#------------------------------------------------------------------------------ #$Date: 2021-01-05 04:00:57 +0200 (Tue, 05 Jan 2021) $ #$Revision: 260500 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/77/7127773.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_7127773 loop_ _publ_author_name 'Yang, Xin' 'wei, rui' 'Shi, Yaping' 'Liu, Liu Leo' 'Wu, Yile' 'Zhao, Yufen' 'Stephan, Douglas W.' _publ_section_title ; Oxyphosphoranes as precursors to bridging phosphate-catecholate ligands ; _journal_name_full 'Chemical Communications' _journal_paper_doi 10.1039/D0CC07736D _journal_year 2021 _chemical_formula_moiety 'C12 H13 Cl6 O6 P Zr' _chemical_formula_sum 'C12 H13 Cl6 O6 P Zr' _chemical_formula_weight 588.11 _chemical_properties_physical Moisture-sensitive _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2020-09-03 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2020-11-01 deposited with the CCDC. 2021-01-04 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 99.301(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.6112(5) _cell_length_b 11.6372(6) _cell_length_c 18.1370(10) _cell_measurement_reflns_used 9953 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 71.99 _cell_measurement_theta_min 4.53 _cell_volume 2001.91(18) _computing_cell_refinement 'SAINT V8.40B (?, 2016)' _computing_data_reduction 'SAINT V8.40B (?, 2016)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'XT (Sheldrick, 2015)' _diffrn_ambient_temperature 100.0 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0704 _diffrn_reflns_av_unetI/netI 0.0267 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 49347 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 72.443 _diffrn_reflns_theta_min 4.532 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 12.894 _exptl_absorpt_correction_T_max 0.7536 _exptl_absorpt_correction_T_min 0.4941 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1419 before and 0.0906 after correction. The Ratio of minimum to maximum transmission is 0.6557. The \l/2 correction factor is Not present. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.951 _exptl_crystal_description plate _exptl_crystal_F_000 1160 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: thf' _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.03 _refine_diff_density_max 1.329 _refine_diff_density_min -0.401 _refine_diff_density_rms 0.108 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 236 _refine_ls_number_reflns 3948 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.073 _refine_ls_R_factor_all 0.0306 _refine_ls_R_factor_gt 0.0291 _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^)+(0.0463P)^2^+1.9516P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0777 _refine_ls_wR_factor_ref 0.0787 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3732 _reflns_number_total 3948 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0cc07736d2.cif _cod_data_source_block 1_CCDC1 _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was changed to 'multi-scan' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas ; _cod_database_code 7127773 _shelx_shelxl_version_number 2018/3 _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_estimated_absorpt_t_max 0.698 _shelx_estimated_absorpt_t_min 0.359 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Secondary CH2 refined with riding coordinates: C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C7(H7A,H7B), C12(H12A,H12B) 2.b Idealised Me refined as rotating group: C8(H8A,H8B,H8C) ; _shelx_res_file ; TITL 1_a.res in P2(1)/c 1.res created by SHELXL-2018/3 at 13:20:33 on 03-Sep-2020 REM Old TITL 1_a.res in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.078, Rweak 0.003, Alpha 0.025 REM 0.543 for 212 systematic absences, Orientation as input REM Formula found by SHELXT: C12 O6 P Cl6 Zr CELL 1.54178 9.6112 11.6372 18.137 90 99.301 90 ZERR 4 0.0005 0.0006 0.001 0 0.002 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Cl O P Zr UNIT 48 52 24 24 4 4 L.S. 4 PLAN -4 0 0 SIZE 0.03 0.09 0.1 TEMP -173.15 BOND list 4 fmap 2 acta REM REM REM WGHT 0.046300 1.951600 FVAR 0.31729 ZR1 6 0.653201 0.402530 0.614578 11.00000 0.01783 0.01400 = 0.01622 -0.00155 0.00069 -0.00048 CL3 3 0.664379 0.124942 0.440180 11.00000 0.03076 0.02257 = 0.02385 -0.00364 0.00433 0.00433 CL1 3 0.576573 0.302731 0.718757 11.00000 0.03114 0.02390 = 0.02232 0.00061 0.00616 -0.00563 CL2 3 0.890949 0.331055 0.641277 11.00000 0.02169 0.02651 = 0.03311 0.00094 0.00203 0.00584 P1 5 0.315517 0.462436 0.551133 11.00000 0.01839 0.01737 = 0.01806 -0.00242 0.00299 0.00029 CL4 3 0.420626 -0.031786 0.355918 11.00000 0.04993 0.01816 = 0.02468 -0.00694 -0.00452 0.00189 CL6 3 0.045802 0.201533 0.492370 11.00000 0.02339 0.04095 = 0.02985 0.00244 0.00124 -0.00850 CL5 3 0.112008 0.005985 0.382965 11.00000 0.04112 0.03182 = 0.03579 -0.00429 -0.00858 -0.01663 O5 4 0.566544 0.291133 0.540148 11.00000 0.02272 0.01588 = 0.01904 -0.00358 0.00231 -0.00263 O6 4 0.711952 0.545068 0.693038 11.00000 0.02514 0.01539 = 0.01756 -0.00110 -0.00353 0.00009 O3 4 0.292088 0.485958 0.468450 11.00000 0.02187 0.01838 = 0.01945 -0.00068 0.00152 -0.00108 O1 4 0.458477 0.494571 0.593464 11.00000 0.01939 0.01851 = 0.02310 -0.00317 0.00073 0.00209 O2 4 0.290958 0.327934 0.562643 11.00000 0.02568 0.02023 = 0.01853 -0.00042 0.00590 -0.00229 O4 4 0.196999 0.522090 0.585276 11.00000 0.02395 0.03090 = 0.02452 -0.00445 0.00583 0.00480 C1 1 0.323545 0.244869 0.513560 11.00000 0.02631 0.01443 = 0.01673 0.00195 0.00182 -0.00238 C3 1 0.492148 0.142237 0.453557 11.00000 0.02995 0.01413 = 0.01842 0.00089 0.00108 0.00083 C2 1 0.463400 0.227519 0.503421 11.00000 0.02494 0.01271 = 0.01663 0.00126 -0.00084 -0.00191 C4 1 0.383449 0.074182 0.415648 11.00000 0.03887 0.01471 = 0.01664 0.00028 -0.00312 -0.00025 C6 1 0.215133 0.177144 0.476531 