# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Thomas, Christine' 'Napoline, J.' 'Rowe, Gerard' 'Foxman, Bruce' _publ_contact_author_name 'Thomas, Christine' _publ_contact_author_email thomasc@brandeis.edu _publ_section_title ; Oxidative Addition Across Co/Zr Multiple Bonds in Early/Late Heterobimetallic Complexes ; # Attachment '- combined_rev.cif' data_4 _database_code_depnum_ccdc_archive 'CCDC 776339' #TrackingRef '- combined_rev.cif' # start Validation Reply Form: Three Alert B issues _vrf_PLAT222_4 ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 4.04 Ratio RESPONSE:The 4.04 ratio is between a typical ring H atom and an H atom attached to methyl group C29, which is slightly disordered. The disorder was not resolved. ; _vrf_PLAT232_4 ; PROBLEM: Hirshfeld Test Diff (M-X) I1 -- Co1 .. 19.09 su Hirshfeld Test Diff (M-X) I2 -- Zr1 .. 10.16 su RESPONSE:For the Hirshfeld test alerts, the differences are quite small. Thus we have I-Co at 0.0010(1); I-Zr at 0.0019(1) and Zr-P averaging 0.0012(2). They may reflect a less than adequate absorption correction, with some difficulty accurately measuring the fragment cut from a larger crystal. ; # end Validation Reply Form _audit_creation_date 09-12-18 _audit_creation_method CRYSTALS_ver_14.01 _oxford_structure_analysis_title 'cmt32_0m in C2/c' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 27.2429(12) _cell_length_b 31.7135(14) _cell_length_c 16.8195(7) _cell_angle_alpha 90 _cell_angle_beta 127.715(2) _cell_angle_gamma 90 _cell_volume 11495.3(9) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/2,y+1/2,z -x+1/2,-y+1/2,-z -x,y,-z+1/2 x,-y,z+1/2 -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' Co 0.3494 0.9721 12.2841 4.2791 7.3409 0.2784 4.0034 13.5359 2.3488 71.1692 1.0118 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Zr -2.9673 0.5597 17.8765 1.2762 10.9480 11.9160 5.4173 0.1176 3.6572 87.6627 2.0693 'International Tables Vol C 4.2.6.8 and 6.1.1.4' I -0.4742 1.8119 20.1472 4.3470 18.9949 0.3814 7.5138 27.7660 2.2735 66.8776 4.0712 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 8 # Given Formula = C45 H75 Co1 I2 N3 P3 Zr1 # Dc = 1.33 Fooo = 4672.00 Mu = 16.56 M = 1154.99 # Found Formula = C45 H75 Co1 I2 N3 P3 Zr1 # Dc = 1.33 FOOO = 4672.00 Mu = 16.56 M = 1154.99 _chemical_formula_sum 'C45 H75 Co1 I2 N3 P3 Zr1' _chemical_formula_moiety 'C45 H75 Co1 I2 N3 P3 Zr1' _chemical_compound_source ? _chemical_formula_weight 1154.99 _cell_measurement_reflns_used 9918 _cell_measurement_theta_min 2 _cell_measurement_theta_max 30 _cell_measurement_temperature 120 _exptl_crystal_description 'acicular fragment' _exptl_crystal_colour orange _exptl_crystal_size_min 0.160 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_max 0.473 _exptl_crystal_density_diffrn 1.335 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 4672 _exptl_absorpt_coefficient_mu 1.656 # Sheldrick geometric approximatio 0.72 0.77 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Analytical Absorption (De Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_min 0.72 _exptl_absorpt_correction_T_max 0.77 _diffrn_measurement_device-type 'Bruker Kappa Apex2' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'Apex2 (Bruker AXS, 2006)' _computing_cell_refinement 'Apex2 (Bruker AXS, 2006)' _computing_data_reduction 'Apex2 (Bruker AXS, 2006)' _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 120 _diffrn_reflns_number 16791 _reflns_number_total 16791 _diffrn_reflns_av_R_equivalents 0.038 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 16791 # Theoretical number of reflections is about 33641 _diffrn_reflns_theta_min 1.142 _diffrn_reflns_theta_max 30.036 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.036 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 44 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _reflns_limit_h_min -38 _reflns_limit_h_max 30 _reflns_limit_k_min 0 _reflns_limit_k_max 44 _reflns_limit_l_min 0 _reflns_limit_l_max 23 _oxford_diffrn_Wilson_B_factor 1.51 _oxford_diffrn_Wilson_scale 67.75 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.66 _refine_diff_density_max 0.92 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 16791 _refine_ls_number_restraints 0 _refine_ls_number_parameters 496 _oxford_refine_ls_R_factor_ref 0.0315 _refine_ls_wR_factor_ref 0.0608 _refine_ls_goodness_of_fit_ref 1.0639 _refine_ls_shift/su_max 0.0050614 _refine_ls_shift/su_mean 0.0001011 # The values computed from all data _oxford_reflns_number_all 16791 _refine_ls_R_factor_all 0.0315 _refine_ls_wR_factor_all 0.0608 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 13736 _refine_ls_R_factor_gt 0.0228 _refine_ls_wR_factor_gt 0.0515 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment none # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.02P)^2^ +18.68P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Bruker Analytical X-ray Systems, Inc., 2006. Apex2, Version 2 User Manual, M86-E01078, Madison, WI. De Meulenaer, J. & Tompa, H. (1965). Acta Cryst. 19, 1014. Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst. 40, 786-790. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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 _oxford_atom_site_special_shape _atom_site_attached_hydrogens I1 I 0.278017(7) 0.401098(4) 0.070007(10) 0.0246 1.0000 Uani . . . . . . . I2 I 0.241408(6) 0.524009(4) -0.057307(9) 0.0172 1.0000 Uani . . . . . . . Zr1 Zr 0.250124(7) 0.564666(5) 0.102945(12) 0.0118 1.0000 Uani . . . . . . . Co1 Co 0.259465(11) 0.477739(8) 0.093936(18) 0.0146 1.0000 Uani . . . . . . . P1 P 0.34471(2) 0.503583(15) 0.24185(3) 0.0139 1.0000 Uani . . . . . . . P2 P 0.16783(2) 0.493313(15) 0.06581(3) 0.0151 1.0000 Uani . . . . . . . P3 P 0.25249(2) 0.646898(15) 0.13584(4) 0.0158 1.0000 Uani . . . . . . . N1 N 0.33947(7) 0.55695(5) 0.24339(11) 0.0143 1.0000 Uani . . . . . . . N2 N 0.16555(7) 0.54655(5) 0.07533(11) 0.0163 1.0000 Uani . . . . . . . N3 N 0.24337(7) 0.62430(5) 0.03714(11) 0.0151 1.0000 Uani . . . . . . . C1 C 0.35471(9) 0.48333(6) 0.35422(14) 0.0193 1.0000 Uani . . . . . . . C2 C 0.41685(10) 0.49318(7) 0.45606(15) 0.0260 1.0000 Uani . . . . . . . C3 C 0.34065(10) 0.43609(7) 0.34802(16) 0.0263 1.0000 Uani . . . . . . . C4 C 0.41789(8) 0.49067(6) 0.26122(14) 0.0171 1.0000 Uani . . . . . . . C5 C 0.44008(9) 0.44506(7) 0.29491(16) 0.0243 1.0000 Uani . . . . . . . C6 C 0.40985(9) 0.49887(7) 0.16419(14) 0.0203 1.0000 Uani . . . . . . . C7 C 0.37925(8) 0.58196(6) 0.33351(13) 0.0169 1.0000 Uani . . . . . . . C8 C 0.43779(9) 0.59642(6) 0.36630(14) 0.0201 1.0000 Uani . . . . . . . C9 C 0.47460(10) 0.61922(7) 0.45629(16) 0.0273 1.0000 Uani . . . . . . . C10 C 0.45598(11) 0.62869(7) 0.51415(15) 0.0303 1.0000 Uani . . . . . . . C11 C 0.39767(11) 0.61494(7) 0.47960(16) 0.0285 1.0000 Uani . . . . . . . C12 C 0.35876(9) 0.59229(6) 0.39045(14) 0.0217 1.0000 Uani . . . . . . . C13 C 0.46353(9) 0.59034(7) 0.30924(16) 0.0245 1.0000 Uani . . . . . . . C14 C 0.49654(13) 0.65447(9) 0.60936(18) 0.0463 1.0000 Uani . . . . . . . C15 C 0.29626(10) 0.58034(7) 0.35962(16) 0.0271 1.0000 Uani . . . . . . . C16 C 0.10090(9) 0.47655(6) -0.06346(15) 0.0215 1.0000 Uani . . . . . . . C17 C 0.03556(9) 0.48576(7) -0.09581(16) 0.0262 1.0000 Uani . . . . . . . C18 C 0.10413(11) 0.43048(8) -0.08547(19) 0.0365 1.0000 Uani . . . . . . . C19 C 0.15968(9) 0.46733(6) 0.15594(14) 0.0185 1.0000 Uani . . . . . . . C20 C 0.09804(9) 0.47342(7) 0.13944(17) 0.0251 1.0000 Uani . . . . . . . C21 C 0.17493(11) 0.42024(7) 0.16824(18) 0.0289 1.0000 Uani . . . . . . . C22 C 0.11447(8) 0.57288(6) 0.04867(15) 0.0191 1.0000 Uani . . . . . . . C23 C 0.10531(9) 0.58423(7) 0.11957(17) 0.0244 1.0000 Uani . . . . . . . C24 C 0.05726(10) 0.61250(7) 0.0907(2) 0.0332 1.0000 Uani . . . . . . . C25 C 0.01963(10) 0.63031(7) -0.0039(2) 0.0372 1.0000 Uani . . . . . . . C26 C 0.02928(10) 0.61887(7) -0.07245(19) 0.0344 1.0000 Uani . . . . . . . C27 C 0.07497(9) 0.59023(7) -0.04951(16) 0.0255 1.0000 Uani . . . . . . . C28 C 0.14400(10) 0.56840(7) 0.22574(17) 0.0285 1.0000 Uani . . . . . . . C29 C -0.02986(12) 0.66223(10) -0.0305(3) 0.0574 1.0000 Uani . . . . . . . C30 C 0.07986(10) 0.57829(7) -0.13104(16) 0.0311 1.0000 Uani . . . . . . . C31 C 0.18615(9) 0.67998(6) 0.10104(17) 0.0243 1.0000 Uani . . . . . . . C32 C 0.18239(12) 0.68300(8) 0.1884(2) 0.0359 1.0000 Uani . . . . . . . C33 C 0.18211(10) 0.72399(7) 0.05978(19) 0.0335 1.0000 Uani . . . . . . . C34 C 0.32357(9) 0.67983(6) 0.20721(15) 0.0205 1.0000 Uani . . . . . . . C35 C 0.32873(9) 0.71374(6) 0.14752(17) 0.0245 1.0000 Uani . . . . . . . C36 C 0.33520(11) 0.69924(7) 0.30084(16) 0.0294 1.0000 Uani . . . . . . . C37 C 0.24623(9) 0.64237(6) -0.03885(13) 0.0169 1.0000 Uani . . . . . . . C38 C 0.30209(10) 0.63966(6) -0.02648(15) 0.0214 1.0000 Uani . . . . . . . C39 C 0.30510(11) 0.65589(6) -0.10065(18) 0.0278 1.0000 Uani . . . . . . . C40 C 0.25447(12) 0.67440(7) -0.18759(17) 0.0307 1.0000 Uani . . . . . . . C41 C 0.20069(11) 0.67730(6) -0.19744(15) 0.0276 1.0000 Uani . . . . . . . C42 C 0.19497(9) 0.66176(6) -0.12564(14) 0.0216 1.0000 Uani . . . . . . . C43 C 0.35898(9) 0.62009(7) 0.06467(17) 0.0247 1.0000 Uani . . . . . . . C44 C 0.25854(16) 0.69002(8) -0.2684(2) 0.0468 1.0000 Uani . . . . . . . C45 C 0.13295(10) 0.66703(8) -0.14746(17) 0.0331 1.0000 Uani . . . . . . . H11 H 0.3232 0.4983 0.3538 0.0228 1.0000 Uiso R . . . . . . H21 H 0.4257 0.5228 0.4606 0.0390 1.0000 Uiso R . . . . . . H22 H 0.4490 0.4771 0.4627 0.0390 1.0000 Uiso R . . . . . . H23 H 0.4148 0.4854 0.5092 0.0387 1.0000 Uiso R . . . . . . H31 H 0.3308 0.4294 0.3920 0.0388 1.0000 Uiso R . . . . . . H32 H 0.3059 0.4291 0.2802 0.0392 1.0000 Uiso R . . . . . . H33 H 0.3759 0.4199 0.3667 0.0390 1.0000 Uiso R . . . . . . H41 H 0.4500 0.5101 0.3137 0.0211 1.0000 Uiso R . . . . . . H51 H 0.4540 0.4406 0.3629 0.0358 1.0000 Uiso R . . . . . . H52 H 0.4746 0.4394 0.2949 0.0357 1.0000 Uiso R . . . . . . H53 H 0.4074 0.4256 0.2501 0.0361 1.0000 Uiso R . . . . . . H61 H 0.3882 0.5255 0.1347 0.0299 1.0000 Uiso R . . . . . . H62 H 0.4498 0.5011 0.1786 0.0299 1.0000 Uiso R . . . . . . H63 H 0.3864 0.4766 0.1167 0.0301 1.0000 Uiso R . . . . . . H91 H 0.5140 0.6284 0.4799 0.0330 1.0000 Uiso R . . . . . . H111 H 0.3837 0.6209 0.5166 0.0340 1.0000 Uiso R . . . . . . H131 H 0.5009 0.5730 0.3468 0.0358 1.0000 Uiso R . . . . . . H132 H 0.4733 0.6169 0.2954 0.0360 1.0000 Uiso R . . . . . . H133 H 0.4329 0.5767 0.2455 0.0359 1.0000 Uiso R . . . . . . H141 H 0.4923 0.6440 0.6587 0.0692 1.0000 Uiso R . . . . . . H142 H 0.5395 0.6511 0.6359 0.0688 1.0000 Uiso R . . . . . . H143 H 0.4857 0.6838 0.5955 0.0689 1.0000 Uiso R . . . . . . H151 H 0.2748 0.6042 0.3591 0.0402 1.0000 Uiso R . . . . . . H152 H 0.2708 0.5695 0.2932 0.0400 1.0000 Uiso R . . . . . . H153 H 0.2980 0.5597 0.4030 0.0401 1.0000 Uiso R . . . . . . H161 H 0.1055 0.4930 -0.1081 0.0259 1.0000 Uiso R . . . . . . H171 H 0.0061 0.4854 -0.1682 0.0378 1.0000 Uiso R . . . . . . H172 H 0.0238 0.4651 -0.0688 0.0378 1.0000 Uiso R . . . . . . H173 H 0.0331 0.5128 -0.0735 0.0375 1.0000 Uiso R . . . . . . H181 H 0.0984 0.4129 -0.0453 0.0550 1.0000 Uiso R . . . . . . H182 H 0.0717 0.4239 -0.1553 0.0548 1.0000 Uiso R . . . . . . H183 H 0.1440 0.4247 -0.0700 0.0550 1.0000 Uiso R . . . . . . H191 H 0.1916 0.4807 0.2197 0.0218 1.0000 Uiso R . . . . . . H201 H 0.0832 0.5014 0.1147 0.0366 1.0000 Uiso R . . . . . . H202 H 0.1050 0.4702 0.2023 0.0367 1.0000 Uiso R . . . . . . H203 H 0.0679 0.4531 0.0909 0.0371 1.0000 Uiso R . . . . . . H211 H 0.1392 0.4052 0.1129 0.0427 1.0000 Uiso R . . . . . . H212 H 0.1849 0.4104 