.9561 10.50000 0.05 0.71 Q18 1 0.4345 0.6516 0.5000 10.50000 0.05 0.71 Q19 1 0.3862 0.6463 0.8530 11.00000 0.05 0.67 Q20 1 0.3751 0.6249 0.8079 10.50000 0.05 0.67 ; _shelx_res_checksum 3151 loop_ _space_group_symop_operation_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z' 'y, -x+y, z' 'x-y, x, z' 'y, x, -z' 'x-y, -y, -z' '-x, -x+y, -z' '-y, -x, -z' '-x+y, y, -z' 'x, x-y, -z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z' '-y, x-y, -z' '-x+y, -x, -z' '-y, -x, z' '-x+y, y, z' 'x, x-y, z' 'y, x, z' 'x-y, -y, z' '-x, -x+y, z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.46632(2) 0.53368(2) 0.500000 0.0342(3) Uani 1 4 d S T P . . Zr2 Zr 0.54182(2) 0.54182(2) 0.60343(4) 0.0418(3) Uani 1 2 d S T P . . Rh1 Rh 0.50054(6) 0.75027(3) 1.000000 0.0878(6) Uani 1 4 d DS T P . . Cl1 Cl 0.4382(7) 0.7191(3) 1.000000 0.069(4) Uiso 0.25 4 d S . P A 1 C12 C 0.4517(5) 0.7258(3) 1.000000 0.040(14) Uiso 0.25 4 d DS . P A 1 Cl2 Cl 0.5613(5) 0.7806(3) 1.000000 0.071(4) Uiso 0.25 4 d S . P A 2 C11 C 0.5495(5) 0.7747(3) 1.000000 0.071(4) Uiso 0.25 4 d DS . P A 2 O11 O 0.5819(7) 0.7909(4) 1.000000 0.13(2) Uiso 0.25 4 d DS . P A 2 N1 N 0.4994(3) 0.7019(2) 1.000000 0.079(3) Uani 1 2 d S T P A . N2 N 0.5009(3) 0.75044(17) 0.8804(4) 0.073(3) Uani 1 2 d S T P A . C1 C 0.4988(3) 0.6822(2) 0.9354(4) 0.087(3) Uani 1 1 d . . . . . C2 C 0.4970(4) 0.6487(3) 0.9605(5) 0.125(5) Uani 1 1 d . . . . . H2 H 0.496049 0.630099 0.927225 0.149 Uiso 1 1 calc R U . . . C5 C 0.5012(3) 0.6935(2) 0.8568(4) 0.084(3) Uani 1 1 d . . . . . C6 C 0.5030(3) 0.7256(2) 0.8325(4) 0.077(3) Uani 1 1 d . . . . . C7 C 0.5065(3) 0.7370(2) 0.7521(4) 0.087(3) Uani 1 1 d . . . . . H7 H 0.508478 0.724546 0.707328 0.104 Uiso 1 1 calc R U . . . C51 C 0.5026(3) 0.6687(2) 0.7962(4) 0.073(3) Uani 1 1 d . . . . . C52 C 0.4750(3) 0.6500(3) 0.7443(5) 0.081(3) Uani 1 1 d . . . . . H52 H 0.454189 0.653050 0.745843 0.097 Uiso 1 1 calc R U . . . C53 C 0.4762(3) 0.6261(2) 0.6884(4) 0.068(2) Uani 1 1 d . . . . . H53 H 0.456554 0.613289 0.652576 0.082 Uiso 1 1 calc R U . . . C54 C 0.5063(2) 0.6213(2) 0.6859(4) 0.059(2) Uani 1 1 d . . . . . C55 C 0.5347(3) 0.6402(3) 0.7386(5) 0.086(3) Uani 1 1 d . . . . . H55 H 0.555435 0.637099 0.738208 0.103 Uiso 1 1 calc R U . . . C56 C 0.5322(3) 0.6636(3) 0.7919(5) 0.102(4) Uani 1 1 d . . . . . H56 H 0.551945 0.676828 0.827326 0.123 Uiso 1 1 calc R U . . . C57 C 0.5068(2) 0.5942(2) 0.6330(4) 0.0514(18) Uani 1 1 d . . . . . O51 O 0.48290(13) 0.58088(12) 0.5800(2) 0.0477(11) Uani 1 1 d . . . . . O52 O 0.53118(16) 0.58572(15) 0.6460(3) 0.0655(15) Uani 1 1 d . . . . . O6 O 0.5574(3) 0.5245(2) 0.500000 0.080(3) Uani 1 2 d S T P . . H6 H 0.584565 0.535800 0.499998 0.096 Uiso 1 2 calc R U P . . O5 O 0.48380(11) 0.51620(11) 0.6028(6) 0.083(3) Uani 1 2 d S T P . . H5 H 0.475922 0.524078 0.650958 0.100 Uiso 0.25 2 calc R U P . . O4 O 0.5382(3) 0.5382(3) 0.7341(4) 0.087(3) Uani 1 2 d S T P . . O3 O 0.5940(2) 0.5940(2) 0.5821(6) 0.094(3) Uani 1 2 d S T P . . O12 O 0.4195(7) 0.7097(4) 1.000000 0.10(2) Uiso 0.25 4 d DS . P A 1 O1W O 0.4643(4) 0.5357(4) 0.7850(14) 0.135(9) Uani 0.5 2 d S T P B 2 O3W O 0.4711(6) 0.5289(6) 0.940(3) 0.246(19) Uiso 0.5 2 d S . P C 3 O2W O 0.569(2) 0.6640(19) 0.500000 0.20(3) Uiso 0.25 2 d S . P D 4 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 Zr1 0.0501(5) 0.0501(5) 0.0198(5) 0.000 0.000 0.0381(5) Zr2 0.0568(4) 0.0568(4) 0.0300(4) -0.0108(3) -0.0108(3) 0.0421(4) Rh1 0.1810(18) 0.0768(6) 0.0405(7) 0.000 0.000 0.0905(9) N1 0.192(12) 0.062(6) 0.025(4) 0.000 0.000 0.096(7) N2 0.161(10) 0.064(4) 0.025(4) -0.002(3) -0.004(5) 0.080(5) C1 0.200(11) 0.073(5) 0.035(4) -0.009(4) -0.009(5) 0.103(7) C2 0.302(17) 0.095(7) 0.045(4) -0.010(5) -0.014(7) 0.151(10) C5 0.179(10) 0.078(6) 0.037(4) -0.002(4) -0.006(5) 0.096(7) C6 0.172(10) 0.069(5) 0.027(3) -0.005(3) -0.004(5) 0.088(6) C7 0.181(10) 0.075(6) 0.035(4) -0.001(4) 0.004(5) 0.088(7) C51 0.149(9) 0.080(6) 0.031(4) -0.014(4) -0.012(5) 0.088(6) C52 0.133(8) 0.090(6) 0.061(5) -0.004(5) 0.008(5) 0.087(7) C53 0.115(7) 0.082(6) 0.044(4) -0.018(4) -0.009(4) 0.076(6) C54 0.096(6) 