11.00000 0.02643 0.02313 = 0.01959 0.00585 -0.00095 -0.00452 C9 1 0.667785 0.665511 0.680461 11.00000 0.02977 0.01691 = 0.02277 -0.00327 0.00038 0.00240 AFIX 23 H9A 2 0.567182 0.675034 0.685045 11.00000 -1.20000 H9B 2 0.681791 0.691486 0.630201 11.00000 -1.20000 AFIX 0 C5 1 0.245560 0.091420 0.427906 11.00000 0.03370 0.01864 = 0.02269 0.00248 -0.00619 -0.00914 C10 1 0.761067 0.732435 0.740678 11.00000 0.02573 0.01991 = 0.02777 -0.00609 0.00191 -0.00195 AFIX 23 H10A 2 0.714215 0.803712 0.753624 11.00000 -1.20000 H10B 2 0.852211 0.752326 0.725145 11.00000 -1.20000 AFIX 0 C11 1 0.781167 0.648064 0.805515 11.00000 0.03091 0.02990 = 0.02072 -0.00626 -0.00004 -0.00168 AFIX 23 H11A 2 0.866764 0.666644 0.841718 11.00000 -1.20000 H11B 2 0.698490 0.648093 0.831752 11.00000 -1.20000 AFIX 0 C7 1 0.200661 0.537292 0.665368 11.00000 0.03310 0.03927 = 0.02382 -0.00133 0.00513 0.00622 AFIX 23 H7A 2 0.298688 0.551035 0.690309 11.00000 -1.20000 H7B 2 0.165064 0.467276 0.687113 11.00000 -1.20000 AFIX 0 C12 1 0.796409 0.533595 0.767959 11.00000 0.03565 0.02408 = 0.01769 0.00011 -0.00631 -0.00068 AFIX 23 H12A 2 0.896428 0.518042 0.764525 11.00000 -1.20000 H12B 2 0.760099 0.470365 0.796042 11.00000 -1.20000 AFIX 0 C8 1 0.110281 0.637669 0.676836 11.00000 0.05143 0.03804 = 0.03371 -0.00262 0.01069 0.01005 AFIX 137 H8A 2 0.014771 0.625178 0.649666 11.00000 -1.50000 H8B 2 0.149865 0.707424 0.658138 11.00000 -1.50000 H8C 2 0.106770 0.646414 0.730245 11.00000 -1.50000 AFIX 0 HKLF 4 REM 1_a.res in P2(1)/c REM wR2 = 0.078664, GooF = S = 1.07288, Restrained GooF = 1.07288 for all data REM R1 = 0.029107 for 3732 Fo > 4sig(Fo) and 0.030585 for all 3948 data REM 236 parameters refined using 0 restraints END WGHT 0.0463 1.9516 REM Highest difference peak 1.329, deepest hole -0.401, 1-sigma level 0.108 Q1 1 0.7587 0.3963 0.6306 11.00000 0.05 1.33 Q2 1 0.7106 0.3970 0.5946 11.00000 0.05 0.98 Q3 1 0.5400 0.4013 0.6011 11.00000 0.05 0.97 Q4 1 0.0875 0.5358 0.5771 11.00000 0.05 0.67 ; _shelx_res_checksum 20535 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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 0.65320(2) 0.40253(2) 0.61458(2) 0.01625(8) Uani 1 1 d . . . . . Cl3 Cl 0.66438(7) 0.12494(5) 0.44018(3) 0.02574(14) Uani 1 1 d . . . . . Cl1 Cl 0.57657(7) 0.30273(5) 0.71876(3) 0.02558(14) Uani 1 1 d . . . . . Cl2 Cl 0.89095(6) 0.33106(5) 0.64128(4) 0.02737(15) Uani 1 1 d . . . . . P1 P 0.31552(6) 0.46244(5) 0.55113(3) 0.01793(14) Uani 1 1 d . . . . . Cl4 Cl 0.42063(8) -0.03179(5) 0.35592(4) 0.03209(16) Uani 1 1 d . . . . . Cl6 Cl 0.04580(7) 0.20153(6) 0.49237(4) 0.03173(16) Uani 1 1 d . . . . . Cl5 Cl 0.11201(8) 0.00598(6) 0.38296(4) 0.03788(18) Uani 1 1 d . . . . . O5 O 0.56654(18) 0.29113(14) 0.54015(9) 0.0193(3) Uani 1 1 d . . . . . O6 O 0.71195(18) 0.54507(14) 0.69304(9) 0.0201(3) Uani 1 1 d . . . . . O3 O 0.29209(18) 0.48596(15) 0.46845(9) 0.0201(3) Uani 1 1 d . . . . . O1 O 