0.2301 0.0431 1.0000 Uiso R . . . . . . H213 H 0.2093 0.4154 0.1664 0.0430 1.0000 Uiso R . . . . . . H241 H 0.0505 0.6192 0.1371 0.0398 1.0000 Uiso R . . . . . . H261 H 0.0045 0.6306 -0.1356 0.0412 1.0000 Uiso R . . . . . . H281 H 0.1180 0.5555 0.2394 0.0430 1.0000 Uiso R . . . . . . H282 H 0.1667 0.5912 0.2727 0.0429 1.0000 Uiso R . . . . . . H283 H 0.1735 0.5477 0.2375 0.0427 1.0000 Uiso R . . . . . . H291 H -0.0485 0.6536 0.0002 0.0852 1.0000 Uiso R . . . . . . H292 H -0.0124 0.6894 -0.0077 0.0852 1.0000 Uiso R . . . . . . H293 H -0.0619 0.6625 -0.1021 0.0850 1.0000 Uiso R . . . . . . H301 H 0.0588 0.5987 -0.1838 0.0459 1.0000 Uiso R . . . . . . H302 H 0.1220 0.5774 -0.1059 0.0455 1.0000 Uiso R . . . . . . H303 H 0.0610 0.5514 -0.1590 0.0456 1.0000 Uiso R . . . . . . H311 H 0.1489 0.6643 0.0466 0.0301 1.0000 Uiso R . . . . . . H321 H 0.2133 0.7026 0.2384 0.0528 1.0000 Uiso R . . . . . . H322 H 0.1428 0.6933 0.1633 0.0531 1.0000 Uiso R . . . . . . H323 H 0.1886 0.6557 0.2179 0.0528 1.0000 Uiso R . . . . . . H331 H 0.1422 0.7360 0.0311 0.0492 1.0000 Uiso R . . . . . . H332 H 0.2133 0.7420 0.1133 0.0489 1.0000 Uiso R . . . . . . H333 H 0.1886 0.7225 0.0089 0.0489 1.0000 Uiso R . . . . . . H341 H 0.3576 0.6595 0.2318 0.0253 1.0000 Uiso R . . . . . . H351 H 0.3700 0.7260 0.1882 0.0369 1.0000 Uiso R . . . . . . H352 H 0.2988 0.7362 0.1257 0.0373 1.0000 Uiso R . . . . . . H353 H 0.3224 0.7023 0.0888 0.0372 1.0000 Uiso R . . . . . . H361 H 0.3768 0.7100 0.3455 0.0438 1.0000 Uiso R . . . . . . H362 H 0.3288 0.6776 0.3346 0.0439 1.0000 Uiso R . . . . . . H363 H 0.3066 0.7220 0.2814 0.0439 1.0000 Uiso R . . . . . . H391 H 0.3426 0.6544 -0.0912 0.0329 1.0000 Uiso R . . . . . . H411 H 0.1663 0.6898 -0.2548 0.0332 1.0000 Uiso R . . . . . . H431 H 0.3748 0.6361 0.1234 0.0371 1.0000 Uiso R . . . . . . H432 H 0.3501 0.5922 0.0762 0.0371 1.0000 Uiso R . . . . . . H433 H 0.3910 0.6172 0.0578 0.0371 1.0000 Uiso R . . . . . . H441 H 0.2926 0.7099 -0.2377 0.0730 1.0000 Uiso R . . . . . . H442 H 0.2207 0.7036 -0.3200 0.0730 1.0000 Uiso R . . . . . . H443 H 0.2670 0.6666 -0.2947 0.0729 1.0000 Uiso R . . . . . . H451 H 0.1010 0.6544 -0.2113 0.0489 1.0000 Uiso R . . . . . . H452 H 0.1324 0.6533 -0.0967 0.0487 1.0000 Uiso R . . . . . . H453 H 0.1236 0.6964 -0.1495 0.0491 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 I1 0.03442(7) 0.01687(6) 0.03224(7) -0.00006(5) 0.02543(6) 0.00102(5) I2 0.02104(6) 0.01857(6) 0.01476(5) -0.00062(4) 0.01242(5) -0.00121(4) Zr1 0.01184(7) 0.01216(8) 0.01219(7) 0.00070(6) 0.00776(6) 0.00015(6) Co1 0.01581(11) 0.01432(12) 0.01584(11) 0.00008(9) 0.01075(10) -0.00047(9) P1 0.01348(19) 0.0158(2) 0.0137(2) 0.00260(16) 0.00908(17) 0.00148(16) P2 0.01363(19) 0.0171(2) 0.0153(2) 0.00119(17) 0.00924(18) -0.00173(16) P3 0.0166(2) 0.0139(2) 0.0177(2) -0.00049(17) 0.01075(18) 0.00029(17) N1 0.0137(7) 0.0158(7) 0.0138(7) 0.0005(5) 0.0086(6) 0.0005(5) N2 0.0138(7) 0.0181(8) 0.0167(7) 0.0022(6) 0.0092(6) 0.0009(6) N3 0.0166(7) 0.0141(7) 0.0156(7) 0.0017(6) 0.0104(6) 0.0005(6) C1 0.0217(9) 0.0215(10) 0.0182(9) 0.0049(7) 0.0140(8) 0.0030(7) C2 0.0312(11) 0.0273(11) 0.0156(9) 0.0054(8) 0.0123(8) 0.0030(9) C3 0.0333(11) 0.0250(11) 0.0252(10) 0.0041(8) 0.0202(9) -0.0033(8) C4 0.0143(8) 0.0200(9) 0.0176(8) 0.0048(7) 0.0101(7) 0.0038(7) C5 0.0218(9) 0.0254(10) 0.0297(10) 0.0083(8) 0.0178(9) 0.0075(8) C6 0.0164(8) 0.0268(10) 0.0221(9) 0.0042(8) 0.0140(8) 0.0033(7) C7 0.0171(8) 0.0170(9) 0.0125(8) 0.0019(6) 0.0069(7) 0.0014(7) C8 0.0172(8) 0.0174(9) 0.0173(9) 0.0034(7) 0.0062(7) 0.0008(7) C9 0.0207(9) 0.0226(10) 0.0220(10) 0.0015(8) 0.0045(8) -0.0012(8) C10 0.0350(12) 0.0216(10) 0.0168(9) -0.0001(8) 0.0069(9) 0.0030(9) C11 0.0376(12) 0.0251(11) 0.0196(10) -0.0005(8) 0.0158(9) 0.0052(9) C12 0.0256(9) 0.0214(10) 0.0166(9) 0.0024(7) 0.0122(8) 0.0046(8) C13 0.0192(9) 0.0252(10) 0.0270(10) 0.0028(8) 0.0131(8) -0.0039(8) C14 0.0496(16) 0.0359(14) 0.0241(12) -0.0100(10) 0.0076(11) -0.0005(12) C15 0.0318(11) 0.0313(11) 0.0264(10) -0.0013(9) 0.0220(9) 0.0028(9) C16 0.0171(8) 0.0257(10) 0.0179(9) -0.0027(7) 0.0087(7) -0.0042(7) C17 0.0163(9) 0.0314(11) 0.0255(10) -0.0038(8) 0.0101(8) -0.0053(8) C18 0.0298(11) 0.0353(13) 0.0325(12) -0.0139(10) 0.0131(10) -0.0022(10) C19 0.0192(8) 0.0201(9) 0.0199(9) 0.0026(7) 0.0139(8) -0.0004(7) C20 0.0236(9) 0.0279(11) 0.0315(11) 0.0043(8) 0.0209(9) -0.0005(8) C21 0.0393(12) 0.0198(10) 0.0398(12) 0.0058(9) 0.0304(11) 0.0017(9) C22 0.0127(8) 0.0159(9) 0.0266(10) 0.0015(7) 0.0109(7) -0.0008(6) C23 0.0194(9) 0.0205(10) 0.0366(11) -0.0023(8) 0.0188(9) -0.0020(7) C24 0.0244(10) 0.0280(12) 0.0516(15) -0.0088(10) 0.0255(11) -0.0025(9) C25 0.0169(9) 0.0239(11) 0.0547(15) -0.0050(10) 0.0137(10) 0.0025(8) C26 0.0160(9) 0.0256(11) 0.0375(13) 0.0018(9) 0.0041(9) 0.0016(8) C27 0.0165(9) 0.0199(10) 0.0290(10) 0.0023(8) 0.0082(8) -0.0016(7) C28 0.0330(11) 0.0298(11) 0.0355(12) -0.0020(9) 0.0276(10) 0.0005(9) C29 0.0282(13) 0.0424(16) 0.077(2) -0.0080(15) 0.0199(14) 0.0140(12) C30 0.0281(11) 0.0294(12) 0.0211(10) 0.0081(8) 0.0076(9) -0.0012(9) C31 0.0210(9) 0.0163(9) 0.0375(11) -0.0037(8) 0.0188(9) 0.0000(7) C32 0.0382(13) 0.0291(12) 0.0585(16) -0.0156(11) 0.0388(13) -0.0071(10) C33 0.0246(10) 0.0192(10) 0.0474(14) 0.0027(9) 0.0172(10) 0.0053(8) C34 0.0173(8) 0.0165(9) 0.0214(9) -0.0006(7) 0.0086(8) 0.0000(7) C35 0.0235(9) 0.0187(9) 0.0336(11) -0.0030(8) 0.0186(9) -0.0042(7) C36 0.0306(11) 0.0238(11) 0.0236(10) -0.0023(8) 0.0114(9) -0.0025(9) C37 0.0240(9) 0.0116(8) 0.0159(8) 0.0002(6) 0.0126(7) -0.0014(7) C38 0.0307(10) 0.0134(9) 0.0267(10) 0.0000(7) 0.0209(9) 0.0000(7) C39 0.0476(13) 0.0150(9) 0.0405(12) -0.0017(8) 0.0370(11) -0.0014(9) C40 0.0619(15) 0.0140(9) 0.0303(11) -0.0016(8) 0.0354(12) -0.0020(9) C41 0.0440(13) 0.0155(9) 0.0163(9) -0.0015(7) 0.0149(9) -0.0031(8) C42 0.0279(10) 0.0122(8) 0.0179(9) -0.0007(7) 0.0105(8) -0.0020(7) C43 0.0249(10) 0.0207(10) 0.0354(11) 0.0015(8) 0.0220(9) 0.0011(8) C44 0.099(2) 0.0242(12) 0.0489(16) 0.0038(11) 0.0618(18) 0.0041(13) C45 0.0225(10) 0.0311(12) 0.0277(11) 0.0099(9) 0.0062(9) -0.0009(9) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.0224655(5) 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 I1 . Co1 . 2.5640(3) yes I2 . Zr1 . 2.8637(2) yes I2 . Co1 . 2.7084(3) yes Zr1 . Co1 . 2.7811(3) yes Zr1 . P1 . 2.9129(5) yes Zr1 . P2 . 2.9705(5) yes Zr1 . P3 . 2.6585(5) yes Zr1 . N1 . 2.1283(14) yes Zr1 . N2 . 2.1320(15) yes Zr1 . N3 . 2.1415(15) yes Co1 . P1 . 2.2772(5) yes Co1 . P2 . 2.2923(5) yes P1 . N1 . 1.7000(16) yes P1 . C1 . 1.8518(19) yes P1 . C4 . 1.8584(18) yes P2 . N2 . 1.7008(17) yes P2 . C16 . 1.8666(19) yes P2 . C19 . 1.8541(19) yes P3 . N3 . 1.6812(16) yes P3 . C31 . 1.848(2) yes P3 . C34 . 1.8540(19) yes N1 . C7 . 1.446(2) yes N2 . C22 . 1.439(2) yes N3 . C37 . 1.446(2) yes C1 . C2 . 1.533(3) yes C1 . C3 . 1.534(3) yes C1 . H11 . 0.976 no C2 . H21 . 0.961 no C2 . H22 . 0.959 no C2 . H23 . 0.961 no C3 . H31 . 0.953 no C3 . H32 . 0.962 no C3 . H33 . 0.957 no C4 . C5 . 1.536(3) yes C4 . C6 . 1.530(3) yes C4 . H41 . 0.990 no C5 . H51 . 0.970 no C5 . H52 . 0.959 no C5 . H53 . 0.959 no C6 . H61 . 0.975 no C6 . H62 . 0.961 no C6 . H63 . 0.961 no C7 . C8 . 1.408(3) yes C7 . C12 . 1.411(3) yes C8 . C9 . 1.401(3) yes C8 . C13 . 1.508(3) yes C9 . C10 . 1.378(3) yes C9 . H91 . 0.933 no C10 . C11 . 1.386(3) yes C10 . C14 . 1.513(3) yes C11 . C12 . 1.394(3) yes C11 . H111 . 0.926 no C12 . C15 . 1.494(3) yes C13 . H131 . 0.976 no C13 . H132 . 0.953 no C13 . H133 . 0.970 no C14 . H141 . 0.965 no C14 . H142 . 0.970 no C14 . H143 . 0.960 no C15 . H151 . 0.954 no C15 . H152 . 0.949 no C15 . H153 . 0.958 no C16 . C17 . 1.538(3) yes C16 . C18 . 1.523(3) yes C16 . H161 . 0.984 no C17 . H171 . 0.965 no C17 . H172 . 0.957 no C17 . H173 . 0.955 no C18 . H181 . 0.960 no C18 . H182 . 0.966 no C18 . H183 . 0.968 no C19 . C20 . 1.538(3) yes C19 . C21 . 1.530(3) yes C19 . H191 . 0.972 no C20 . H201 . 0.957 no C20 . H202 . 0.959 no C20 . H203 . 0.967 no C21 . H211 . 0.965 no C21 . H212 . 0.952 no C21 . H213 . 0.967 no C22 . C23 . 1.406(3) yes C22 . C27 . 1.419(3) yes C23 . C24 . 1.405(3) yes C23 . C28 . 1.500(3) yes C24 . C25 . 1.380(4) yes C24 . H241 . 0.931 no C25 . C26 . 1.379(4) yes C25 . C29 . 1.518(3) yes C26 . C27 . 1.391(3) yes C26 . H261 . 0.919 no C27 . C30 . 1.505(3) yes C28 . H281 . 0.959 no C28 . H282 . 0.966 no C28 . H283 . 0.961 no C29 . H291 . 0.959 no C29 . H292 . 0.945 no C29 . H293 . 0.962 no C30 . H301 . 0.955 no C30 . H302 . 0.950 no C30 . H303 . 0.957 no C31 . C32 . 1.537(3) yes C31 . C33 . 1.533(3) yes C31 . H311 . 0.989 no C32 . H321 . 0.967 no C32 . H322 . 0.943 no C32 . H323 . 0.961 no C33 . H331 . 0.958 no C33 . H332 . 0.961 no C33 . H333 . 0.974 no C34 . C35 . 1.535(3) yes C34 . C36 . 1.533(3) yes C34 . H341 . 0.988 no C35 . H351 . 0.970 no C35 . H352 . 0.970 no C35 . H353 . 0.964 no C36 . H361 . 0.962 no C36 . H362 . 0.971 no C36 . H363 . 0.961 no C37 . C38 . 1.407(3) yes C37 . C42 . 1.402(3) yes C38 . C39 . 1.397(3) yes C38 . C43 . 1.493(3) yes C39 . C40 . 1.385(3) yes C39 . H391 . 0.935 no C40 . C41 . 1.373(3) yes C40 . C44 . 1.513(3) yes C41 . C42 . 1.399(3) yes C41 . H411 . 0.928 no C42 . C45 . 1.503(3) yes C43 . H431 . 0.946 no C43 . H432 . 0.967 no C43 . H433 . 0.950 no C44 . H441 . 0.969 no C44 . H442 . 0.953 no C44 . H443 . 0.961 no C45 . H451 . 0.964 no C45 . H452 . 0.965 no C45 . H453 . 0.960 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 Zr1 . I2 . Co1 . 59.806(7) yes I2 . Zr1 . Co1 . 57.322(7) yes I2 . Zr1 . P1 . 88.786(11) yes Co1 . Zr1 . P1 . 47.076(11) yes I2 . Zr1 . P2 . 80.893(11) yes Co1 . Zr1 . P2 . 46.833(11) yes P1 . Zr1 . P2 . 81.118(14) yes I2 . Zr1 . P3 . 127.955(12) yes Co1 . Zr1 . P3 . 172.896(13) yes P1 . Zr1 . P3 . 126.049(15) yes P2 . Zr1 . P3 . 135.248(15) yes I2 . Zr1 . N1 . 111.90(4) yes Co1 . Zr1 . N1 . 82.29(4) yes P1 . Zr1 . N1 . 35.26(4) yes P2 . Zr1 . N1 . 110.45(4) yes P3 . Zr1 . N1 . 90.92(4) yes I2 . Zr1 . N2 . 102.55(4) yes Co1 . Zr1 . N2 . 81.01(4) yes P1 . Zr1 . N2 . 107.66(4) yes P2 . Zr1 . N2 . 34.19(4) yes P3 . Zr1 . N2 . 101.25(4) yes I2 . Zr1 . N3 . 88.84(4) yes Co1 . Zr1 . N3 . 146.00(4) yes P1 . Zr1 . N3 . 139.11(4) yes P2 . Zr1 . N3 . 138.49(4) yes P3 . Zr1 . N3 . 39.17(4) yes N1 . Zr1 . N2 . 124.10(6) yes N1 . Zr1 . N3 . 110.70(6) yes N2 . Zr1 . N3 . 112.68(6) yes I2 . Co1 . Zr1 . 62.872(8) yes I2 . Co1 . I1 . 107.827(10) yes Zr1 . Co1 . I1 . 168.995(11) yes I2 . Co1 . P1 . 107.999(15) yes Zr1 . Co1 . P1 . 69.503(14) yes I1 . Co1 . P1 . 110.212(15) yes I2 . Co1 . P2 . 98.063(15) yes Zr1 . Co1 . P2 . 70.930(14) yes I1 . Co1 . P2 . 117.789(16) yes P1 . Co1 . P2 . 113.70(2) yes Zr1 . P1 . Co1 . 63.421(13) yes Co1 . P1 . N1 . 109.63(5) yes Zr1 . P1 . C1 . 123.71(6) yes Co1 . P1 . C1 . 113.90(6) yes N1 . P1 . C1 . 106.92(8) yes Zr1 . P1 . C4 . 127.95(6) yes Co1 . P1 . C4 . 112.33(6) yes N1 . P1 . C4 . 107.93(8) yes C1 . P1 . C4 . 105.80(8) yes Zr1 . P2 . Co1 . 62.237(13) yes Co1 . P2 . N2 . 107.00(5) yes Zr1 . P2 . C16 . 122.39(7) yes Co1 . P2 . C16 . 110.09(7) yes N2 . P2 . C16 . 109.06(8) yes Zr1 . P2 . C19 . 128.24(6) yes Co1 . P2 . C19 . 113.29(6) yes N2 . P2 . C19 . 109.55(8) yes C16 . P2 . C19 . 107.79(9) yes Zr1 . P3 . N3 . 53.57(5) yes Zr1 . P3 . C31 . 126.61(7) yes N3 . P3 . C31 . 113.83(9) yes Zr1 . P3 . C34 . 124.76(6) yes N3 . P3 . C34 . 110.15(8) yes C31 . P3 . C34 . 108.48(9) yes P1 . N1 . Zr1 . 98.47(7) yes P1 . N1 . C7 . 123.09(12) yes Zr1 . N1 . C7 . 135.66(12) yes P2 . N2 . Zr1 . 101.02(7) yes P2 . N2 . C22 . 129.10(13) yes Zr1 . N2 . C22 . 128.45(12) yes P3 . N3 . Zr1 . 87.25(6) yes P3 . N3 . C37 . 130.44(13) yes Zr1 . N3 . C37 . 