0.066(5) 0.041(4) -0.008(3) -0.001(4) 0.059(5) C55 0.110(8) 0.103(7) 0.078(6) -0.046(6) -0.031(6) 0.078(7) C56 0.179(12) 0.104(8) 0.055(5) -0.044(5) -0.051(6) 0.094(8) C57 0.078(5) 0.060(4) 0.041(4) -0.015(3) -0.010(4) 0.053(4) O51 0.072(3) 0.055(3) 0.036(2) -0.011(2) -0.007(2) 0.046(3) O52 0.091(4) 0.078(4) 0.059(3) -0.037(3) -0.027(3) 0.066(3) O6 0.163(9) 0.095(6) 0.029(3) 0.000 0.000 0.101(7) O5 0.068(4) 0.068(4) 0.116(7) 0.032(3) -0.032(3) 0.035(4) O4 0.142(7) 0.142(7) 0.034(4) -0.027(4) -0.027(4) 0.114(7) O3 0.059(4) 0.059(4) 0.172(9) -0.015(5) -0.015(5) 0.037(4) O1W 0.156(16) 0.156(16) 0.090(15) -0.003(8) 0.003(8) 0.074(18) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh 0.0927 3.6045 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -0.1862 2.2449 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 O6 Zr1 O6 107.8(5) 7_556 13_666 ? O6 Zr1 O5 69.57(19) 7_556 . ? O6 Zr1 O5 69.57(19) 13_666 . ? O6 Zr1 O5 69.57(19) 7_556 16_556 ? O6 Zr1 O5 69.57(19) 13_666 16_556 ? O5 Zr1 O5 107.4(5) . 16_556 ? O6 Zr1 O51 142.12(12) 7_556 10_666 ? O6 Zr1 O51 78.9(2) 13_666 10_666 ? O5 Zr1 O51 142.42(13) . 10_666 ? O5 Zr1 O51 78.8(2) 16_556 10_666 ? O6 Zr1 O51 142.12(12) 7_556 19_665 ? O6 Zr1 O51 78.9(2) 13_666 19_665 ? O5 Zr1 O51 78.8(2) . 19_665 ? O5 Zr1 O51 142.42(13) 16_556 19_665 ? O51 Zr1 O51 75.5(2) 10_666 19_665 ? O6 Zr1 O51 78.9(2) 7_556 16_556 ? O6 Zr1 O51 142.12(12) 13_666 16_556 ? O5 Zr1 O51 142.42(13) . 16_556 ? O5 Zr1 O51 78.8(2) 16_556 16_556 ? O51 Zr1 O51 74.9(3) 10_666 16_556 ? O51 Zr1 O51 119.3(2) 19_665 16_556 ? O6 Zr1 O51 78.9(2) 7_556 . ? O6 Zr1 O51 142.12(12) 13_666 . ? O5 Zr1 O51 78.8(2) . . ? O5 Zr1 O51 142.43(13) 16_556 . ? O51 Zr1 O51 119.3(2) 10_666 . ? O51 Zr1 O51 74.9(3) 19_665 . ? O51 Zr1 O51 75.5(2) 16_556 . ? O6 Zr1 Zr2 89.6(2) 7_556 13_666 ? O6 Zr1 Zr2 34.69(13) 13_666 13_666 ? O5 Zr1 Zr2 89.2(2) . 13_666 ? O5 Zr1 Zr2 34.92(13) 16_556 13_666 ? O51 Zr1 Zr2 75.10(11) 10_666 13_666 ? O51 Zr1 Zr2 110.81(13) 19_665 13_666 ? O51 Zr1 Zr2 110.88(11) 16_556 13_666 ? O51 Zr1 Zr2 165.65(12) . 