0.45848(18) 0.49457(15) 0.59346(10) 0.0206(3) Uani 1 1 d . . . . . O2 O 0.29096(19) 0.32793(15) 0.56264(10) 0.0212(4) Uani 1 1 d . . . . . O4 O 0.1970(2) 0.52209(17) 0.58528(11) 0.0262(4) Uani 1 1 d . . . . . C1 C 0.3235(3) 0.2449(2) 0.51356(13) 0.0193(5) Uani 1 1 d . . . . . C3 C 0.4921(3) 0.1422(2) 0.45356(14) 0.0211(5) Uani 1 1 d . . . . . C2 C 0.4634(3) 0.2275(2) 0.50342(13) 0.0186(5) Uani 1 1 d . . . . . C4 C 0.3834(3) 0.0742(2) 0.41565(14) 0.0242(5) Uani 1 1 d . . . . . C6 C 0.2151(3) 0.1771(2) 0.47653(14) 0.0236(5) Uani 1 1 d . . . . . C9 C 0.6678(3) 0.6655(2) 0.68046(15) 0.0236(5) Uani 1 1 d . . . . . H9A H 0.567182 0.675034 0.685045 0.028 Uiso 1 1 calc R . . . . H9B H 0.681791 0.691486 0.630201 0.028 Uiso 1 1 calc R . . . . C5 C 0.2456(3) 0.0914(2) 0.42791(15) 0.0262(6) Uani 1 1 d . . . . . C10 C 0.7611(3) 0.7324(2) 0.74068(15) 0.0247(5) Uani 1 1 d . . . . . H10A H 0.714215 0.803712 0.753624 0.030 Uiso 1 1 calc R . . . . H10B H 0.852211 0.752326 0.725145 0.030 Uiso 1 1 calc R . . . . C11 C 0.7812(3) 0.6481(2) 0.80551(15) 0.0276(6) Uani 1 1 d . . . . . H11A H 0.866764 0.666644 0.841718 0.033 Uiso 1 1 calc R . . . . H11B H 0.698490 0.648093 0.831752 0.033 Uiso 1 1 calc R . . . . C7 C 0.2007(3) 0.5373(3) 0.66537(16) 0.0320(6) Uani 1 1 d . . . . . H7A H 0.298688 0.551035 0.690309 0.038 Uiso 1 1 calc R . . . . H7B H 0.165064 0.467276 0.687113 0.038 Uiso 1 1 calc R . . . . C12 C 0.7964(3) 0.5336(2) 0.76796(14) 0.0270(6) Uani 1 1 d . . . . . H12A H 0.896428 0.518042 0.764525 0.032 Uiso 1 1 calc R . . . . H12B H 0.760099 0.470365 0.796042 0.032 Uiso 1 1 calc R . . . . C8 C 0.1103(4) 0.6377(3) 0.67684(19) 0.0406(7) Uani 1 1 d . . . . . H8A H 0.014771 0.625178 0.649666 0.061 Uiso 1 1 calc GR . . . . H8B H 0.149865 0.707424 0.658138 0.061 Uiso 1 1 calc GR . . . . H8C H 0.106770 0.646414 0.730245 0.061 Uiso 1 1 calc GR . . . . 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 0.01783(13) 0.01400(12) 0.01622(12) -0.00155(6) 0.00069(8) -0.00048(6) Cl3 0.0308(3) 0.0226(3) 0.0238(3) -0.0036(2) 0.0043(2) 0.0043(2) Cl1 0.0311(3) 0.0239(3) 0.0223(3) 0.0006(2) 0.0062(2) -0.0056(2) Cl2 0.0217(3) 0.0265(3) 0.0331(3) 0.0009(2) 0.0020(2) 0.0058(2) P1 0.0184(3) 0.0174(3) 0.0181(3) -0.0024(2) 0.0030(2) 0.0003(2) Cl4 0.0499(4) 0.0182(3) 0.0247(3) -0.0069(2) -0.0045(3) 0.0019(3) Cl6 0.0234(3) 0.0409(4) 0.0298(3) 0.0024(3) 0.0012(3) -0.0085(3) Cl5 0.0411(4) 0.0318(4) 0.0358(4) -0.0043(3) -0.0086(3) -0.0166(3) O5 0.0227(8) 0.0159(8) 0.0190(8) -0.0036(6) 0.0023(7) -0.0026(6) O6 0.0251(9) 0.0154(8) 0.0176(8) -0.0011(6) -0.0035(7) 0.0001(7) O3 0.0219(8) 0.0184(8) 0.0195(8) -0.0007(6) 0.0015(7) -0.0011(6) O1 0.0194(8) 0.0185(8) 0.0231(8) -0.0032(7) 0.0007(7) 0.0021(7) O2 0.0257(9) 0.0202(9) 0.0185(8) -0.0004(7) 0.0059(7) -0.0023(7) O4 0.0240(9) 0.0309(10) 0.0245(9) -0.0044(7) 0.0058(7) 0.0048(7) C1 0.0263(12) 0.0144(11) 0.0167(11) 0.0019(9) 0.0018(9) -0.0024(9) C3 0.0300(13) 