140.62(12) yes P1 . C1 . C2 . 116.24(14) yes P1 . C1 . C3 . 113.24(14) yes C2 . C1 . C3 . 109.53(16) yes P1 . C1 . H11 . 104.2 no C2 . C1 . H11 . 105.9 no C3 . C1 . H11 . 107.0 no C1 . C2 . H21 . 109.9 no C1 . C2 . H22 . 109.2 no H21 . C2 . H22 . 110.1 no C1 . C2 . H23 . 109.5 no H21 . C2 . H23 . 109.4 no H22 . C2 . H23 . 108.8 no C1 . C3 . H31 . 109.9 no C1 . C3 . H32 . 109.2 no H31 . C3 . H32 . 109.3 no C1 . C3 . H33 . 110.0 no H31 . C3 . H33 . 109.3 no H32 . C3 . H33 . 109.2 no P1 . C4 . C5 . 114.21(13) yes P1 . C4 . C6 . 109.71(12) yes C5 . C4 . C6 . 108.70(16) yes P1 . C4 . H41 . 106.7 no C5 . C4 . H41 . 108.9 no C6 . C4 . H41 . 108.4 no C4 . C5 . H51 . 110.7 no C4 . C5 . H52 . 110.0 no H51 . C5 . H52 . 107.3 no C4 . C5 . H53 . 110.5 no H51 . C5 . H53 . 109.8 no H52 . C5 . H53 . 108.5 no C4 . C6 . H61 . 109.8 no C4 . C6 . H62 . 110.0 no H61 . C6 . H62 . 107.6 no C4 . C6 . H63 . 110.5 no H61 . C6 . H63 . 109.2 no H62 . C6 . H63 . 109.8 no N1 . C7 . C8 . 122.16(16) yes N1 . C7 . C12 . 119.00(16) yes C8 . C7 . C12 . 118.84(17) yes C7 . C8 . C9 . 118.82(19) yes C7 . C8 . C13 . 124.44(17) yes C9 . C8 . C13 . 116.72(18) yes C8 . C9 . C10 . 123.1(2) yes C8 . C9 . H91 . 119.8 no C10 . C9 . H91 . 117.0 no C9 . C10 . C11 . 117.25(19) yes C9 . C10 . C14 . 121.3(2) yes C11 . C10 . C14 . 121.4(2) yes C10 . C11 . C12 . 122.4(2) yes C10 . C11 . H111 . 119.4 no C12 . C11 . H111 . 118.2 no C7 . C12 . C11 . 119.57(19) yes C7 . C12 . C15 . 123.08(18) yes C11 . C12 . C15 . 117.35(19) yes C8 . C13 . H131 . 111.5 no C8 . C13 . H132 . 110.5 no H131 . C13 . H132 . 108.7 no C8 . C13 . H133 . 109.9 no H131 . C13 . H133 . 108.4 no H132 . C13 . H133 . 107.8 no C10 . C14 . H141 . 109.2 no C10 . C14 . H142 . 108.8 no H141 . C14 . H142 . 108.2 no C10 . C14 . H143 . 110.5 no H141 . C14 . H143 . 111.2 no H142 . C14 . H143 . 108.9 no C12 . C15 . H151 . 111.4 no C12 . C15 . H152 . 110.9 no H151 . C15 . H152 . 106.0 no C12 . C15 . H153 . 113.2 no H151 . C15 . H153 . 107.0 no H152 . C15 . H153 . 108.0 no P2 . C16 . C17 . 116.90(14) yes P2 . C16 . C18 . 113.31(15) yes C17 . C16 . C18 . 108.83(17) yes P2 . C16 . H161 . 104.3 no C17 . C16 . H161 . 106.8 no C18 . C16 . H161 . 105.7 no C16 . C17 . H171 . 109.4 no C16 . C17 . H172 . 110.6 no H171 . C17 . H172 . 109.2 no C16 . C17 . H173 . 112.2 no H171 . C17 . H173 . 107.7 no H172 . C17 . H173 . 107.8 no C16 . C18 . H181 . 109.2 no C16 . C18 . H182 . 110.8 no H181 . C18 . H182 . 108.0 no C16 . C18 . H183 . 109.8 no H181 . C18 . H183 . 109.9 no H182 . C18 . H183 . 109.2 no P2 . C19 . C20 . 117.42(14) yes P2 . C19 . C21 . 112.70(14) yes C20 . C19 . C21 . 108.85(16) yes P2 . C19 . H191 . 103.6 no C20 . C19 . H191 . 106.7 no C21 . C19 . H191 . 106.8 no C19 . C20 . H201 . 108.5 no C19 . C20 . H202 . 109.3 no H201 . C20 . H202 . 109.0 no C19 . C20 . H203 . 109.8 no H201 . C20 . H203 . 109.5 no H202 . C20 . H203 . 110.7 no C19 . C21 . H211 . 108.8 no C19 . C21 . H212 . 109.8 no H211 . C21 . H212 . 109.6 no C19 . C21 . H213 . 109.8 no H211 . C21 . H213 . 108.3 no H212 . C21 . H213 . 110.4 no N2 . C22 . C23 . 121.58(17) yes N2 . C22 . C27 . 119.20(18) yes C23 . C22 . C27 . 119.07(18) yes C22 . C23 . C24 . 118.7(2) yes C22 . C23 . C28 . 124.33(18) yes C24 . C23 . C28 . 116.9(2) yes C23 . C24 . C25 . 122.5(2) yes C23 . C24 . H241 . 118.5 no C25 . C24 . H241 . 119.0 no C24 . C25 . C26 . 118.0(2) yes C24 . C25 . C29 . 120.8(3) yes C26 . C25 . C29 . 121.2(3) yes C25 . C26 . C27 . 122.4(2) yes C25 . C26 . H261 . 118.6 no C27 . C26 . H261 . 119.0 no C22 . C27 . C26 . 119.3(2) yes C22 . C27 . C30 . 122.41(19) yes C26 . C27 . C30 . 118.3(2) yes C23 . C28 . H281 . 110.1 no C23 . C28 . H282 . 110.8 no H281 . C28 . H282 . 108.7 no C23 . C28 . H283 . 111.4 no H281 . C28 . H283 . 107.8 no H282 . C28 . H283 . 107.9 no C25 . C29 . H291 . 108.5 no C25 . C29 . H292 . 110.7 no H291 . C29 . H292 . 110.0 no C25 . C29 . H293 . 109.6 no H291 . C29 . H293 . 107.6 no H292 . C29 . H293 . 110.2 no C27 . C30 . H301 . 109.8 no C27 . C30 . H302 . 111.0 no H301 . C30 . H302 . 108.0 no C27 . C30 . H303 . 110.5 no H301 . C30 . H303 . 108.1 no H302 . C30 . H303 . 109.4 no P3 . C31 . C32 . 110.91(16) yes P3 . C31 . C33 . 116.48(15) yes C32 . C31 . C33 . 110.35(18) yes P3 . C31 . H311 . 104.9 no C32 . C31 . H311 . 106.6 no C33 . C31 . H311 . 106.9 no C31 . C32 . H321 . 109.9 no C31 . C32 . H322 . 108.7 no H321 . C32 . H322 . 108.4 no C31 . C32 . H323 . 110.2 no H321 . C32 . H323 . 110.2 no H322 . C32 . H323 . 109.4 no C31 . C33 . H331 . 109.6 no C31 . C33 . H332 . 109.9 no H331 . C33 . H332 . 108.4 no C31 . C33 . H333 . 110.6 no H331 . C33 . H333 . 109.6 no H332 . C33 . H333 . 108.6 no P3 . C34 . C35 . 116.64(14) yes P3 . C34 . C36 . 111.65(14) yes C35 . C34 . C36 . 110.28(17) yes P3 . C34 . H341 . 104.2 no C35 . C34 . H341 . 107.0 no C36 . C34 . H341 . 106.2 no C34 . C35 . H351 . 110.4 no C34 . C35 . H352 . 111.8 no H351 . C35 . H352 . 108.3 no C34 . C35 . H353 . 112.1 no H351 . C35 . H353 . 106.1 no H352 . C35 . H353 . 107.9 no C34 . C36 . H361 . 110.4 no C34 . C36 . H362 . 108.6 no H361 . C36 . H362 . 110.0 no C34 . C36 . H363 . 109.7 no H361 . C36 . H363 . 108.8 no H362 . C36 . H363 . 109.3 no N3 . C37 . C38 . 118.92(16) yes N3 . C37 . C42 . 122.44(17) yes C38 . C37 . C42 . 118.63(17) yes C37 . C38 . C39 . 119.62(19) yes C37 . C38 . C43 . 121.77(17) yes C39 . C38 . C43 . 118.61(19) yes C38 . C39 . C40 . 122.3(2) yes C38 . C39 . H391 . 118.9 no C40 . C39 . H391 . 118.8 no C39 . C40 . C41 . 117.12(19) yes C39 . C40 . C44 . 121.0(2) yes C41 . C40 . C44 . 121.9(2) yes C40 . C41 . C42 . 123.1(2) yes C40 . C41 . H411 . 118.6 no C42 . C41 . H411 . 118.2 no C37 . C42 . C41 . 119.2(2) yes C37 . C42 . C45 . 123.92(18) yes C41 . C42 . C45 . 116.90(19) yes C38 . C43 . H431 . 111.9 no C38 . C43 . H432 . 110.8 no H431 . C43 . H432 . 106.8 no C38 . C43 . H433 . 111.6 no H431 . C43 . H433 . 108.1 no H432 . C43 . H433 . 107.4 no C40 . C44 . H441 . 107.8 no C40 . C44 . H442 . 109.5 no H441 . C44 . H442 . 109.8 no C40 . C44 . H443 . 109.3 no H441 . C44 . H443 . 109.1 no H442 . C44 . H443 . 111.2 no C42 . C45 . H451 . 109.8 no C42 . C45 . H452 . 110.9 no H451 . C45 . H452 . 107.9 no C42 . C45 . H453 . 110.6 no H451 . C45 . H453 . 109.0 no H452 . C45 . H453 . 108.7 no # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.025 0.250 0.165 1279 268 ' ' 2 -0.010 0.750 0.232 1279 268 ' ' _platon_squeeze_details ;During the structure solution, electron density difference maps revealed that there were considerable disordered solvent molecules (from history, likely pentane) in a volume of 2562.8 \%A3 per unit cell (22.3%); the peaks could not be modeled successfully. Areas of continuous electron density appeared in the ac plane (in the n-glide planes), creating bilayer arrangements at b = 1/4 and 3/4.Attempts at modeling the disordered pentane using restraints was unsuccessful, as was step by step acquisition of peaks using successive electron density difference maps. Thus, the structure factors were modified using the PLATON SQUEEZE technique, in order to produce a ?solvate-free? structure factor set. PLATON reported a total electron density of 536 e- per unit cell, likely representing twelve pentane molecules. Use of the SQUEEZE technique resulted in a decrease of ca. 1.6 % in R. ; #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 776340' #TrackingRef '- combined_rev.cif' _audit_creation_date 09-12-18 _audit_creation_method CRYSTALS_ver_14.01 _oxford_structure_analysis_title 'cmt31_0m in P-1' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 10.0365(4) _cell_length_b 15.6058(7) _cell_length_c 18.1449(8) _cell_angle_alpha 83.098(2) _cell_angle_beta 74.691(2) _cell_angle_gamma 85.221(2) _cell_volume 2717.3(2) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' Co 0.3494 0.9721 12.2841 4.2791 7.3409 0.2784 4.0034 13.5359 2.3488 71.1692 1.0118 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Zr -2.9673 0.5597 17.8765 1.2762 10.9480 11.9160 5.4173 0.1176 3.6572 87.6627 2.0693 'International Tables Vol C 4.2.6.8 and 6.1.1.4' I -0.4742 1.8119 20.1472 4.3470 18.9949 0.3814 7.5138 27.7660 2.2735 66.8776 4.0712 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C51.97 H83.95 Co1 I1.03 N3 P3 Zr1 # Dc = 1.37 Fooo = 1166.70 Mu = 12.06 M = 1124.68 # Found Formula = C51.97 H83.91 Co1 I1.03 N3 P3 Zr1 # Dc = 1.37 FOOO = 1166.70 Mu = 12.06 M = 1124.67 _chemical_formula_sum 'C51.97 H83.91 Co1 I1.03 N3 P3 Zr1' _chemical_formula_moiety 'C51.97 H83.91 Co1 I1.03 N3 P3 Zr1' _chemical_compound_source ? _chemical_formula_weight 1124.67 _cell_measurement_reflns_used 9314 _cell_measurement_theta_min 3 _cell_measurement_theta_max 30 _cell_measurement_temperature 120 _exptl_crystal_description 'prism fragment' _exptl_crystal_colour green _exptl_crystal_size_min 0.348 _exptl_crystal_size_mid 0.391 _exptl_crystal_size_max 0.610 _exptl_crystal_density_diffrn 1.374 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1166.702 _exptl_absorpt_coefficient_mu 1.206 # Sheldrick geometric approximatio 0.62 0.66 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Analytical Absorption (De Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_min 0.62 _exptl_absorpt_correction_T_max 0.66 _diffrn_measurement_device-type 'Bruker Kappa Apex2' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'Apex2 (Bruker AXS, 2006)' _computing_cell_refinement 'Apex2 (Bruker AXS, 2006)' _computing_data_reduction 'Apex2 (Bruker AXS, 2006)' _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 120 _diffrn_reflns_number 82444 _reflns_number_total 15766 _diffrn_reflns_av_R_equivalents 0.019 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 15766 # Theoretical number of reflections is about 31688 _diffrn_reflns_theta_min 2.107 _diffrn_reflns_theta_max 29.994 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 29.994 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _reflns_limit_h_min -13 _reflns_limit_h_max 14 _reflns_limit_k_min -21 _reflns_limit_k_max 21 _reflns_limit_l_min 0 _reflns_limit_l_max 25 _oxford_diffrn_Wilson_B_factor 1.35 _oxford_diffrn_Wilson_scale 62.19 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.71 _refine_diff_density_max 0.77 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 15766 _refine_ls_number_restraints 0 _refine_ls_number_parameters 567 _oxford_refine_ls_R_factor_ref 0.0196 _refine_ls_wR_factor_ref 0.0480 _refine_ls_goodness_of_fit_ref 1.0161 _refine_ls_shift/su_max 0.0032166 _refine_ls_shift/su_mean 0.0000755 # The values computed from all data _oxford_reflns_number_all 15766 _refine_ls_R_factor_all 0.0196 _refine_ls_wR_factor_all 0.0480 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 15133 _refine_ls_R_factor_gt 0.0185 _refine_ls_wR_factor_gt 0.0454 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment none # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.02P)^2^ + 1.44P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Bruker Analytical X-ray Systems, Inc., 2006. Apex2, Version 2 User Manual, M86-E01078, Madison, WI. De Meulenaer, J. & Tompa, H. (1965). Acta Cryst. 19, 1014. Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst. 40, 786-790. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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 _oxford_atom_site_special_shape _atom_site_attached_hydrogens I1 I 0.549215(8) 0.241985(6) 0.479152(4) 0.0239 1.0000 Uani . . . . . . . I2 I 0.5713(4) 0.2053(2) 0.2548(2) 0.0210(11) 0.0307(7) Uiso . . P 1 2 . . Zr1 Zr 0.302620(9) 0.258160(6) 0.261524(5) 0.0103 1.0000 Uani . . . . . . . Co1 Co 0.399145(14) 0.253878(9) 0.382409(8) 0.0132 1.0000 Uani . . . . . . . P1 P 0.32770(3) 0.392461(17) 0.353598(15) 0.0123 1.0000 Uani . . . . . . . P2 P 0.21955(3) 0.162899(18) 0.408227(15) 0.0140 1.0000 Uani . . . . . . . P3 P 0.22117(3) 0.273139(19) 0.129921(16) 0.0156 1.0000 Uani . . . . . . . N1 N 0.24888(9) 0.39174(6) 0.28188(5) 0.0123 1.0000 Uani . . . . . . . N2 N 0.18330(9) 0.15381(6) 0.32316(5) 0.0143 1.0000 Uani . . . . . . . N3 N 0.37793(9) 0.23831(6) 0.14238(5) 0.0148 1.0000 Uani . . . . . . . C1 C 0.46938(11) 0.46885(7) 0.32093(6) 0.0174 1.0000 Uani . . . . . . . C2 C 0.52125(13) 0.49775(9) 0.38598(7) 0.0237 1.0000 Uani . . . . . . . C3 C 0.59258(12) 0.42730(9) 0.26478(7) 0.0229 1.0000 Uani . . . . . . . C4 C 0.20318(11) 0.44048(7) 0.43556(6) 0.0153 1.0000 Uani . . . . . . . C5 C 0.24781(12) 0.42518(8) 0.51122(6) 0.0197 1.0000 Uani . . . . . . . C6 C 0.16182(12) 0.53652(7) 0.41916(7) 0.0194 1.0000 Uani . . . . . . . C7 C 0.16731(11) 0.46256(7) 0.25444(6) 0.0136 1.0000 Uani . . . . . . . C8 C 0.02303(11) 0.47091(7) 0.28671(6) 0.0152 1.0000 Uani . . . . . . . C9 C -0.05518(12) 0.53974(7) 0.25955(7) 0.0201 1.0000 Uani . . . . . . . C10 C 0.00339(13) 0.60107(8) 0.20043(8) 0.0230 1.0000 Uani . . . . . . . C11 C 0.14447(13) 0.59138(7) 0.16838(7) 0.0211 1.0000 Uani . . . . . . . C12 C 0.22752(11) 0.52439(7) 0.19413(6) 0.0162 1.0000 Uani . . . . . . . C13 C 0.37944(12) 0.52280(8) 0.15438(7) 0.0203 1.0000 Uani . . . . . . . C14 C -0.08313(16) 0.67537(10) 0.17273(10) 0.0384 1.0000 Uani . . . . . . . C15 C -0.05248(11) 0.41122(7) 0.35293(7) 0.0180 1.0000 Uani . . . . . . . C16 C 0.05397(12) 0.19681(7) 0.47467(6) 0.0185 1.0000 Uani . . . . . . . C17 C 0.06940(15) 0.23194(9) 0.54733(7) 0.0273 1.0000 Uani . . . . . . . C18 C -0.05657(12) 0.12981(8) 0.49435(7) 0.0231 1.0000 Uani . . . . . . . C19 C 0.27362(12) 0.05544(7) 0.44977(7) 0.0190 1.0000 Uani . . . . . . . C20 C 0.25126(13) 0.04842(9) 0.53714(7) 0.0256 1.0000 Uani . . . . . . . C21 C 0.42687(12) 0.03199(8) 0.41356(7) 0.0229 1.0000 Uani . . . . . . . C22 C 0.09188(11) 0.09674(7) 0.30591(6) 0.0157 1.0000 Uani . . . . . . . C23 C 0.13078(12) 0.00960(7) 0.29340(6) 0.0186 1.0000 Uani . . . . . . . C24 C 0.03930(14) -0.04042(8) 0.27288(7) 0.0241 1.0000 Uani . . . . . . . C25 C -0.08819(14) -0.00854(9) 0.26340(8) 0.0265 1.0000 Uani . . . . . . . C26 C -0.12448(12) 0.07765(9) 0.27460(7) 0.0243 1.0000 Uani . . . . . . . C27 C -0.03811(11) 0.13038(7) 0.29544(7) 0.0183 1.0000 Uani . . . . . . . C28 C 0.26721(13) -0.03478(8) 0.29875(7) 0.0229 1.0000 Uani . . . . . . . C29 C -0.18526(17) -0.06388(11) 0.24184(11) 0.0430 1.0000 Uani . . . . . . . C30 C -0.08795(12) 0.22231(8) 0.30722(7) 0.0208 1.0000 Uani . . . . . . . C31 C 0.14089(13) 0.18916(8) 0.09452(7) 0.0231 1.0000 Uani . . . . . . . C32 C -0.01168(15) 0.21360(11) 0.09865(9) 0.0340 1.0000 Uani . . . . . . . C33 C 0.21493(17) 0.16121(10) 0.01477(8) 0.0324 1.0000 Uani . . . . . . . C34 C 0.23540(13) 0.37206(8) 0.06148(7) 0.0204 1.0000 Uani . . . . . . . C35 C 0.09501(15) 0.42122(9) 0.06685(9) 0.0309 1.0000 Uani . . . . . . . C36 C 0.31355(16) 0.36399(9) -0.02251(7) 0.0290 1.0000 Uani . . . . . . . C37 C 0.49836(11) 0.20362(7) 0.09041(6) 0.0156 1.0000 Uani . . . . . . . C38 C 0.60664(11) 0.25669(7) 0.05040(6) 0.0165 1.0000 Uani . . . . . . . C39 C 0.72445(12) 0.22052(8) 0.00211(6) 0.0185 1.0000 Uani . . . . . . . C40 C 0.74110(12) 0.13315(8) -0.00778(7) 0.0212 1.0000 Uani . . . . . . . C41 C 0.63583(13) 0.08132(8) 0.03412(7) 0.0232 1.0000 Uani . . . . . . . C42 C 0.51579(13) 0.11432(7) 0.08326(6) 0.0201 1.0000 Uani . . . . . . . C43 C 0.60235(13) 0.35104(8) 0.06068(7) 0.0220 1.0000 Uani . . . . . . . C44 C 0.86979(14) 0.09611(9) -0.06068(8) 0.0308 1.0000 Uani . . . . . . . C45 C 0.41224(15) 0.05154(8) 0.12911(8) 0.0305 1.0000 Uani . . . . . . . C46 C 0.5258(2) 0.20883(9) 0.26948(9) 0.0183 0.9693(7) Uani . . P 1 1 . . C47 C 0.33261(17) 0.76110(9) 0.19261(8) 0.0309 1.0000 Uani . . . . . . . C48 C 0.30333(18) 0.72829(9) 0.26944(8) 0.0340 1.0000 Uani . . . . . . . C49 C 0.39894(19) 0.73243(10) 0.31110(9) 0.0380 1.0000 Uani . . . . . . . C50 C 0.52385(19) 0.76908(11) 0.27603(11) 0.0430 1.0000 Uani . . . . . . . C51 C 0.55329(17) 0.80125(11) 0.19930(10) 0.0404 1.0000 Uani . . . . . . . C52 C 0.45710(16) 0.79725(9) 0.15758(8) 0.0321 1.0000 Uani . . . . . . . H11 H 0.4327 0.5189 0.2952 0.0210 1.0000 Uiso R . . . . . . H21 H 0.4531 0.5336 0.4183 0.0349 1.0000 Uiso R . . . . . . H22 H 0.5464 0.4490 0.4170 0.0352 1.0000 Uiso R . . . . . . H23 H 0.6036 0.5309 0.3635 0.0367 1.0000 Uiso R . . . . . . H31 H 0.6567 0.4703 0.2389 0.0356 1.0000 Uiso R . . . . . . H32 H 0.6402 0.3824 0.2920 0.0339 1.0000 Uiso R . . . . . . H33 H 0.5638 0.4023 0.2263 0.0333 1.0000 Uiso R . . . . . . H41 H 0.1221 0.4072 0.4425 0.0187 1.0000 Uiso R . . . . . . H51 H 0.1658 0.4246 0.5547 0.0300 1.0000 Uiso R . . . . . . H52 H 0.3031 0.4712 0.5158 0.0302 1.0000 Uiso R . . . . . . H53 H 0.2991 0.3719 0.5163 0.0306 1.0000 Uiso R . . . . . . H61 H 0.1296 0.5480 0.3731 0.0296 1.0000 Uiso R . . . . . . H62 H 0.0886 0.5542 0.4612 0.0304 1.0000 Uiso R . . . . . . H63 H 0.2380 0.5715 0.4140 0.0298 1.0000 Uiso R . . . . . . H91 H -0.1509 0.5438 0.2833 0.0253 1.0000 Uiso R . . . . . . H111 H 0.1859 0.6303 0.1269 0.0260 1.0000 Uiso R . . . . . . H131 H 0.4227 0.4676 0.1639 0.0301 1.0000 Uiso R . . . . . . H132 H 0.3942 0.5343 0.0995 0.0307 1.0000 Uiso R . . . . . . H133 H 0.4279 0.5646 0.1708 0.0313 1.0000 Uiso R . . . . . . H141 H -0.0578 0.6879 0.1184 0.0594 1.0000 Uiso R . . . . . . H142 H -0.0718 0.7263 0.1925 0.0599 1.0000 Uiso R . . . . . . H143 H -0.1783 0.6653 0.1879 0.0585 1.0000 Uiso R . . . . . . H151 H -0.0796 0.4387 0.3995 0.0278 1.0000 Uiso R . . . . . . H152 H -0.1364 0.3937 0.3445 0.0273 1.0000 Uiso R . . . . . . H153 H 0.0041 0.3606 0.3619 0.0251 1.0000 Uiso R . . . . . . H161 H 0.0209 0.2454 0.4431 0.0229 1.0000 Uiso R . . . . . . H171 H 0.0699 0.1869 0.5873 0.0411 1.0000 Uiso R . . . . . . H172 H 0.1507 0.2636 0.5383 0.0428 1.0000 Uiso R . . . . . . H173 H -0.0066 0.2711 0.5651 0.0425 1.0000 Uiso R . . . . . . H181 H -0.1452 0.1542 0.5197 0.0355 1.0000 Uiso R . . . . . . H182 H -0.0334 0.0823 0.5293 0.0343 1.0000 Uiso R . . . . . . H183 H -0.0671 0.1065 0.4489 0.0340 1.0000 Uiso R . . . . . . H191 H 0.2161 0.0149 0.4379 0.0223 1.0000 Uiso R . . . . . . H201 H 0.2883 -0.0072 0.5540 0.0388 1.0000 Uiso R . . . . . . H202 H 0.2999 0.0921 0.5518 0.0382 1.0000 Uiso R . . . . . . H203 H 0.1553 0.0537 0.5655 0.0374 1.0000 Uiso R . . . . . . H211 H 0.4537 0.0461 0.3591 0.0330 1.0000 Uiso R . . . . . . H212 H 0.4469 -0.0296 0.4251 0.0354 1.0000 Uiso R . . . . . . H213 H 0.4836 0.0624 0.4356 0.0340 1.0000 Uiso R . . . . . . H241 H 0.0671 -0.0979 0.2640 0.0299 1.0000 Uiso R . . . . . . H261 H -0.2109 0.1019 0.2684 0.0305 1.0000 Uiso R . . . . . . H281 H 0.3352 0.0058 0.2933 0.0330 1.0000 Uiso R . . . . . . H282 H 0.2997 -0.0723 0.2593 0.0336 1.0000 Uiso R . . . . . . H283 H 0.2583 -0.0699 0.3474 0.0345 1.0000 Uiso R . . . . . . H291 H -0.2022 -0.0418 0.1951 0.0677 1.0000 Uiso R . . . . . . H292 H -0.1477 -0.1207 0.2348 0.0676 1.0000 Uiso R . . . . . . H293 H -0.2700 -0.0676 0.2779 0.0667 1.0000 Uiso R . . . . . . H301 H -0.1105 0.2328 0.3600 0.0309 1.0000 Uiso R . . . . . . H302 H -0.1692 0.2375 0.2902 0.0332 1.0000 Uiso R . . . . . . H303 H -0.0215 0.2628 0.2792 0.0301 1.0000 Uiso R . . . . . . H311 H 0.1434 0.1406 0.1327 0.0279 1.0000 Uiso R . . . . . . H321 H -0.0587 0.1644 0.0933 0.0516 1.0000 Uiso R . . . . . . H322 H -0.0189 0.2571 0.0562 0.0515 1.0000 Uiso R . . . . . . H323 H -0.0595 0.2377 0.1450 0.0503 1.0000 Uiso R . . . . . . H331 H 0.3155 0.1526 0.0083 0.0487 1.0000 Uiso R . . . . . . H332 H 0.1983 0.2034 -0.0256 0.0481 1.0000 Uiso R . . . . . . H333 H 0.1792 0.1088 0.0079 0.0481 1.0000 Uiso R . . . . . . H341 H 0.2878 0.4076 0.0825 0.0232 1.0000 Uiso R . . . . . . H351 H 0.1107 0.4788 0.0417 0.0459 1.0000 Uiso R . . . . . . H352 H 0.0456 0.4269 0.1187 0.0455 1.0000 Uiso R . . . . . . H353 H 0.0378 0.3942 0.0418 0.0457 1.0000 Uiso R . . . . . . H361 H 0.2560 0.3394 -0.0493 0.0430 1.0000 Uiso R . . . . . . H362 H 0.3362 0.4201 -0.0488 0.0434 1.0000 Uiso R . . . . . . H363 H 0.3978 0.3277 -0.0267 0.0435 1.0000 Uiso R . . . . . . H391 H 0.7971 0.2565 -0.0235 0.0220 1.0000 Uiso R . . . . . . H411 H 0.6445 0.0213 0.0302 0.0280 1.0000 Uiso R . . . . . . H431 H 0.5302 0.3829 0.0440 0.0367 1.0000 Uiso R . . . . . . H432 H 0.6858 0.3770 0.0312 0.0373 1.0000 Uiso R . . . . . . H433 H 0.5897 0.3598 0.1116 0.0377 1.0000 Uiso R . . . . . . H441 H 0.9128 0.0496 -0.0349 0.0497 1.0000 Uiso R . . . . . . H442 H 0.9352 0.1391 -0.0817 0.0488 1.0000 Uiso R . . . . . . H443 H 0.8485 0.0729 -0.1005 0.0494 1.0000 Uiso R . . . . . . H451 H 0.3568 0.0330 0.0992 0.0468 1.0000 Uiso R . . . . . . H452 H 0.4575 0.0015 0.1485 0.0467 1.0000 Uiso R . . . . . . H453 H 0.3514 0.0767 0.1711 0.0441 1.0000 Uiso R . . . . . . H461 H 0.5219(18) 0.1542(12) 0.2493(10) 0.029(4) 0.9693(7) Uiso . . P 1 1 . . H462 H 0.5749(19) 0.1987(12) 0.3096(11) 0.035(5) 0.9693(7) Uiso . . P 1 1 . . H463 H 0.5855(17) 0.2447(13) 0.2289(11) 0.022(4) 0.9693(7) Uiso . . P 1 1 . . H471 H 0.2647 0.7601 0.1650 0.0377 1.0000 Uiso R . . . . . . H481 H 0.2179 0.7027 0.2929 0.0418 1.0000 Uiso R . . . . . . H491 H 0.3801 0.7112 0.3622 0.0472 1.0000 Uiso R . . . . . . H501 H 0.5883 0.7726 0.3045 0.0524 1.0000 Uiso R . . . . . . H511 H 0.6384 0.8243 0.1744 0.0490 1.0000 Uiso R . . . . . . H521 H 0.4766 0.8190 0.1061 0.0390 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 I1 0.02301(4) 0.03227(4) 0.02066(4) -0.00465(3) -0.01391(3) 0.00508(3) Zr1 0.00974(4) 0.01129(4) 0.00981(4) -0.00128(3) -0.00273(3) -0.00001(3) Co1 0.01176(6) 0.01623(7) 0.01223(6) -0.00082(5) -0.00465(5) 0.00080(5) P1 0.01176(11) 0.01424(11) 0.01172(11) -0.00268(9) -0.00372(9) -0.00078(9) P2 0.01331(11) 0.01449(12) 0.01286(11) 0.00138(9) -0.00264(9) -0.00007(9) P3 0.01638(12) 0.01892(13) 0.01288(11) -0.00254(9) -0.00601(9) -0.00057(10) N1 0.0133(4) 0.0121(4) 0.0124(4) -0.0019(3) -0.0050(3) 0.0006(3) N2 0.0133(4) 0.0143(4) 0.0149(4) 0.0000(3) -0.0034(3) -0.0016(3) N3 0.0154(4) 0.0167(4) 0.0124(4) -0.0032(3) -0.0035(3) 0.0012(3) C1 0.0165(5) 0.0199(5) 0.0172(5) -0.0032(4) -0.0050(4) -0.0046(4) C2 0.0210(5) 0.0310(6) 0.0225(5) -0.0074(5) -0.0071(4) -0.0086(5) C3 0.0163(5) 0.0316(6) 0.0209(5) -0.0064(5) -0.0016(4) -0.0061(4) C4 0.0153(4) 0.0169(5) 0.0143(4) -0.0044(4) -0.0035(4) -0.0006(4) C5 0.0217(5) 0.0241(5) 0.0143(5) -0.0054(4) -0.0053(4) 0.0011(4) C6 0.0217(5) 0.0176(5) 0.0196(5) -0.0061(4) -0.0055(4) 0.0014(4) C7 0.0152(4) 0.0124(4) 0.0146(4) -0.0025(3) -0.0061(4) 0.0005(3) C8 0.0151(4) 0.0146(4) 0.0176(5) -0.0032(4) -0.0064(4) 0.0002(4) C9 0.0170(5) 0.0185(5) 0.0266(6) -0.0036(4) -0.0093(4) 0.0029(4) C10 0.0253(6) 0.0167(5) 0.0298(6) 0.0006(4) -0.0147(5) 0.0029(4) C11 0.0261(6) 0.0162(5) 0.0222(5) 0.0029(4) -0.0103(4) -0.0016(4) C12 0.0188(5) 0.0153(5) 0.0156(5) -0.0013(4) -0.0061(4) -0.0015(4) C13 0.0205(5) 0.0216(5) 0.0169(5) 0.0014(4) -0.0025(4) -0.0028(4) C14 0.0350(7) 0.0277(7) 0.0534(9) 0.0083(6) -0.0211(7) 0.0078(6) C15 0.0145(4) 0.0182(5) 0.0208(5) -0.0024(4) -0.0036(4) -0.0013(4) C16 0.0172(5) 0.0183(5) 0.0165(5) 0.0014(4) -0.0001(4) 0.0011(4) C17 0.0341(7) 0.0250(6) 0.0186(5) -0.0036(4) 0.0014(5) -0.0024(5) C18 0.0162(5) 0.0259(6) 0.0230(5) 0.0038(4) -0.0001(4) -0.0021(4) C19 0.0187(5) 0.0173(5) 0.0194(5) 0.0039(4) -0.0050(4) 0.0006(4) C20 0.0250(6) 0.0295(6) 0.0195(5) 0.0073(5) -0.0059(4) 0.0014(5) C21 0.0199(5) 0.0214(5) 0.0259(6) 0.0016(4) -0.0065(4) 0.0039(4) C22 0.0155(4) 0.0156(5) 0.0148(4) -0.0021(4) -0.0010(4) -0.0032(4) C23 