13_666 ? O6 Zr1 Zr2 89.6(2) 7_556 4_665 ? O6 Zr1 Zr2 34.69(13) 13_666 4_665 ? O5 Zr1 Zr2 34.93(13) . 4_665 ? O5 Zr1 Zr2 89.2(2) 16_556 4_665 ? O51 Zr1 Zr2 110.81(13) 10_666 4_665 ? O51 Zr1 Zr2 75.10(11) 19_665 4_665 ? O51 Zr1 Zr2 165.64(12) 16_556 4_665 ? O51 Zr1 Zr2 110.88(11) . 4_665 ? Zr2 Zr1 Zr2 60.05(3) 13_666 4_665 ? O6 Zr1 Zr2 34.69(13) 7_556 16_556 ? O6 Zr1 Zr2 89.6(2) 13_666 16_556 ? O5 Zr1 Zr2 89.2(2) . 16_556 ? O5 Zr1 Zr2 34.92(13) 16_556 16_556 ? O51 Zr1 Zr2 110.88(11) 10_666 16_556 ? O51 Zr1 Zr2 165.64(12) 19_665 16_556 ? O51 Zr1 Zr2 75.10(11) 16_556 16_556 ? O51 Zr1 Zr2 110.81(13) . 16_556 ? Zr2 Zr1 Zr2 60.59(3) 13_666 16_556 ? Zr2 Zr1 Zr2 90.55(3) 4_665 16_556 ? O6 Zr1 Zr2 34.69(13) 7_556 . ? O6 Zr1 Zr2 89.6(2) 13_666 . ? O5 Zr1 Zr2 34.93(13) . . ? O5 Zr1 Zr2 89.2(2) 16_556 . ? O51 Zr1 Zr2 165.65(12) 10_666 . ? O51 Zr1 Zr2 110.88(11) 19_665 . ? O51 Zr1 Zr2 110.81(13) 16_556 . ? O51 Zr1 Zr2 75.10(11) . . ? Zr2 Zr1 Zr2 90.55(3) 13_666 . ? Zr2 Zr1 Zr2 60.59(3) 4_665 . ? Zr2 Zr1 Zr2 60.05(3) 16_556 . ? O6 Zr2 O6 68.9(3) . 7_556 ? O6 Zr2 O5 70.5(3) . 4_665 ? O6 Zr2 O5 107.2(4) 7_556 4_665 ? O6 Zr2 O5 107.2(4) . . ? O6 Zr2 O5 70.5(3) 7_556 . ? O5 Zr2 O5 67.7(4) 4_665 . ? O6 Zr2 O4 145.20(16) . . ? O6 Zr2 O4 145.20(16) 7_556 . ? O5 Zr2 O4 87.0(3) 4_665 . ? O5 Zr2 O4 87.0(3) . . ? O6 Zr2 O3 83.3(4) . . ? O6 Zr2 O3 83.3(4) 7_556 . ? O5 Zr2 O3 144.95(17) 4_665 . ? O5 Zr2 O3 144.94(16) . . ? O4 Zr2 O3 103.3(4) . . ? O6 Zr2 O52 141.0(2) . . ? O6 Zr2 O52 76.5(2) 7_556 . ? O5 Zr2 O52 139.5(2) 4_665 . ? O5 Zr2 O52 76.4(3) . . ? O4 Zr2 O52 72.51(17) . . ? O3 Zr2 O52 75.1(2) . . ? O6 Zr2 O52 76.5(2) . 22 ? O6 Zr2 O52 141.0(2) 7_556 22 ? O5 Zr2 O52 76.4(3) 4_665 22 ? O5 Zr2 O52 139.5(2) . 22 ? O4 Zr2 O52 72.51(17) . 22 ? O3 Zr2 O52 75.1(2) . 22 ? O52 Zr2 O52 126.4(3) . 22 ? O6 Zr2 Zr1 35.0(2) . 13_666 ? O6 Zr2 Zr1 88.7(2) 7_556 13_666 ? O5 Zr2 Zr1 35.6(2) 4_665 13_666 ? O5 Zr2 Zr1 88.3(2) . 13_666 ? O4 Zr2 Zr1 117.67(17) . 13_666 ? O3 Zr2 Zr1 114.62(18) . 13_666 ? O52 Zr2 Zr1 161.50(13) . 