0.0141(11) 0.0184(11) 0.0009(9) 0.0011(10) 0.0008(9) C2 0.0249(12) 0.0127(10) 0.0166(11) 0.0013(9) -0.0008(9) -0.0019(9) C4 0.0389(15) 0.0147(11) 0.0166(11) 0.0003(9) -0.0031(10) -0.0003(10) C6 0.0264(13) 0.0231(12) 0.0196(11) 0.0058(10) -0.0009(10) -0.0045(10) C9 0.0298(13) 0.0169(12) 0.0228(12) -0.0033(9) 0.0004(10) 0.0024(10) C5 0.0337(15) 0.0186(12) 0.0227(13) 0.0025(9) -0.0062(11) -0.0091(10) C10 0.0257(13) 0.0199(12) 0.0278(13) -0.0061(10) 0.0019(10) -0.0020(10) C11 0.0309(14) 0.0299(14) 0.0207(12) -0.0063(11) 0.0000(10) -0.0017(11) C7 0.0331(15) 0.0393(16) 0.0238(13) -0.0013(11) 0.0051(11) 0.0062(12) C12 0.0356(15) 0.0241(13) 0.0177(12) 0.0001(10) -0.0063(10) -0.0007(11) C8 0.051(2) 0.0380(17) 0.0337(16) -0.0026(13) 0.0107(14) 0.0100(15) 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' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 '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 Cl2 Zr1 Cl1 94.33(2) . . ? O5 Zr1 Cl1 94.07(5) . . ? O5 Zr1 Cl2 101.20(5) . . ? O5 Zr1 O6 169.05(7) . . ? O5 Zr1 O3 92.42(7) . 3_666 ? O5 Zr1 O1 86.88(7) . . ? O6 Zr1 Cl1 86.32(5) . . ? O6 Zr1 Cl2 89.68(5) . . ? O3 Zr1 Cl1 170.62(5) 3_666 . ? O3 Zr1 Cl2 91.04(5) 3_666 . ? O3 Zr1 O6 86.02(6) 3_666 . ? O3 Zr1 O1 82.90(7) 3_666 . ? O1 Zr1 Cl1 90.70(5) . . ? O1 Zr1 Cl2 170.13(5) . . ? O1 Zr1 O6 82.17(7) . . ? O3 P1 O1 116.06(10) . . ? O3 P1 O2 107.83(10) . . ? O3 P1 O4 108.43(10) . . ? O1 P1 O2 108.49(10) . . ? O1 P1 O4 110.74(10) . . ? O4 P1 O2 104.65(10) . . ? C2 O5 Zr1 156.28(16) . . ? C9 O6 Zr1 125.50(14) . . ? C9 O6 C12 109.37(18) . . ? C12 O6 Zr1 125.07(14) . . ? P1 O3 Zr1 143.67(11) . 3_666 ? P1 O1 Zr1 131.78(10) . . ? C1 O2 P1 123.05(15) . . ? C7 O4 P1 123.55(18) . . ? O2 C1 C2 120.5(2) . . ? O2 C1 C6 118.5(2) . . ? C6 C1 C2 121.0(2) . . ? C2 C3 Cl3 117.9(2) . . ? C4 C3 Cl3 121.5(2) . . ? C4 C3 C2 120.6(2) . . ? O5 C2 C1 120.6(2) . . ? O5 C2 C3 120.7(2) . . ? C3 C2 C1 118.7(2) . . ? C3 C4 Cl4 120.1(2) . . ? C5 C4 Cl4 120.3(2) . . ? C5 C4 C3 119.6(2) . . ? C1 C6 Cl6 118.8(2) . . ? C1 C6 C5 119.6(2) . . ? C5 C6 Cl6 121.6(2) . . ? O6 C9 C10 104.8(2) . . ? C4 C5 Cl5 119.8(2) . . ? C4 C5 C6 120.4(2) . . ? C6 C5 Cl5 119.8(2) . . ? C9 C10 C11 102.3(2) . . ? C12 C11 C10 103.3(2) . . ? O4 C7 C8 108.3(2) . . ? O6 C12 C11 104.9(2) . . ? 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 Cl1 2.4313(6) . ? Zr1 Cl2 2.4063(6) . ? Zr1 O5 1.9578(17) . ? Zr1 O6 2.1990(17) . ? Zr1 O3 2.1176(17) 3_666 ? Zr1 O1 2.1366(17) . ? Cl3 C3 1.723(3) . ? P1 O3 1.5051(18) . ? P1 O1 1.5087(18) . ? P1 O2 1.6016(18) . ? P1 O4 1.5463(18) . ? Cl4 C4 1.717(3) . ? Cl6 C6 1.721(3) . ? Cl5 C5 1.721(3) . ? O5 C2 1.327(3) . ? O6 C9 1.472(3) . ? O6 C12 1.472(3) . ? O2 C1 1.384(3) . ? O4 C7 1.458(3) . ? C1 C2 1.400(4) . ? C1 C6 1.390(4) . ? C3 C2 1.400(3) . ? C3 C4 1.400(4) . ? C4 C5 1.393(4) . ? C6 C5 1.394(4) . ? C9 C10 1.512(4) . ? C10 C11 1.520(4) . ? C11 C12 1.514(4) . ? C7 C8 1.490(4) . ?