0.0209(5) 0.0158(5) 0.0160(5) -0.0018(4) 0.0008(4) -0.0016(4) C24 0.0296(6) 0.0173(5) 0.0228(5) -0.0066(4) 0.0009(5) -0.0053(4) C25 0.0254(6) 0.0275(6) 0.0268(6) -0.0107(5) -0.0008(5) -0.0109(5) C26 0.0167(5) 0.0295(6) 0.0280(6) -0.0094(5) -0.0043(4) -0.0050(4) C27 0.0152(5) 0.0192(5) 0.0203(5) -0.0052(4) -0.0026(4) -0.0023(4) C28 0.0267(6) 0.0178(5) 0.0209(5) -0.0022(4) -0.0020(4) 0.0043(4) C29 0.0365(8) 0.0416(9) 0.0559(10) -0.0236(8) -0.0081(7) -0.0163(7) C30 0.0157(5) 0.0213(5) 0.0266(6) -0.0067(4) -0.0065(4) 0.0019(4) C31 0.0272(6) 0.0262(6) 0.0196(5) -0.0018(4) -0.0106(4) -0.0080(5) C32 0.0300(7) 0.0424(8) 0.0367(7) -0.0003(6) -0.0203(6) -0.0099(6) C33 0.0464(8) 0.0335(7) 0.0216(6) -0.0075(5) -0.0110(6) -0.0123(6) C34 0.0247(5) 0.0202(5) 0.0184(5) -0.0007(4) -0.0104(4) -0.0001(4) C35 0.0310(7) 0.0280(6) 0.0377(7) -0.0026(5) -0.0188(6) 0.0066(5) C36 0.0390(7) 0.0296(6) 0.0178(5) 0.0024(5) -0.0074(5) -0.0051(5) C37 0.0177(5) 0.0179(5) 0.0110(4) -0.0027(4) -0.0036(4) 0.0017(4) C38 0.0185(5) 0.0179(5) 0.0139(4) -0.0023(4) -0.0057(4) 0.0007(4) C39 0.0172(5) 0.0230(5) 0.0149(5) -0.0010(4) -0.0042(4) -0.0002(4) C40 0.0207(5) 0.0247(6) 0.0164(5) -0.0046(4) -0.0025(4) 0.0044(4) C41 0.0276(6) 0.0186(5) 0.0203(5) -0.0047(4) -0.0008(4) 0.0033(4) C42 0.0243(5) 0.0181(5) 0.0152(5) -0.0024(4) -0.0003(4) 0.0004(4) C43 0.0226(5) 0.0194(5) 0.0235(5) -0.0045(4) -0.0035(4) -0.0020(4) C44 0.0245(6) 0.0321(7) 0.0303(7) -0.0084(5) 0.0029(5) 0.0049(5) C45 0.0358(7) 0.0180(5) 0.0283(6) -0.0014(5) 0.0081(5) -0.0022(5) C46 0.0156(6) 0.0239(7) 0.0155(6) -0.0022(5) -0.0047(5) 0.0002(5) C47 0.0447(8) 0.0242(6) 0.0283(6) -0.0053(5) -0.0147(6) -0.0058(5) C48 0.0486(9) 0.0260(6) 0.0294(7) -0.0008(5) -0.0118(6) -0.0115(6) C49 0.0624(10) 0.0274(7) 0.0290(7) 0.0009(5) -0.0208(7) -0.0056(7) C50 0.0469(9) 0.0412(9) 0.0495(10) -0.0047(7) -0.0287(8) 0.0011(7) C51 0.0313(7) 0.0426(9) 0.0460(9) -0.0063(7) -0.0070(6) -0.0010(6) C52 0.0432(8) 0.0278(6) 0.0236(6) -0.0064(5) -0.0048(6) 0.0009(6) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.127061(13) 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 I1 . Co1 . 2.57987(18) yes I2 . Zr1 . 2.729(4) yes I2 . Co1 . 2.647(4) yes Zr1 . Co1 . 2.61347(19) yes Zr1 . P1 . 2.8981(3) yes Zr1 . P2 . 2.8415(3) yes Zr1 . P3 . 2.7000(3) yes Zr1 . N1 . 2.1600(9) yes Zr1 . N2 . 2.1253(9) yes Zr1 . N3 . 2.1448(9) yes Zr1 . C46 . 2.3430(18) yes Zr1 . Co1 . 2.61347(19) yes Zr1 . P1 . 2.8981(3) yes Zr1 . P2 . 2.8415(3) yes Zr1 . P3 . 2.7000(3) yes Zr1 . N1 . 2.1600(9) yes Zr1 . N2 . 2.1253(9) yes Zr1 . N3 . 2.1448(9) yes Co1 . P1 . 2.2655(3) yes Co1 . P2 . 2.3032(3) yes Co1 . C46 . 2.2653(19) yes Co1 . H462 . 2.095(19) no Co1 . P1 . 2.2655(3) yes Co1 . P2 . 2.3032(3) yes P1 . N1 . 1.6936(9) yes P1 . C1 . 1.8606(11) yes P1 . C4 . 1.8616(11) yes P2 . N2 . 1.7008(10) yes P2 . C16 . 1.8558(11) yes P2 . C19 . 1.8535(11) yes P3 . N3 . 1.6845(10) yes P3 . C31 . 1.8523(12) yes P3 . C34 . 1.8515(12) yes N1 . C7 . 1.4394(13) yes N2 . C22 . 1.4450(13) yes N3 . C37 . 1.4335(13) yes C1 . C2 . 1.5359(15) yes C1 . C3 . 1.5321(16) yes C1 . H11 . 0.958 no C2 . H21 . 0.963 no C2 . H22 . 0.948 no C2 . H23 . 0.979 no C3 . H31 . 0.959 no C3 . H32 . 0.975 no C3 . H33 . 0.957 no C4 . C5 . 1.5396(15) yes C4 . C6 . 1.5367(15) yes C4 . H41 . 0.973 no C5 . H51 . 0.978 no C5 . H52 . 0.967 no C5 . H53 . 0.949 no C6 . H61 . 0.966 no C6 . H62 . 0.958 no C6 . H63 . 0.955 no C7 . C8 . 1.4127(14) yes C7 . C12 . 1.4099(14) yes C8 . C9 . 1.3962(15) yes C8 . C15 . 1.5012(15) yes C9 . C10 . 1.3879(17) yes C9 . H91 . 0.944 no C10 . C11 . 1.3844(18) yes C10 . C14 . 1.5080(17) yes C11 . C12 . 1.3961(15) yes C11 . H111 . 0.936 no C12 . C13 . 1.5043(16) yes C13 . H131 . 0.950 no C13 . H132 . 0.965 no C13 . H133 . 0.963 no C14 . H141 . 0.952 no C14 . H142 . 0.937 no C14 . H143 . 0.943 no C15 . H151 . 0.959 no C15 . H152 . 0.961 no C15 . H153 . 0.958 no C16 . C17 . 1.5359(17) yes C16 . C18 . 1.5316(16) yes C16 . H161 . 0.984 no C17 . H171 . 0.949 no C17 . H172 . 0.956 no C17 . H173 . 0.948 no C18 . H181 . 0.958 no C18 . H182 . 0.970 no C18 . H183 . 0.973 no C19 . C20 . 1.5331(17) yes C19 . C21 . 1.5368(16) yes C19 . H191 . 0.969 no C20 . H201 . 0.963 no C20 . H202 . 0.970 no C20 . H203 . 0.967 no C21 . H211 . 0.956 no C21 . H212 . 0.974 no C21 . H213 . 0.960 no C22 . C23 . 1.4114(15) yes C22 . C27 . 1.4166(15) yes C23 . C24 . 1.4003(17) yes C23 . C28 . 1.5034(17) yes C24 . C25 . 1.380(2) yes C24 . H241 . 0.937 no C25 . C26 . 1.3885(18) yes C25 . C29 . 1.5069(18) yes C26 . C27 . 1.3922(16) yes C26 . H261 . 0.946 no C27 . C30 . 1.5006(16) yes C28 . H281 . 0.948 no C28 . H282 . 0.952 no C28 . H283 . 0.969 no C29 . H291 . 0.929 no C29 . H292 . 0.944 no C29 . H293 . 0.927 no C30 . H301 . 0.956 no C30 . H302 . 0.948 no C30 . H303 . 0.957 no C31 . C32 . 1.5313(19) yes C31 . C33 . 1.5382(18) yes C31 . H311 . 0.966 no C32 . H321 . 0.962 no C32 . H322 . 0.977 no C32 . H323 . 0.956 no C33 . H331 . 0.984 no C33 . H332 . 0.964 no C33 . H333 . 0.954 no C34 . C35 . 1.5326(17) yes C34 . C36 . 1.5336(17) yes C34 . H341 . 0.966 no C35 . H351 . 0.963 no C35 . H352 . 0.951 no C35 . H353 . 0.969 no C36 . H361 . 0.973 no C36 . H362 . 0.960 no C36 . H363 . 0.969 no C37 . C38 . 1.4082(15) yes C37 . C42 . 1.4073(15) yes C38 . C39 . 1.3947(15) yes C38 . C43 . 1.5020(16) yes C39 . C40 . 1.3871(17) yes C39 . H391 . 0.943 no C40 . C41 . 1.3852(17) yes C40 . C44 . 1.5092(17) yes C41 . C42 . 1.3970(16) yes C41 . H411 . 0.943 no C42 . C45 . 1.4998(17) yes C43 . H431 . 0.940 no C43 . H432 . 0.959 no C43 . H433 . 0.923 no C44 . H441 . 0.951 no C44 . H442 . 0.952 no C44 . H443 . 0.925 no C45 . H451 . 0.955 no C45 . H452 . 0.949 no C45 . H453 . 0.946 no C46 . H461 . 0.974(19) no C46 . H462 . 0.97(2) no C46 . H463 . 0.97(2) no C47 . C48 . 1.389(2) yes C47 . C52 . 1.377(2) yes C47 . H471 . 0.948 no C48 . C49 . 1.379(2) yes C48 . H481 . 0.948 no C49 . C50 . 1.384(3) yes C49 . H491 . 0.921 no C50 . C51 . 1.385(3) yes C50 . H501 . 0.937 no C51 . C52 . 1.384(2) yes C51 . H511 . 0.934 no C52 . H521 . 0.929 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 Zr1 . I2 . Co1 . 58.15(8) yes Co1 . Zr1 . P1 . 48.201(6) yes Co1 . Zr1 . P2 . 49.734(7) yes P1 . Zr1 . P2 . 82.142(9) yes Co1 . Zr1 . P3 . 174.628(8) yes P1 . Zr1 . P3 . 128.931(9) yes P2 . Zr1 . P3 . 135.637(9) yes Co1 . Zr1 . N1 . 83.41(2) yes P1 . Zr1 . N1 . 35.47(2) yes P2 . Zr1 . N1 . 105.15(2) yes P3 . Zr1 . N1 . 94.26(2) yes Co1 . Zr1 . N2 . 85.55(3) yes P1 . Zr1 . N2 . 114.85(3) yes P2 . Zr1 . N2 . 36.58(3) yes P3 . Zr1 . N2 . 99.76(3) yes N1 . Zr1 . N2 . 123.58(3) yes Co1 . Zr1 . N3 . 138.50(2) yes P1 . Zr1 . N3 . 134.57(3) yes P2 . Zr1 . N3 . 140.49(3) yes P3 . Zr1 . N3 . 38.59(3) yes N1 . Zr1 . N3 . 113.95(3) yes Co1 . Zr1 . C46 . 54.06(4) yes P1 . Zr1 . C46 . 86.23(3) yes P2 . Zr1 . C46 . 83.90(4) yes P3 . Zr1 . C46 . 123.36(4) yes N1 . Zr1 . C46 . 114.97(4) yes N2 . Zr1 . N3 . 110.58(4) yes N2 . Zr1 . C46 . 101.71(4) yes N3 . Zr1 . C46 . 84.77(5) yes I2 . Zr1 . Co1 . 59.36(8) yes I2 . Zr1 . P1 . 88.65(7) yes Co1 . Zr1 . P1 . 48.201(6) yes I2 . Zr1 . P2 . 89.57(8) yes Co1 . Zr1 . P2 . 49.734(7) yes P1 . Zr1 . P2 . 82.142(9) yes I2 . Zr1 . P3 . 117.83(8) yes Co1 . Zr1 . P3 . 174.628(8) yes P1 . Zr1 . P3 . 128.931(9) yes P2 . Zr1 . P3 . 135.637(9) yes I2 . Zr1 . N1 . 115.09(8) yes Co1 . Zr1 . N1 . 83.41(2) yes P1 . Zr1 . N1 . 35.47(2) yes P2 . Zr1 . N1 . 105.15(2) yes P3 . Zr1 . N1 . 94.26(2) yes I2 . Zr1 . N2 . 105.58(8) yes Co1 . Zr1 . N2 . 85.55(3) yes P1 . Zr1 . N2 . 114.85(3) yes P2 . Zr1 . N2 . 36.58(3) yes P3 . Zr1 . N2 . 99.76(3) yes I2 . Zr1 . N3 . 79.27(8) yes Co1 . Zr1 . N3 . 138.50(2) yes P1 . Zr1 . N3 . 134.57(3) yes P2 . Zr1 . N3 . 140.49(3) yes P3 . Zr1 . N3 . 38.59(3) yes N1 . Zr1 . N2 . 123.58(3) yes N1 . Zr1 . N3 . 113.95(3) yes N2 . Zr1 . N3 . 110.58(4) yes I1 . Co1 . Zr1 . 166.525(7) yes I1 . Co1 . P1 . 111.994(9) yes Zr1 . Co1 . P1 . 72.484(8) yes I1 . Co1 . P2 . 117.441(9) yes Zr1 . Co1 . P2 . 70.287(9) yes P1 . Co1 . P2 . 111.260(11) yes I1 . Co1 . C46 . 109.88(4) yes Zr1 . Co1 . C46 . 56.86(4) yes P1 . Co1 . C46 . 105.44(4) yes P2 . Co1 . C46 . 99.44(4) yes I1 . Co1 . H462 . 84.7(5) no Zr1 . Co1 . H462 . 82.2(5) no P1 . Co1 . H462 . 119.7(5) no P2 . Co1 . H462 . 109.8(5) no C46 . Co1 . H462 . 25.4(5) no I2 . Co1 . I1 . 104.15(8) yes I2 . Co1 . Zr1 . 62.49(8) yes I1 . Co1 . Zr1 . 166.525(7) yes I2 . Co1 . P1 . 106.12(8) yes I1 . Co1 . P1 . 111.994(9) yes Zr1 . Co1 . P1 . 72.484(8) yes I2 . Co1 . P2 . 104.69(8) yes I1 . Co1 . P2 . 117.441(9) yes Zr1 . Co1 . P2 . 70.287(9) yes P1 . Co1 . P2 . 111.260(11) yes Zr1 . P1 . Co1 . 59.315(8) yes Zr1 . P1 . N1 . 47.74(3) yes Co1 . P1 . N1 . 106.65(3) yes Zr1 . P1 . C1 . 121.50(4) yes Co1 . P1 . C1 . 114.39(4) yes N1 . P1 . C1 . 108.45(5) yes Zr1 . P1 . C4 . 132.01(3) yes Co1 . P1 . C4 . 113.77(4) yes N1 . P1 . C4 . 108.56(5) yes C1 . P1 . C4 . 104.84(5) yes Zr1 . P2 . Co1 . 59.978(8) yes Zr1 . P2 . N2 . 48.14(3) yes Co1 . P2 . N2 . 106.97(3) yes Zr1 . P2 . C16 . 118.27(4) yes Co1 . P2 . C16 . 117.46(4) yes N2 . P2 . C16 . 106.28(5) yes Zr1 . P2 . C19 . 133.73(4) yes Co1 . P2 . C19 . 109.56(4) yes N2 . P2 . C19 . 109.92(5) yes C16 . P2 . C19 . 106.51(5) yes Zr1 . P3 . N3 . 52.58(3) yes Zr1 . P3 . C31 . 126.35(4) yes N3 . P3 . C31 . 111.51(5) yes Zr1 . P3 . C34 . 124.17(4) yes N3 . P3 . C34 . 110.33(5) yes C31 . P3 . C34 . 109.47(5) yes P1 . N1 . Zr1 . 96.79(4) yes P1 . N1 . C7 . 125.75(7) yes Zr1 . N1 . C7 . 137.31(7) yes P2 . N2 . Zr1 . 95.27(4) yes P2 . N2 . C22 . 129.28(7) yes Zr1 . N2 . C22 . 135.28(7) yes P3 . N3 . Zr1 . 88.83(4) yes P3 . N3 . C37 . 131.01(7) yes Zr1 . N3 . C37 . 139.91(7) yes P1 . C1 . C2 . 114.43(8) yes P1 . C1 . C3 . 109.67(8) yes C2 . C1 . C3 . 108.19(9) yes P1 . C1 . H11 . 106.3 no C2 . C1 . H11 . 108.4 no C3 . C1 . H11 . 109.8 no C1 . C2 . H21 . 112.5 no C1 . C2 . H22 . 110.5 no H21 . C2 . H22 . 108.5 no C1 . C2 . H23 . 109.0 no H21 . C2 . H23 . 108.3 no H22 . C2 . H23 . 108.0 no C1 . C3 . H31 . 110.0 no C1 . C3 . H32 . 110.6 no H31 . C3 . H32 . 108.8 no C1 . C3 . H33 . 111.4 no H31 . C3 . H33 . 107.4 no H32 . C3 . H33 . 108.6 no P1 . C4 . C5 . 113.86(7) yes P1 . C4 . C6 . 114.66(8) yes C5 . C4 . C6 . 110.22(9) yes P1 . C4 . H41 . 102.0 no C5 . C4 . H41 . 107.0 no C6 . C4 . H41 . 108.3 no C4 . C5 . H51 . 109.6 no C4 . C5 . H52 . 111.1 no H51 . C5 . H52 . 107.3 no C4 . C5 . H53 . 113.0 no H51 . C5 . H53 . 107.5 no H52 . C5 . H53 . 108.2 no C4 . C6 . H61 . 112.4 no C4 . C6 . H62 . 109.5 no H61 . C6 . H62 . 107.8 no C4 . C6 . H63 . 110.7 no H61 . C6 . H63 . 108.5 no H62 . C6 . H63 . 107.8 no N1 . C7 . C8 . 120.42(9) yes N1 . C7 . C12 . 121.50(9) yes C8 . C7 . C12 . 118.08(9) yes C7 . C8 . C9 . 119.95(10) yes C7 . C8 . C15 . 123.18(9) yes C9 . C8 . C15 . 116.80(10) yes C8 . C9 . C10 . 122.32(11) yes C8 . C9 . H91 . 117.4 no C10 . C9 . H91 . 120.3 no C9 . C10 . C11 . 117.20(10) yes C9 . C10 . C14 . 121.28(12) yes C11 . C10 . C14 . 121.52(12) yes C10 . C11 . C12 . 122.69(11) yes C10 . C11 . H111 . 119.0 no C12 . C11 . H111 . 118.3 no C7 . C12 . C11 . 119.74(10) yes C7 . C12 . C13 . 123.55(10) yes C11 . C12 . C13 . 116.71(10) yes C12 . C13 . H131 . 110.9 no C12 . C13 . H132 . 111.0 no H131 . C13 . H132 . 106.9 no C12 . C13 . H133 . 112.8 no H131 . C13 . H133 . 107.4 no H132 . C13 . H133 . 107.5 no C10 . C14 . H141 . 112.8 no C10 . C14 . H142 . 110.8 no H141 . C14 . H142 . 105.7 no C10 . C14 . H143 . 112.3 no H141 . C14 . H143 . 107.7 no H142 . C14 . H143 . 107.3 no C8 . C15 . H151 . 111.5 no C8 . C15 . H152 . 111.7 no H151 . C15 . H152 . 106.0 no C8 . C15 . H153 . 111.4 no H151 . C15 . H153 . 