13_666 ? O52 Zr2 Zr1 72.06(13) 22 13_666 ? O6 Zr2 Zr1 88.7(2) . . ? O6 Zr2 Zr1 35.0(2) 7_556 . ? O5 Zr2 Zr1 88.3(2) 4_665 . ? O5 Zr2 Zr1 35.6(2) . . ? O4 Zr2 Zr1 117.67(17) . . ? O3 Zr2 Zr1 114.62(18) . . ? O52 Zr2 Zr1 72.06(13) . . ? O52 Zr2 Zr1 161.50(13) 22 . ? Zr1 Zr2 Zr1 89.44(3) 13_666 . ? O6 Zr2 Zr2 34.48(17) . 16_556 ? O6 Zr2 Zr2 34.48(17) 7_556 16_556 ? O5 Zr2 Zr2 89.7(3) 4_665 16_556 ? O5 Zr2 Zr2 89.7(3) . 16_556 ? O4 Zr2 Zr2 176.0(3) . 16_556 ? O3 Zr2 Zr2 80.7(3) . 16_556 ? O52 Zr2 Zr2 108.84(13) . 16_556 ? O52 Zr2 Zr2 108.84(13) 22 16_556 ? Zr1 Zr2 Zr2 59.974(14) 13_666 16_556 ? Zr1 Zr2 Zr2 59.976(14) . 16_556 ? O6 Zr2 Zr2 89.0(3) . 4_665 ? O6 Zr2 Zr2 89.0(3) 7_556 4_665 ? O5 Zr2 Zr2 33.85(17) 4_665 4_665 ? O5 Zr2 Zr2 33.86(17) . 4_665 ? O4 Zr2 Zr2 86.0(3) . 4_665 ? O3 Zr2 Zr2 170.7(3) . 4_665 ? O52 Zr2 Zr2 108.32(16) . 4_665 ? O52 Zr2 Zr2 108.32(16) 22 4_665 ? Zr1 Zr2 Zr2 59.704(15) 13_666 4_665 ? Zr1 Zr2 Zr2 59.706(15) . 4_665 ? Zr2 Zr2 Zr2 90.0 16_556 4_665 ? C12 Rh1 N1 88.8(4) . 21_565 ? C12 Rh1 N1 88.8(4) . . ? C11 Rh1 N1 91.2(4) . . ? N1 Rh1 N1 177.5(7) 21_565 . ? C12 Rh1 N2 90.3(4) . 16_557 ? N1 Rh1 N2 90.005(8) 21_565 16_557 ? N1 Rh1 N2 90.010(7) . 16_557 ? C12 Rh1 N2 90.3(4) . . ? C11 Rh1 N2 89.7(4) . . ? N1 Rh1 N2 90.007(8) 21_565 . ? N1 Rh1 N2 90.007(7) . . ? N2 Rh1 N2 179.3(8) 16_557 . ? C11 Rh1 Cl2 0.0(6) . . ? N1 Rh1 Cl2 91.2(4) 21_565 . ? N1 Rh1 Cl2 91.2(4) . . ? N2 Rh1 Cl2 89.7(3) 16_557 . ? N2 Rh1 Cl2 89.7(4) . . ? C12 Rh1 Cl1 0.0(7) . . ? N1 Rh1 Cl1 88.8(4) 21_565 . ? N1 Rh1 Cl1 88.8(4) . . ? N2 Rh1 Cl1 90.3(4) 16_557 . ? N2 Rh1 Cl1 90.3(4) . . ? O12 Cl1 Rh1 180(4) . . ? O12 C12 Rh1 180.0(13) . . ? O11 Cl2 Rh1 180(2) . . ? O11 C11 Rh1 180.0(18) . . ? Cl2 O11 C11 0.0(17) . . ? C1 N1 C1 106.2(8) 16_557 . ? C1 N1 Rh1 126.9(4) 16_557 . ? C1 N1 Rh1 126.9(4) . . ? C6 N2 C6 106.6(8) 21_565 . ? C6 N2 Rh1 126.6(4) 21_565 . ? C6 N2 Rh1 126.6(4) . . ? N1 C1 C5 125.2(7) . . ? N1 C1 C2 109.7(6) . . ? C5 C1 C2 125.0(7) . . ? C2 C2 C1 107.2(4) 16_557 . ? C2 C2 H2 126.4 16_557 . ? C1 C2 H2 126.4 . . ? C6 C5 C1 125.2(7) . . ? C6 C5 C51 118.8(7) . . ? C1 C5 C51 116.0(7) . . ? N2 C6 C5 125.7(7) . . ? N2 C6 C7 110.1(6) . . ? C5 C6 C7 124.1(7) . . ? C7 C7 C6 106.6(4) 21_565 . ? C7 C7 H7 126.7 21_565 . ? C6 C7 H7 126.7 . . ? C52 C51 C56 117.4(7) . . ? C52 C51 C5 122.1(9) . . ? C56 C51 C5 120.4(9) . . ? C51 C52 C53 121.7(8) . . ? C51 C52 H52 119.2 . . ? C53 C52 H52 119.1 . . ? C54 C53 C52 119.6(8) . . ? C54 C53 H53 120.2 . . ? C52 C53 H53 120.2 . . ? C55 C54 C53 119.3(7) . . ? C55 C54 C57 120.1(7) . . ? C53 C54 C57 120.4(7) . . ? C56 C55 C54 118.8(9) . . ? C56 C55 H55 120.6 . . ? C54 C55 H55 120.6 . . ? C51 C56 C55 123.2(9) . . ? C51 C56 H56 118.4 . . ? C55 C56 H56 118.4 . . ? O51 C57 O52 125.6(6) . . ? O51 C57 C54 118.0(6) . . ? O52 C57 C54 116.4(6) . . ? C57 O51 Zr1 131.6(4) . . ? C57 O52 Zr2 135.0(4) . . ? Zr2 O6 Zr2 111.0(3) . 16_556 ? Zr2 O6 Zr1 110.4(3) . 13_666 ? Zr2 O6 Zr1 110.3(3) 16_556 13_666 ? Zr2 O6 H6 108.3 . . ? Zr2 O6 H6 108.3 16_556 . ? Zr1 O6 H6 108.3 13_666 . ? Zr2 O5 Zr2 112.3(4) 4_665 . ? Zr2 O5 Zr1 109.5(3) 4_665 . ? Zr2 O5 Zr1 109.5(3) . . ? Zr2 O5 H5 108.5 4_665 . ? Zr2 O5 H5 108.5 . . ? Zr1 O5 H5 108.5 . . ? Cl1 O12 C12 0.0(11) . . ? 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 Zr1 O6 2.141(8) 7_556 ? Zr1 O6 2.141(8) 13_666 ? Zr1 O5 2.162(7) . ? Zr1 O5 2.162(7) 16_556 ? Zr1 O51 2.216(4) 10_666 ? Zr1 O51 2.216(4) 19_665 ? Zr1 O51 2.216(4) 16_556 ? Zr1 O51 2.216(4) . ? Zr1 Zr2 3.5038(10) 13_666 ? Zr1 Zr2 3.5038(10) 4_665 ? Zr1 Zr2 3.5038(10) 16_556 ? Zr1 Zr2 3.5039(10) . ? Zr2 O6 2.127(4) . ? Zr2 O6 2.127(4) 7_556 ? Zr2 O5 2.128(4) 4_665 ? Zr2 O5 2.129(4) . ? Zr2 O4 2.220(8) . ? Zr2 O3 2.234(9) . ? Zr2 O52 2.236(4) . ? Zr2 O52 2.236(4) 22 ? Zr2 Zr2 3.5064(15) 16_556 ? Zr2 Zr2 3.5349(18) 4_665 ? Rh1 C12 1.788(19) . ? Rh1 C11 1.792(19) . ? Rh1 N1 2.018(7) 21_565 ? Rh1 N1 2.018(7) . ? Rh1 N2 2.027(7) 16_557 ? Rh1 N2 2.027(7) . ? Rh1 Cl2 2.22(2) . ? Rh1 Cl1 2.28(3) . ? Cl1 O12 0.68(3) . ? C12 O12 1.18(2) . ? Cl2 O11 0.75(3) . ? C11 O11 1.18(2) . ? N1 C1 1.370(8) 16_557 ? N1 