107.4 no H152 . C15 . H153 . 108.7 no P2 . C16 . C17 . 114.62(9) yes P2 . C16 . C18 . 114.49(8) yes C17 . C16 . C18 . 111.24(10) yes P2 . C16 . H161 . 101.5 no C17 . C16 . H161 . 107.4 no C18 . C16 . H161 . 106.6 no C16 . C17 . H171 . 111.4 no C16 . C17 . H172 . 112.8 no H171 . C17 . H172 . 109.1 no C16 . C17 . H173 . 109.3 no H171 . C17 . H173 . 107.7 no H172 . C17 . H173 . 106.3 no C16 . C18 . H181 . 111.4 no C16 . C18 . H182 . 110.3 no H181 . C18 . H182 . 106.7 no C16 . C18 . H183 . 112.3 no H181 . C18 . H183 . 107.3 no H182 . C18 . H183 . 108.6 no P2 . C19 . C20 . 113.57(9) yes P2 . C19 . C21 . 111.26(8) yes C20 . C19 . C21 . 108.11(10) yes P2 . C19 . H191 . 105.4 no C20 . C19 . H191 . 108.5 no C21 . C19 . H191 . 109.8 no C19 . C20 . H201 . 108.9 no C19 . C20 . H202 . 111.0 no H201 . C20 . H202 . 107.5 no C19 . C20 . H203 . 114.1 no H201 . C20 . H203 . 107.3 no H202 . C20 . H203 . 107.7 no C19 . C21 . H211 . 113.3 no C19 . C21 . H212 . 109.9 no H211 . C21 . H212 . 108.8 no C19 . C21 . H213 . 109.4 no H211 . C21 . H213 . 107.9 no H212 . C21 . H213 . 107.3 no N2 . C22 . C23 . 122.54(10) yes N2 . C22 . C27 . 119.25(9) yes C23 . C22 . C27 . 118.05(10) yes C22 . C23 . C24 . 119.23(11) yes C22 . C23 . C28 . 124.69(10) yes C24 . C23 . C28 . 116.07(10) yes C23 . C24 . C25 . 123.16(11) yes C23 . C24 . H241 . 118.3 no C25 . C24 . H241 . 118.5 no C24 . C25 . C26 . 117.15(11) yes C24 . C25 . C29 . 122.15(13) yes C26 . C25 . C29 . 120.70(13) yes C25 . C26 . C27 . 122.25(12) yes C25 . C26 . H261 . 119.6 no C27 . C26 . H261 . 118.1 no C22 . C27 . C26 . 120.16(11) yes C22 . C27 . C30 . 121.78(10) yes C26 . C27 . C30 . 118.05(10) yes C23 . C28 . H281 . 111.3 no C23 . C28 . H282 . 110.4 no H281 . C28 . H282 . 108.0 no C23 . C28 . H283 . 111.0 no H281 . C28 . H283 . 108.8 no H282 . C28 . H283 . 107.2 no C25 . C29 . H291 . 110.6 no C25 . C29 . H292 . 112.4 no H291 . C29 . H292 . 105.3 no C25 . C29 . H293 . 112.8 no H291 . C29 . H293 . 107.5 no H292 . C29 . H293 . 107.8 no C27 . C30 . H301 . 112.6 no C27 . C30 . H302 . 111.5 no H301 . C30 . H302 . 106.3 no C27 . C30 . H303 . 112.5 no H301 . C30 . H303 . 107.6 no H302 . C30 . H303 . 106.0 no P3 . C31 . C32 . 111.29(10) yes P3 . C31 . C33 . 117.01(9) yes C32 . C31 . C33 . 109.96(11) yes P3 . C31 . H311 . 102.0 no C32 . C31 . H311 . 107.0 no C33 . C31 . H311 . 108.8 no C31 . C32 . H321 . 110.8 no C31 . C32 . H322 . 109.7 no H321 . C32 . H322 . 106.9 no C31 . C32 . H323 . 112.9 no H321 . C32 . H323 . 109.3 no H322 . C32 . H323 . 106.9 no C31 . C33 . H331 . 111.5 no C31 . C33 . H332 . 111.3 no H331 . C33 . H332 . 108.5 no C31 . C33 . H333 . 109.7 no H331 . C33 . H333 . 109.3 no H332 . C33 . H333 . 106.4 no P3 . C34 . C35 . 111.92(9) yes P3 . C34 . C36 . 117.95(9) yes C35 . C34 . C36 . 110.95(11) yes P3 . C34 . H341 . 101.7 no C35 . C34 . H341 . 105.5 no C36 . C34 . H341 . 107.6 no C34 . C35 . H351 . 108.6 no C34 . C35 . H352 . 111.8 no H351 . C35 . H352 . 106.9 no C34 . C35 . H353 . 112.2 no H351 . C35 . H353 . 107.9 no H352 . C35 . H353 . 109.2 no C34 . C36 . H361 . 110.7 no C34 . C36 . H362 . 110.1 no H361 . C36 . H362 . 106.8 no C34 . C36 . H363 . 111.9 no H361 . C36 . H363 . 108.2 no H362 . C36 . H363 . 109.0 no N3 . C37 . C38 . 120.85(10) yes N3 . C37 . C42 . 120.42(10) yes C38 . C37 . C42 . 118.52(10) yes C37 . C38 . C39 . 119.53(10) yes C37 . C38 . C43 . 121.96(10) yes C39 . C38 . C43 . 118.45(10) yes C38 . C39 . C40 . 122.64(11) yes C38 . C39 . H391 . 118.7 no C40 . C39 . H391 . 118.6 no C39 . C40 . C41 . 117.09(10) yes C39 . C40 . C44 . 121.30(11) yes C41 . C40 . C44 . 121.60(11) yes C40 . C41 . C42 . 122.51(11) yes C40 . C41 . H411 . 119.7 no C42 . C41 . H411 . 117.8 no C37 . C42 . C41 . 119.62(11) yes C37 . C42 . C45 . 122.43(10) yes C41 . C42 . C45 . 117.90(11) yes C38 . C43 . H431 . 112.6 no C38 . C43 . H432 . 111.3 no H431 . C43 . H432 . 105.7 no C38 . C43 . H433 . 111.6 no H431 . C43 . H433 . 106.7 no H432 . C43 . H433 . 108.6 no C40 . C44 . H441 . 111.7 no C40 . C44 . H442 . 111.2 no H441 . C44 . H442 . 108.6 no C40 . C44 . H443 . 110.9 no H441 . C44 . H443 . 105.3 no H442 . C44 . H443 . 108.9 no C42 . C45 . H451 . 112.2 no C42 . C45 . H452 . 110.6 no H451 . C45 . H452 . 107.4 no C42 . C45 . H453 . 110.9 no H451 . C45 . H453 . 107.2 no H452 . C45 . H453 . 108.3 no Co1 . C46 . Zr1 . 69.08(6) yes Co1 . C46 . H461 . 127.7(11) no Zr1 . C46 . H461 . 94.0(10) no Co1 . C46 . H462 . 67.5(11) no Zr1 . C46 . H462 . 136.3(11) no H461 . C46 . H462 . 109.0(15) no Co1 . C46 . H463 . 124.9(10) no Zr1 . C46 . H463 . 103.7(11) no H461 . C46 . H463 . 106.9(15) no H462 . C46 . H463 . 104.3(15) no C48 . C47 . C52 . 120.36(14) yes C48 . C47 . H471 . 119.3 no C52 . C47 . H471 . 120.3 no C47 . C48 . C49 . 119.91(15) yes C47 . C48 . H481 . 119.8 no C49 . C48 . H481 . 120.3 no C48 . C49 . C50 . 119.77(15) yes C48 . C49 . H491 . 120.5 no C50 . C49 . H491 . 119.7 no C49 . C50 . C51 . 120.26(15) yes C49 . C50 . H501 . 119.8 no C51 . C50 . H501 . 119.9 no C50 . C51 . C52 . 119.92(15) yes C50 . C51 . H511 . 121.3 no C52 . C51 . H511 . 118.8 no C51 . C52 . C47 . 119.78(14) yes C51 . C52 . H521 . 120.0 no C47 . C52 . H521 . 120.2 no C46 . H462 . Co1 . 87.1(12) no #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 776341' #TrackingRef '- combined_rev.cif' _audit_creation_date 10-01-26 _audit_creation_method CRYSTALS_ver_14.01 _oxford_structure_analysis_title 'cmt34_0m in P2(1)/n' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 12.6346(10) _cell_length_b 29.449(2) _cell_length_c 13.3675(10) _cell_angle_alpha 90 _cell_angle_beta 106.141(4) _cell_angle_gamma 90 _cell_volume 4777.7(6) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' Co 0.3494 0.9721 12.2841 4.2791 7.3409 0.2784 4.0034 13.5359 2.3488 71.1692 1.0118 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Zr -2.9673 0.5597 17.8765 1.2762 10.9480 11.9160 5.4173 0.1176 3.6572 87.6627 2.0693 'International Tables Vol C 4.2.6.8 and 6.1.1.4' I -0.4742 1.8119 20.1472 4.3470 18.9949 0.3814 7.5138 27.7660 2.2735 66.8776 4.0712 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C45 H74 Co1 I1 N3 P3 Zr1 # Dc = 1.43 Fooo = 2120.00 Mu = 13.45 M = 1027.08 # Found Formula = C45 H74 Co1 I1 N3 P3 Zr1 # Dc = 1.43 FOOO = 2120.00 Mu = 13.45 M = 1027.08 _chemical_formula_sum 'C45 H74 Co1 I1 N3 P3 Zr1' _chemical_formula_moiety 'C45 H74 Co1 I1 N3 P3 Zr1' _chemical_compound_source ? _chemical_formula_weight 1027.08 _cell_measurement_reflns_used 9455 _cell_measurement_theta_min 3 _cell_measurement_theta_max 30 _cell_measurement_temperature 120 _exptl_crystal_description 'acicular fragment' _exptl_crystal_colour yellow-green _exptl_crystal_size_min 0.064 _exptl_crystal_size_mid 0.156 _exptl_crystal_size_max 0.631 _exptl_crystal_density_diffrn 1.428 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 2120 _exptl_absorpt_coefficient_mu 1.345 # Sheldrick geometric approximatio 0.81 0.92 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Analytical Absorption (De Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_min 0.81 _exptl_absorpt_correction_T_max 0.92 _diffrn_measurement_device-type 'Bruker Kappa Apex2' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'Apex2 (Bruker AXS, 2006)' _computing_cell_refinement 'Apex2 (Bruker AXS, 2006)' _computing_data_reduction 'Apex2 (Bruker AXS, 2006)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 120 _diffrn_reflns_number 81515 _reflns_number_total 13879 _diffrn_reflns_av_R_equivalents 0.035 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 13879 # Theoretical number of reflections is about 27889 _diffrn_reflns_theta_min 2.669 _diffrn_reflns_theta_max 30.007 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.007 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 40 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _reflns_limit_h_min -17 _reflns_limit_h_max 17 _reflns_limit_k_min 0 _reflns_limit_k_max 41 _reflns_limit_l_min 0 _reflns_limit_l_max 18 _oxford_diffrn_Wilson_B_factor 1.36 _oxford_diffrn_Wilson_scale 134.48 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.66 _refine_diff_density_max 1.40 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 13879 _refine_ls_number_restraints 4 _refine_ls_number_parameters 495 _oxford_refine_ls_R_factor_ref 0.0417 _refine_ls_wR_factor_ref 0.0859 _refine_ls_goodness_of_fit_ref 1.0000 _refine_ls_shift/su_max 0.0020412 _refine_ls_shift/su_mean 4.0074372 # The values computed from all data _oxford_reflns_number_all 13879 _refine_ls_R_factor_all 0.0417 _refine_ls_wR_factor_all 0.0859 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 11309 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_gt 0.0819 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment none # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.01P)^2^ +16.15P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Bruker Analytical X-ray Systems, Inc., 2006. Apex2, Version 2 User Manual, M86-E01078, Madison, WI. De Meulenaer, J. & Tompa, H. (1965). Acta Cryst. 19, 1014. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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 _oxford_atom_site_special_shape _atom_site_attached_hydrogens I1 I 0.467845(16) 0.683020(8) 0.332795(16) 0.0282 1.0000 Uani . . . . . . . Zr1 Zr 0.795053(19) 0.648584(8) 0.195326(18) 0.0132 1.0000 Uani . . . . . . . Co1 Co 0.63220(3) 0.654455(12) 0.27311(3) 0.0162 1.0000 Uani . . . . . . . P1 P 0.60552(5) 0.59374(2) 0.15725(5) 0.0151 1.0000 Uani . . . . . . . P2 P 0.78969(6) 0.64356(2) 0.40694(5) 0.0168 1.0000 Uani . . . . . . . P3 P 0.93836(6) 0.67091(2) 0.08759(5) 0.0170 1.0000 Uani . . . . . . . N1 N 0.70512(17) 0.59683(8) 0.09532(17) 0.0156 1.0000 Uani . . . . . . . N2 N 0.89008(17) 0.63291(8) 0.35027(17) 0.0165 1.0000 Uani . . . . . . . N3 N 0.87344(18) 0.70480(8) 0.15074(17) 0.0169 1.0000 Uani . . . . . . . C1 C 0.6184(2) 0.53679(9) 0.2187(2) 0.0199 1.0000 Uani . . . . . . . C2 C 0.5551(3) 0.53144(11) 0.3016(2) 0.0288 1.0000 Uani . . . . . . . C3 C 0.5976(3) 0.49658(10) 0.1429(3) 0.0253 1.0000 Uani . . . . . . . C4 C 0.4677(2) 0.59609(10) 0.0604(2) 0.0194 1.0000 Uani . . . . . . . C5 C 0.4318(2) 0.64468(10) 0.0295(2) 0.0232 1.0000 Uani . . . . . . . C6 C 0.3776(2) 0.57356(11) 0.0991(3) 0.0293 1.0000 Uani . . . . . . . C7 C 0.7216(2) 0.57179(9) 0.0093(2) 0.0164 1.0000 Uani . . . . . . . C8 C 0.8049(2) 0.53832(9) 0.0270(2) 0.0182 1.0000 Uani . . . . . . . C9 C 0.8237(2) 0.51445(10) -0.0562(2) 0.0212 1.0000 Uani . . . . . . . C10 C 0.7632(2) 0.52242(10) -0.1589(2) 0.0213 1.0000 Uani . . . . . . . C11 C 0.6853(2) 0.55646(10) -0.1756(2) 0.0203 1.0000 Uani . . . . . . . C12 C 0.6645(2) 0.58208(9) -0.0947(2) 0.0180 1.0000 Uani . . . . . . . C13 C 0.8752(2) 0.52774(10) 0.1341(2) 0.0233 1.0000 Uani . . . . . . . C14 C 0.7819(3) 0.49476(11) -0.2471(2) 0.0284 1.0000 Uani . . . . . . . C15 C 0.5847(2) 0.62095(10) -0.1247(2) 0.0238 1.0000 Uani . . . . . . . C16 C 0.8337(3) 0.69211(11) 0.4964(2) 0.0268 1.0000 Uani . . . . . . . C17 C 0.8158(3) 0.73660(11) 0.4337(3) 0.0312 1.0000 Uani . . . . . . . C18 C 0.7779(3) 0.69567(13) 0.5830(3) 0.0366 1.0000 Uani . . . . . . . C19 C 0.7791(2) 0.59496(10) 0.4928(2) 0.0219 1.0000 Uani . . . . . . . C20 C 0.6752(3) 0.59505(13) 0.5306(2) 0.0309 1.0000 Uani . . . . . . . C21 C 0.8823(3) 0.58777(11) 0.5846(2) 0.0259 1.0000 Uani . . . . . . . C22 C 1.0037(2) 0.62049(10) 0.3944(2) 0.0179 1.0000 Uani . . . . . . . C23 C 1.0335(2) 0.57429(10) 0.4080(2) 0.0187 1.0000 Uani . . . . . . . C24 C 1.1448(2) 0.56251(10) 0.4419(2) 0.0220 1.0000 Uani . . . . . . . C25 C 1.2282(2) 0.59480(11) 0.4612(2) 0.0251 1.0000 Uani . . . . . . . C26 C 1.1975(2) 0.63987(11) 0.4475(2) 0.0243 1.0000 Uani . . . . . . . C27 C 1.0875(2) 0.65367(10) 0.4154(2) 0.0200 1.0000 Uani . . . . . . . C28 C 0.9501(2) 0.53645(10) 0.3870(2) 0.0214 1.0000 Uani . . . . . . . C29 C 1.3482(3) 0.58092(13) 0.4943(3) 0.0358 1.0000 Uani . . . . . . . C30 C 1.0644(2) 0.70381(10) 0.4034(2) 0.0239 1.0000 Uani . . . . . . . C31 C 1.0910(2) 0.67002(10) 0.1449(2) 0.0220 1.0000 Uani . . . . . . . C32 C 1.1283(3) 0.62136(11) 0.1719(3) 0.0282 1.0000 Uani . . . . . . . C33 C 1.1611(2) 0.69208(12) 0.0817(3) 0.0311 1.0000 Uani . . . . . . . C34 C 0.9153(2) 0.68866(11) -0.0496(2) 0.0231 1.0000 Uani . . . . . . . C35 C 0.9320(3) 0.64749(14) -0.1132(3) 0.0373 1.0000 Uani . . . . . . . C36 C 0.8018(3) 0.70962(13) -0.0924(3) 0.0322 1.0000 Uani . . . . . . . C37 C 0.8372(2) 0.74955(9) 0.1613(2) 0.0169 1.0000 Uani . . . . . . . C38 C 0.7297(2) 0.75119(9) 0.1740(2) 0.0185 1.0000 Uani D . . . . . . C39 C 0.6886(2) 0.79269(10) 0.1973(2) 0.0216 1.0000 Uani . . . . . . . C40 C 0.7505(2) 0.83242(10) 0.2058(2) 0.0231 1.0000 Uani . . . . . . . C41 C 0.8543(2) 0.82961(10) 0.1889(2) 0.0221 1.0000 Uani . . . . . . . C42 C 0.8989(2) 0.78926(10) 0.1657(2) 0.0194 1.0000 Uani . . . . . . . C43 C 0.6646(2) 0.70919(10) 0.1598(2) 0.0199 1.0000 Uani D . . . . . . C44 C 0.7044(3) 0.87723(11) 0.2291(3) 0.0316 1.0000 Uani . . . . . . . C45 C 1.0112(2) 0.78811(10) 0.1483(2) 0.0247 1.0000 Uani . . . . . . . H11 H 0.6958 0.5352 0.2584 0.0245 1.0000 Uiso . . . . . . . H21 H 0.5555 0.5605 0.3362 0.0425 1.0000 Uiso . . . . . . . H22 H 0.5904 0.5095 0.3527 0.0429 1.0000 Uiso . . . . . . . H23 H 0.4798 0.5230 0.2702 0.0429 1.0000 Uiso . . . . . . . H31 H 0.6213 0.4685 0.1802 0.0384 1.0000 Uiso . . . . . . . H32 H 0.5217 0.4943 0.1066 0.0373 1.0000 Uiso . . . . . . . H33 H 0.6377 0.5003 0.0924 0.0383 1.0000 Uiso . . . . . . . H41 H 0.4731 0.5793 -0.0011 0.0228 1.0000 Uiso . . . . . . . H51 H 0.3685 0.6453 -0.0273 0.0344 1.0000 Uiso . . . . . . . H52 H 0.4132 0.6596 0.0869 0.0342 1.0000 Uiso . . . . . . . H53 H 0.4866 0.6620 0.0104 0.0341 1.0000 Uiso . . . . . . . H61 H 0.3857 0.5406 0.1052 0.0426 1.0000 Uiso . . . . . . . H62 H 0.3069 0.5791 0.0513 0.0431 1.0000 Uiso . . . . . . . H63 H 0.3750 0.5856 0.1626 0.0443 1.0000 Uiso . . . . . . . H91 H 0.8788 0.4922 -0.0418 0.0253 1.0000 Uiso . . . . . . . H111 H 0.6436 0.5626 -0.2440 0.0242 1.0000 Uiso . . . . . . . H131 H 0.9096 0.5545 0.1679 0.0343 1.0000 Uiso . . . . . . . H132 H 0.8308 0.5148 0.1744 0.0350 1.0000 Uiso . . . . . . . H133 H 0.9290 0.5063 0.1310 0.0354 1.0000 Uiso . . . . . . . H141 H 0.7561 0.4646 -0.2451 0.0427 1.0000 Uiso . . . . . . . H142 H 0.7427 0.5076 -0.3113 0.0420 1.0000 Uiso . . . . . . . H143 H 0.8580 0.4943 -0.2436 0.0421 1.0000 Uiso . . . . . . . H151 H 0.5983 0.6432 -0.0712 0.0342 1.0000 Uiso . . . . . . . H152 H 0.5936 0.6353 -0.1853 0.0351 1.0000 Uiso . . . . . . . H153 H 0.5097 0.6105 -0.1384 0.0350 1.0000 Uiso . . . . . . . H161 H 0.9144 0.6893 0.5339 0.0325 1.0000 Uiso . . . . . . . H171 H 0.7402 0.7434 0.4082 0.0458 1.0000 Uiso . . . . . . . H172 H 0.8448 0.7350 0.3753 0.0460 1.0000 Uiso . . . . . . . H173 H 0.8503 0.7608 0.4770 0.0467 1.0000 Uiso . . . . . . . H181 H 0.7995 0.6704 0.6330 0.0528 1.0000 Uiso . . . . . . . H182 H 0.6971 0.6969 0.5536 0.0526 1.0000 Uiso . . . . . . . H183 H 0.8021 0.7246 0.6203 0.0529 1.0000 Uiso . . . . . . . H191 H 0.7715 0.5686 0.4467 0.0257 1.0000 Uiso . . . . . . . H201 H 0.6154 0.6089 0.4804 0.0452 1.0000 Uiso . . . . . . . H202 H 0.6544 0.5644 0.5441 0.0460 1.0000 Uiso . . . . . . . H203 H 0.6880 0.6137 0.5911 0.0464 1.0000 Uiso . . . . . . . H211 H 0.8846 0.6097 0.6368 0.0392 1.0000 Uiso . . . . . . . H212 H 0.8781 0.5583 0.6149 0.0388 1.0000 Uiso . . . . . . . H213 H 0.9500 0.5893 0.5644 0.0387 1.0000 Uiso . . . . . . . H241 H 1.1617 0.5315 0.4500 0.0272 1.0000 Uiso . . . . . . . H261 H 1.2523 0.6620 0.4608 0.0288 1.0000 Uiso . . . . . . . H281 H 0.9345 0.5270 0.4510 0.0318 1.0000 Uiso . . . . . . . H282 H 0.9763 0.5110 0.3556 0.0323 1.0000 Uiso . . . . . . . H283 H 0.8822 0.5452 0.3392 0.0314 1.0000 Uiso . . . . . . . H291 H 1.3918 0.6044 0.4787 0.0543 1.0000 Uiso . . . . . . . H292 H 1.3597 0.5543 0.4613 0.0549 1.0000 Uiso . . . . . . . H293 H 1.3696 0.5760 0.5653 0.0548 1.0000 Uiso . . . . . . . H301 H 1.0477 0.7156 0.4642 0.0354 1.0000 Uiso . . . . . . . H302 H 1.0033 0.7100 0.3438 0.0359 1.0000 Uiso . . . . . . . H303 H 1.1275 0.7188 0.3944 0.0359 1.0000 Uiso . . . . . . . H311 H 1.1034 0.6863 0.2117 0.0277 1.0000 Uiso . . . . . . . H321 H 1.0926 0.6083 0.2195 0.0421 1.0000 Uiso . . . . . . . H322 H 1.2054 0.6204 0.2064 0.0415 1.0000 Uiso . . . . . . . H323 H 1.1127 0.6031 0.1086 0.0419 1.0000 Uiso . . . . . . . H331 H 1.2361 0.6931 0.1242 0.0450 1.0000 Uiso . . . . . . . H332 H 1.1358 0.7221 0.0621 0.0458 1.0000 Uiso . . . . . . . H333 H 1.1549 0.6743 0.0200 0.0462 1.0000 Uiso . . . . . . . H341 H 0.9713 0.7106 -0.0519 0.0268 1.0000 Uiso . . . . . . . H351 H 0.8755 0.6263 -0.1169 0.0547 1.0000 Uiso . . . . . . . H352 H 0.9999 0.6334 -0.0830 0.0542 1.0000 Uiso . . . . . . . H353 H 0.9313 0.6577 -0.1799 0.0551 1.0000 Uiso . . . . . . . H361 H 0.7980 0.7363 -0.0522 0.0476 1.0000 Uiso . . . . . . . H362 H 0.7902 0.7188 -0.1645 0.0480 1.0000 Uiso . . . . . . . H363 H 0.7444 0.6884 -0.0886 0.0468 1.0000 Uiso . . . . . . . H391 H 0.6163 0.7937 0.2058 0.0262 1.0000 Uiso . . . . . . . H411 H 0.8962 0.8563 0.1925 0.0262 1.0000 Uiso . . . . . . . H431 H 0.600(2) 0.7152(5) 0.168(3) 0.024(9) 1.0000 Uiso D . . . . . . H432 H 0.657(3) 0.6984(9) 0.093(3) 0.037(11) 1.0000 Uiso D . . . . . . H441 H 0.7595 0.8949 0.2751 0.0476 1.0000 Uiso . . . . . . . H442 H 0.6444 0.8731 0.2578 0.0479 1.0000 Uiso . . . . . . . H443 H 0.6793 0.8936 0.1666 0.0477 1.0000 Uiso . . . . . . . H451 H 1.0395 0.8185 0.1515 0.0376 1.0000 Uiso . . . . . . . H452 H 1.0064 0.7750 0.0820 0.0366 1.0000 Uiso . . . . . . . H453 H 1.0591 0.7701 0.2024 0.0364 1.0000 Uiso . . . . . . . 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 I1 0.02264(9) 0.03612(11) 0.03039(10) -0.00433(8) 0.01485(7) 0.00543(8) Zr1 0.01196(10) 0.01420(11) 0.01374(11) -0.00035(9) 0.00426(8) -0.00053(8) Co1 0.01466(15) 0.01663(17) 0.01886(17) -0.00229(13) 0.00747(13) -0.00012(13) P1 0.0133(3) 0.0154(3) 0.0172(3) -0.0013(2) 0.0050(2) -0.0011(2) P2 0.0187(3) 0.0184(3) 0.0146(3) -0.0017(2) 0.0066(2) -0.0018(2) P3 0.0155(3) 0.0185(3) 0.0189(3) 0.0012(2) 0.0078(2) 0.0000(2) N1 0.0137(9) 0.0182(10) 0.0155(10) -0.0026(8) 0.0050(8) -0.0008(8) N2 0.013(1) 0.0215(11) 0.0143(10) 0.0005(8) 0.0032(8) -0.0015(8) N3 0.0151(10) 0.0174(11) 0.0186(10) 0.0008(8) 0.0053(8) -0.0005(8) C1 0.0198(12) 0.0178(12) 0.0221(13) 0.0005(10) 0.0057(10) -0.0021(10) C2 0.0332(16) 0.0281(16) 0.0268(15) 0.0026(12) 0.0114(12) -0.0067(12) C3 0.0265(14) 0.0172(13) 0.0327(16) -0.0019(11) 0.0089(12) -0.0018(11) C4 0.0134(11) 0.0211(13) 0.0235(13) -0.0020(10) 0.0049(10) -0.0010(9) C5 0.0174(12) 0.0241(14) 0.0264(14) -0.0026(11) 0.0033(10) 0.0030(10) C6 0.0170(13) 0.0314(16) 0.0399(18) 0.0003(13) 0.0087(12) -0.0035(11) C7 0.0157(11) 0.0176(12) 0.0168(11) -0.0019(9) 0.0063(9) -0.0026(9) C8 0.0159(11) 0.0206(13) 0.0186(12) -0.0005(10) 0.0056(9) -0.0001(10) C9 0.0206(12) 0.0213(13) 0.0236(13) -0.0024(11) 0.0095(10) 0.0012(10) C10 0.0251(13) 0.0215(13) 0.0205(13) -0.0037(10) 0.0115(11) -0.0053(11) C11 0.0220(13) 0.0231(13) 0.0158(12) 0.0003(10) 0.0054(10) -0.0045(10) C12 0.0158(11) 0.0193(12) 0.0189(12) 0.0017(10) 0.0049(9) -0.0021(9) C13 0.0195(12) 0.0275(15) 0.0217(13) -0.0012(11) 0.0037(10) 0.0069(11) C14 0.0387(17) 0.0272(15) 0.0239(14) -0.0050(12) 0.0163(13) 0.0012(13) C15 0.0245(14) 0.0252(14) 0.0216(13) 0.0052(11) 0.0062(11) 0.0052(11) C16 0.0380(17) 0.0234(14) 0.0194(13) -0.0034(11) 0.0086(12) -0.0050(12) C17 0.048(2) 0.0224(15) 0.0261(15) -0.0059(12) 0.0148(14) -0.0055(13) C18 0.049(2) 0.0335(18) 0.0301(17) -0.0036(14) 0.0165(15) 0.0056(15) C19 0.0241(13) 0.0256(14) 0.0181(12) 0.0019(10) 0.0095(10) -0.0024(11) C20 0.0281(15) 0.0444(19) 0.0241(15) 0.0025(13) 0.0136(12) -0.0060(14) C21 0.0314(15) 0.0288(15) 0.0178(13) 0.0039(11) 0.0075(11) 0.0026(12) C22 0.0151(11) 0.0259(14) 0.0125(11) 0.0010(10) 0.0036(9) -0.0004(10) C23 0.0178(12) 0.0252(13) 0.0137(11) -0.0001(10) 0.0053(9) -0.0016(10) C24 0.0201(13) 0.0277(15) 0.0181(12) 0.0026(11) 0.0050(10) 0.0031(11) C25 0.0175(12) 0.0368(17) 0.0202(13) 0.0010(12) 0.0042(10) 0.0004(11) C26 0.0166(12) 0.0352(16) 0.0202(13) -0.0010(11) 0.0035(10) -0.0048(11) C27 0.0177(12) 0.0264(14) 0.0151(11) -0.0004(10) 0.0034(9) -0.0033(10) C28 0.0222(13) 0.0203(13) 0.0207(13) 0.0019(10) 0.0041(10) -0.0008(10) C29 0.0192(14) 0.045(2) 0.0413(19) 0.0007(16) 0.0056(13) 0.0043(13) C30 0.0214(13) 0.0267(14) 0.0221(13) -0.0020(11) 0.0037(10) -0.0071(11) C31 0.0154(12) 0.0260(14) 0.0262(14) 0.0013(11) 0.0086(10) 0.0001(10) C32 0.0244(14) 0.0296(16) 0.0337(16) 0.0053(13) 0.0131(12) 0.0076(12) C33 0.0183(13) 0.0353(17) 0.0429(18) 0.0082(14) 0.0138(13) 0.0005(12) C34 0.0229(13) 0.0288(15) 0.0193(13) 0.0014(11) 0.0086(10) -0.0026(11) C35 0.045(2) 0.044(2) 0.0263(16) -0.0090(15) 0.0157(14) 0.0000(16) C36 0.0254(15) 0.046(2) 0.0237(15) 0.0089(14) 0.0049(12) 0.0018(14) C37 0.0180(12) 0.0167(12) 0.0164(11) 0.0014(9) 0.0057(9) 0.0003(9) C38 0.0184(12) 0.0178(12) 0.0189(12) 0.0018(10) 0.0047(10) 0.0011(10) C39 0.0213(13) 0.0200(13) 0.0239(13) -0.0002(11) 0.0069(10) 0.0026(10) C40 0.0274(14) 0.0180(13) 0.0217(13) -0.0007(10) 0.0033(11) 0.0020(11) C41 0.0247(13) 0.0185(13) 0.0215(13) -0.0001(10) 0.0041(10) -0.0034(10) C42 0.0192(12) 0.0215(13) 0.0169(12) 0.0020(10) 0.0040(9) -0.0025(10) C43 0.0109(11) 0.0319(15) 0.0178(12) 0.0018(11) 0.0054(9) 0.0005(10) C44 0.0360(17) 0.0194(14) 0.0403(18) -0.0032(13) 0.0119(14) 0.0038(12) C45 0.0228(13) 0.0228(14) 0.0294(15) -0.0010(11) 0.0087(11) -0.0062(11) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.067419(6) 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 I1 . Co1 . 2.5647(4) yes Zr1 . Co1 . 2.5562(4) yes Zr1 . P1 . 2.8151(7) yes Zr1 . P2 . 2.8522(7) yes Zr1 . P3 . 2.6897(7) yes Zr1 . N1 . 2.135(2) yes Zr1 . N2 . 2.136(2) yes Zr1 . N3 . 2.099(2) yes Zr1 . C43 . 2.386(3) yes Co1 . P1 . 2.3279(8) yes Co1 . P2 . 2.2986(8) yes Co1 . C43 . 2.325(3) yes P1 . N1 . 1.690(2) yes P1 . C1 . 1.855(3) yes P1 . C4 . 1.860(3) yes P2 . N2 . 1.678(2) yes P2 . C16 . 1.848(3) yes P2 . C19 . 1.862(3) yes P3 . N3 . 1.663(2) yes P3 . C31 . 1.867(3) yes P3 . C34 . 1.850(3) yes N1 . C7 . 1.430(3) yes N2 . C22 . 1.439(3) yes N3 . C37 . 1.415(3) yes C1 . C2 . 1.545(4) yes C1 . C3 . 1.533(4) yes C1 . H11 . 0.975 no C2 . H21 . 0.973 no C2 . H22 . 0.956 no C2 . H23 . 0.960 no C3 . H31 . 0.970 no C3 . H32 . 0.949 no C3 . H33 . 0.956 no C4 . C5 . 1.523(4) yes C4 . C6 . 1.526(4) yes C4 . H41 . 0.978 no C5 . H51 . 0.938 no C5 . H52 . 0.968 no C5 . H53 . 0.951 no C6 . H61 . 0.976 no C6 . H62 . 0.957 no C6 . H63 . 0.930 no C7 . C8 . 1.413(4) yes C7 . C12 . 1.410(4) yes C8 . C9 . 1.391(4) yes C8 . C13 . 1.493(4) yes C9 . C10 . 1.394(4) yes C9 . H91 . 0.935 no C10 . C11 . 1.379(4) yes C10 . C14 . 1.504(4) yes C11 . C12 . 1.402(4) yes C11 . H111 . 0.937 no C12 . C15 . 1.505(4) yes C13 . H131 . 0.951 no C13 . H132 . 0.958 no C13 . H133 . 0.938 no C14 . H141 . 0.950 no C14 . H142 . 0.943 no C14 . H143 . 0.949 no C15 . H151 . 0.949 no C15 . H152 . 0.949 no C15 . H153 . 0.964 no C16 . C17 . 1.538(5) yes C16 . C18 . 1.517(5) yes C16 . H161 . 1.006 no C17 . H171 . 0.942 no C17 . H172 . 0.952 no C17 . H173 . 0.946 no C18 . H181 . 0.987 no C18 . H182 . 0.987 no C18 . H183 . 0.991 no C19 . C20 . 1.533(4) yes C19 . C21 . 1.537(4) yes C19 . H191 . 