C1 1.370(8) . ? N2 C6 1.366(8) 21_565 ? N2 C6 1.366(8) . ? C1 C5 1.401(10) . ? C1 C2 1.446(10) . ? C2 C2 1.339(16) 16_557 ? C2 H2 0.9500 . ? C5 C6 1.384(10) . ? C5 C51 1.489(10) . ? C6 C7 1.429(10) . ? C7 C7 1.374(15) 21_565 ? C7 H7 0.9500 . ? C51 C52 1.358(12) . ? C51 C56 1.372(13) . ? C52 C53 1.405(10) . ? C52 H52 0.9500 . ? C53 C54 1.386(11) . ? C53 H53 0.9500 . ? C54 C55 1.383(11) . ? C54 C57 1.461(9) . ? C55 C56 1.382(11) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C57 O51 1.254(8) . ? C57 O52 1.270(8) . ? O6 H6 1.0000 . ? O5 H5 1.0000 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 N1 C1 C5 -176.1(7) 16_557 . . . ? Rh1 N1 C1 C5 4(2) . . . . ? C1 N1 C1 C2 1.4(18) 16_557 . . . ? Rh1 N1 C1 C2 -178.5(9) . . . . ? N1 C1 C2 C2 -0.9(11) . . . 16_557 ? C5 C1 C2 C2 176.7(10) . . . 16_557 ? N1 C1 C5 C6 -3(2) . . . . ? C2 C1 C5 C6 -179.9(13) . . . . ? N1 C1 C5 C51 176.0(12) . . . . ? C2 C1 C5 C51 -1.2(18) . . . . ? C6 N2 C6 C5 -178.7(7) 21_565 . . . ? Rh1 N2 C6 C5 7.6(19) . . . . ? C6 N2 C6 C7 0.1(17) 21_565 . . . ? Rh1 N2 C6 C7 -173.7(9) . . . . ? C1 C5 C6 N2 -3(2) . . . . ? C51 C5 C6 N2 177.9(11) . . . . ? C1 C5 C6 C7 178.0(12) . . . . ? C51 C5 C6 C7 -0.7(18) . . . . ? N2 C6 C7 C7 0.0(10) . . . 21_565 ? C5 C6 C7 C7 178.8(10) . . . 21_565 ? C6 C5 C51 C52 -68.8(14) . . . . ? C1 C5 C51 C52 112.4(11) . . . . ? C6 C5 C51 C56 112.4(12) . . . . ? C1 C5 C51 C56 -66.5(14) . . . . ? C56 C51 C52 C53 0.2(14) . . . . ? C5 C51 C52 C53 -178.6(8) . . . . ? C51 C52 C53 C54 0.2(14) . . . . ? C52 C53 C54 C55 0.0(13) . . . . ? C52 C53 C54 C57 174.6(8) . . . . ? C53 C54 C55 C56 -0.6(15) . . . . ? C57 C54 C55 C56 -175.3(9) . . . . ? C52 C51 C56 C55 -0.9(16) . . . . ? C5 C51 C56 C55 178.0(10) . . . . ? C54 C55 C56 C51 1.1(17) . . . . ? C55 C54 C57 O51 -171.8(8) . . . . ? C53 C54 C57 O51 13.6(12) . . . . ? C55 C54 C57 O52 9.6(12) . . . . ? C53 C54 C57 O52 -165.0(8) . . . . ? O52 C57 O51 Zr1 10.1(12) . . . . ? C54 C57 O51 Zr1 -168.4(5) . . . . ? O51 C57 O52 Zr2 -10.2(13) . . . . ? C54 C57 O52 Zr2 168.2(5) . . . . ?