0.979 no C20 . H201 . 0.952 no C20 . H202 . 0.971 no C20 . H203 . 0.953 no C21 . H211 . 0.945 no C21 . H212 . 0.964 no C21 . H213 . 0.966 no C22 . C23 . 1.410(4) yes C22 . C27 . 1.411(4) yes C23 . C24 . 1.396(4) yes C23 . C28 . 1.505(4) yes C24 . C25 . 1.390(4) yes C24 . H241 . 0.936 no C25 . C26 . 1.380(5) yes C25 . C29 . 1.513(4) yes C26 . C27 . 1.396(4) yes C26 . H261 . 0.931 no C27 . C30 . 1.505(4) yes C28 . H281 . 0.972 no C28 . H282 . 0.962 no C28 . H283 . 0.951 no C29 . H291 . 0.943 no C29 . H292 . 0.930 no C29 . H293 . 0.924 no C30 . H301 . 0.960 no C30 . H302 . 0.960 no C30 . H303 . 0.947 no C31 . C32 . 1.520(4) yes C31 . C33 . 1.528(4) yes C31 . H311 . 0.987 no C32 . H321 . 0.957 no C32 . H322 . 0.956 no C32 . H323 . 0.974 no C33 . H331 . 0.960 no C33 . H332 . 0.952 no C33 . H333 . 0.962 no C34 . C35 . 1.529(5) yes C34 . C36 . 1.519(4) yes C34 . H341 . 0.964 no C35 . H351 . 0.939 no C35 . H352 . 0.938 no C35 . H353 . 0.938 no C36 . H361 . 0.961 no C36 . H362 . 0.972 no C36 . H363 . 0.970 no C37 . C38 . 1.415(4) yes C37 . C42 . 1.398(4) yes C38 . C39 . 1.397(4) yes C38 . C43 . 1.468(4) yes C39 . C40 . 1.395(4) yes C39 . H391 . 0.951 no C40 . C41 . 1.394(4) yes C40 . C44 . 1.510(4) yes C41 . C42 . 1.387(4) yes C41 . H411 . 0.941 no C42 . C45 . 1.500(4) yes C43 . H431 . 0.87(2) no C43 . H432 . 0.92(3) no C44 . H441 . 0.946 no C44 . H442 . 0.948 no C44 . H443 . 0.941 no C45 . H451 . 0.960 no C45 . H452 . 0.954 no C45 . H453 . 0.963 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 Co1 . Zr1 . P1 . 51.089(17) yes Co1 . Zr1 . P2 . 49.934(17) yes P1 . Zr1 . P2 . 84.03(2) yes Co1 . Zr1 . P3 . 159.89(2) yes P1 . Zr1 . P3 . 135.14(2) yes P2 . Zr1 . P3 . 138.49(2) yes Co1 . Zr1 . N1 . 87.39(6) yes P1 . Zr1 . N1 . 36.79(6) yes P2 . Zr1 . N1 . 115.39(6) yes P3 . Zr1 . N1 . 99.18(6) yes Co1 . Zr1 . N2 . 85.37(6) yes P1 . Zr1 . N2 . 105.78(6) yes P2 . Zr1 . N2 . 35.80(6) yes P3 . Zr1 . N2 . 106.94(6) yes N1 . Zr1 . N2 . 120.72(9) yes Co1 . Zr1 . N3 . 123.98(6) yes P1 . Zr1 . N3 . 147.79(6) yes P2 . Zr1 . N3 . 117.76(6) yes P3 . Zr1 . N3 . 38.20(6) yes N1 . Zr1 . N3 . 126.61(9) yes Co1 . Zr1 . C43 . 56.01(6) yes P1 . Zr1 . C43 . 83.53(7) yes P2 . Zr1 . C43 . 91.77(7) yes P3 . Zr1 . C43 . 103.95(7) yes N1 . Zr1 . C43 . 101.03(9) yes N2 . Zr1 . N3 . 105.27(9) yes N2 . Zr1 . C43 . 121.73(9) yes N3 . Zr1 . C43 . 73.00(9) yes I1 . Co1 . Zr1 . 164.080(18) yes I1 . Co1 . P1 . 118.61(2) yes Zr1 . Co1 . P1 . 70.21(2) yes I1 . Co1 . P2 . 113.84(2) yes Zr1 . Co1 . P2 . 71.74(2) yes P1 . Co1 . P2 . 110.15(3) yes I1 . Co1 . C43 . 106.24(7) yes Zr1 . Co1 . C43 . 58.29(7) yes P1 . Co1 . C43 . 96.78(8) yes P2 . Co1 . C43 . 109.44(7) yes Zr1 . P1 . Co1 . 58.696(18) yes Zr1 . P1 . N1 . 49.14(8) yes Co1 . P1 . N1 . 107.14(8) yes Zr1 . P1 . C1 . 118.24(9) yes Co1 . P1 . C1 . 114.92(9) yes N1 . P1 . C1 . 106.26(12) yes Zr1 . P1 . C4 . 133.56(9) yes Co1 . P1 . C4 . 111.65(9) yes N1 . P1 . C4 . 109.72(12) yes C1 . P1 . C4 . 106.98(13) yes Zr1 . P2 . Co1 . 58.328(18) yes Zr1 . P2 . N2 . 48.13(8) yes Co1 . P2 . N2 . 105.91(8) yes Zr1 . P2 . C16 . 121.06(10) yes Co1 . P2 . C16 . 115.82(11) yes N2 . P2 . C16 . 107.91(13) yes Zr1 . P2 . C19 . 132.56(9) yes Co1 . P2 . C19 . 113.09(10) yes N2 . P2 . C19 . 109.09(12) yes C16 . P2 . C19 . 104.84(13) yes Zr1 . P3 . N3 . 51.29(8) yes Zr1 . P3 . C31 . 123.32(9) yes N3 . P3 . C31 . 113.53(12) yes Zr1 . P3 . C34 . 130.98(9) yes N3 . P3 . C34 . 111.68(13) yes C31 . P3 . C34 . 105.69(13) yes P1 . N1 . Zr1 . 94.07(10) yes P1 . N1 . C7 . 131.39(18) yes Zr1 . N1 . C7 . 134.51(17) yes P2 . N2 . Zr1 . 96.07(10) yes P2 . N2 . C22 . 130.96(18) yes Zr1 . N2 . C22 . 132.84(17) yes P3 . N3 . Zr1 . 90.52(10) yes P3 . N3 . C37 . 145.95(19) yes Zr1 . N3 . C37 . 120.98(16) yes P1 . C1 . C2 . 114.2(2) yes P1 . C1 . C3 . 115.3(2) yes C2 . C1 . C3 . 111.6(2) yes P1 . C1 . H11 . 103.7 no C2 . C1 . H11 . 104.2 no C3 . C1 . H11 . 106.5 no C1 . C2 . H21 . 108.4 no C1 . C2 . H22 . 110.5 no H21 . C2 . H22 . 108.4 no C1 . C2 . H23 . 111.2 no H21 . C2 . H23 . 108.1 no H22 . C2 . H23 . 110.2 no C1 . C3 . H31 . 110.3 no C1 . C3 . H32 . 110.8 no H31 . C3 . H32 . 109.0 no C1 . C3 . H33 . 110.5 no H31 . C3 . H33 . 108.3 no H32 . C3 . H33 . 107.9 no P1 . C4 . C5 . 111.98(19) yes P1 . C4 . C6 . 112.9(2) yes C5 . C4 . C6 . 107.9(2) yes P1 . C4 . H41 . 107.2 no C5 . C4 . H41 . 109.4 no C6 . C4 . H41 . 107.3 no C4 . C5 . H51 . 111.2 no C4 . C5 . H52 . 109.3 no H51 . C5 . H52 . 106.9 no C4 . C5 . H53 . 113.2 no H51 . C5 . H53 . 107.1 no H52 . C5 . H53 . 109.0 no C4 . C6 . H61 . 112.9 no C4 . C6 . H62 . 110.2 no H61 . C6 . H62 . 106.4 no C4 . C6 . H63 . 111.3 no H61 . C6 . H63 . 109.5 no H62 . C6 . H63 . 106.2 no N1 . C7 . C8 . 119.6(2) yes N1 . C7 . C12 . 122.3(2) yes C8 . C7 . C12 . 117.9(2) yes C7 . C8 . C9 . 120.2(2) yes C7 . C8 . C13 . 121.5(2) yes C9 . C8 . C13 . 118.3(2) yes C8 . C9 . C10 . 122.3(3) yes C8 . C9 . H91 . 118.2 no C10 . C9 . H91 . 119.6 no C9 . C10 . C11 . 117.0(3) yes C9 . C10 . C14 . 121.2(3) yes C11 . C10 . C14 . 121.8(3) yes C10 . C11 . C12 . 123.0(3) yes C10 . C11 . H111 . 118.8 no C12 . C11 . H111 . 118.2 no C7 . C12 . C11 . 119.4(2) yes C7 . C12 . C15 . 123.2(2) yes C11 . C12 . C15 . 117.4(2) yes C8 . C13 . H131 . 110.7 no C8 . C13 . H132 . 109.8 no H131 . C13 . H132 . 109.0 no C8 . C13 . H133 . 110.0 no H131 . C13 . H133 . 109.7 no H132 . C13 . H133 . 107.6 no C10 . C14 . H141 . 110.8 no C10 . C14 . H142 . 109.9 no H141 . C14 . H142 . 107.6 no C10 . C14 . H143 . 110.3 no H141 . C14 . H143 . 109.6 no H142 . C14 . H143 . 108.6 no C12 . C15 . H151 . 110.9 no C12 . C15 . H152 . 109.7 no H151 . C15 . H152 . 107.2 no C12 . C15 . H153 . 111.0 no H151 . C15 . H153 . 109.1 no H152 . C15 . H153 . 108.9 no P2 . C16 . C17 . 109.5(2) yes P2 . C16 . C18 . 115.3(2) yes C17 . C16 . C18 . 109.1(3) yes P2 . C16 . H161 . 109.8 no C17 . C16 . H161 . 108.5 no C18 . C16 . H161 . 104.3 no C16 . C17 . H171 . 111.1 no C16 . C17 . H172 . 112.0 no H171 . C17 . H172 . 107.2 no C16 . C17 . H173 . 109.7 no H171 . C17 . H173 . 108.0 no H172 . C17 . H173 . 108.7 no C16 . C18 . H181 . 111.4 no C16 . C18 . H182 . 110.3 no H181 . C18 . H182 . 110.9 no C16 . C18 . H183 . 107.4 no H181 . C18 . H183 . 108.7 no H182 . C18 . H183 . 108.1 no P2 . C19 . C20 . 114.6(2) yes P2 . C19 . C21 . 114.1(2) yes C20 . C19 . C21 . 110.5(2) yes P2 . C19 . H191 . 103.5 no C20 . C19 . H191 . 105.3 no C21 . C19 . H191 . 107.9 no C19 . C20 . H201 . 110.7 no C19 . C20 . H202 . 111.2 no H201 . C20 . H202 . 109.0 no C19 . C20 . H203 . 108.8 no H201 . C20 . H203 . 105.5 no H202 . C20 . H203 . 111.6 no C19 . C21 . H211 . 109.9 no C19 . C21 . H212 . 109.0 no H211 . C21 . H212 . 107.4 no C19 . C21 . H213 . 112.9 no H211 . C21 . H213 . 109.1 no H212 . C21 . H213 . 108.4 no N2 . C22 . C23 . 119.9(2) yes N2 . C22 . C27 . 120.9(2) yes C23 . C22 . C27 . 118.9(2) yes C22 . C23 . C24 . 119.4(3) yes C22 . C23 . C28 . 122.8(2) yes C24 . C23 . C28 . 117.8(3) yes C23 . C24 . C25 . 122.3(3) yes C23 . C24 . H241 . 117.2 no C25 . C24 . H241 . 120.5 no C24 . C25 . C26 . 117.6(3) yes C24 . C25 . C29 . 121.1(3) yes C26 . C25 . C29 . 121.3(3) yes C25 . C26 . C27 . 122.6(3) yes C25 . C26 . H261 . 118.8 no C27 . C26 . H261 . 118.6 no C22 . C27 . C26 . 119.2(3) yes C22 . C27 . C30 . 123.1(2) yes C26 . C27 . C30 . 117.7(3) yes C23 . C28 . H281 . 110.5 no C23 . C28 . H282 . 110.6 no H281 . C28 . H282 . 109.8 no C23 . C28 . H283 . 112.3 no H281 . C28 . H283 . 107.6 no H282 . C28 . H283 . 105.9 no C25 . C29 . H291 . 109.7 no C25 . C29 . H292 . 111.4 no H291 . C29 . H292 . 109.6 no C25 . C29 . H293 . 109.0 no H291 . C29 . H293 . 108.7 no H292 . C29 . H293 . 108.4 no C27 . C30 . H301 . 110.3 no C27 . C30 . H302 . 111.2 no H301 . C30 . H302 . 108.6 no C27 . C30 . H303 . 109.0 no H301 . C30 . H303 . 109.2 no H302 . C30 . H303 . 108.5 no P3 . C31 . C32 . 109.1(2) yes P3 . C31 . C33 . 117.3(2) yes C32 . C31 . C33 . 110.1(2) yes P3 . C31 . H311 . 104.5 no C32 . C31 . H311 . 106.4 no C33 . C31 . H311 . 108.8 no C31 . C32 . H321 . 111.3 no C31 . C32 . H322 . 110.5 no H321 . C32 . H322 . 105.8 no C31 . C32 . H323 . 109.8 no H321 . C32 . H323 . 109.8 no H322 . C32 . H323 . 109.6 no C31 . C33 . H331 . 108.3 no C31 . C33 . H332 . 110.2 no H331 . C33 . H332 . 109.5 no C31 . C33 . H333 . 108.7 no H331 . C33 . H333 . 110.8 no H332 . C33 . H333 . 109.3 no P3 . C34 . C35 . 108.6(2) yes P3 . C34 . C36 . 111.1(2) yes C35 . C34 . C36 . 112.0(3) yes P3 . C34 . H341 . 107.9 no C35 . C34 . H341 . 107.2 no C36 . C34 . H341 . 109.9 no C34 . C35 . H351 . 109.6 no C34 . C35 . H352 . 111.2 no H351 . C35 . H352 . 108.6 no C34 . C35 . H353 . 108.0 no H351 . C35 . H353 . 110.9 no H352 . C35 . H353 . 108.5 no C34 . C36 . H361 . 108.1 no C34 . C36 . H362 . 110.7 no H361 . C36 . H362 . 108.0 no C34 . C36 . H363 . 111.2 no H361 . C36 . H363 . 110.0 no H362 . C36 . H363 . 108.7 no N3 . C37 . C38 . 113.1(2) yes N3 . C37 . C42 . 126.2(2) yes C38 . C37 . C42 . 120.6(2) yes C37 . C38 . C39 . 119.1(2) yes C37 . C38 . C43 . 118.5(2) yes C39 . C38 . C43 . 122.4(2) yes C38 . C39 . C40 . 121.1(3) yes C38 . C39 . H391 . 118.9 no C40 . C39 . H391 . 119.9 no C39 . C40 . C41 . 118.0(3) yes C39 . C40 . C44 . 120.7(3) yes C41 . C40 . C44 . 121.3(3) yes C40 . C41 . C42 . 123.1(3) yes C40 . C41 . H411 . 118.9 no C42 . C41 . H411 . 118.0 no C37 . C42 . C41 . 118.0(2) yes C37 . C42 . C45 . 121.0(3) yes C41 . C42 . C45 . 121.0(3) yes Zr1 . C43 . C38 . 105.84(17) yes Zr1 . C43 . Co1 . 65.70(8) yes C38 . C43 . Co1 . 133.89(19) yes Zr1 . C43 . H431 . 138.4(15) no C38 . C43 . H431 . 108.9(9) no Co1 . C43 . H431 . 73.8(18) no Zr1 . C43 . H432 . 80(2) no C38 . C43 . H432 . 108.8(9) no Co1 . C43 . H432 . 113.4(12) no H431 . C43 . H432 . 109(3) no C40 . C44 . H441 . 110.9 no C40 . C44 . H442 . 111.6 no H441 . C44 . H442 . 109.6 no C40 . C44 . H443 . 108.7 no H441 . C44 . H443 . 107.5 no H442 . C44 . H443 . 108.4 no C42 . C45 . H451 . 109.2 no C42 . C45 . H452 . 109.5 no H451 . C45 . H452 . 110.2 no C42 . C45 . H453 . 108.7 no H451 . C45 . H453 . 109.4 no H452 . C45 . H453 . 109.8 no #===END data_7 _database_code_depnum_ccdc_archive 'CCDC 776342' #TrackingRef '- combined_rev.cif' _audit_creation_date 10-02-15 _audit_creation_method CRYSTALS_ver_14.01 # start Validation Reply Form: One Alert B issue _vrf_PLAT222_7 ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 4.70 Ratio RESPONSE: The molecule is 7:1 disordered as a mixed Cl/I complex. While the I/Cl disorder was modeled successfully, there were large peaks 1.5 - 2.0 e- near the Zr and Cl atoms, and several of the mesityl rings had large in-plane ellipsoid excursions, likely indicative of disorder. Attempts to model the other disorder (Zr, Co, mesityl) invariably failed. The large range of H atom Uiso parameters arises from the ratio of H293 on a disordered mesityl group to isopropyl methine H atom H311. ; # end Validation Reply Form _oxford_structure_analysis_title 'CMT36_0m in P-1' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 12.2227(5) _cell_length_b 14.2597(7) _cell_length_c 18.3302(9) _cell_angle_alpha 77.154(3) _cell_angle_beta 82.246(2) _cell_angle_gamma 79.036(2) _cell_volume 3043.6(2) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' Co 0.3494 0.9721 12.2841 4.2791 7.3409 0.2784 4.0034 13.5359 2.3488 71.1692 1.0118 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Zr -2.9673 0.5597 17.8765 1.2762 10.9480 11.9160 5.4173 0.1176 3.6572 87.6627 2.0693 'International Tables Vol C 4.2.6.8 and 6.1.1.4' I -0.4742 1.8119 20.1472 4.3470 18.9949 0.3814 7.5138 27.7660 2.2735 66.8776 4.0712 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C50 H86 Cl0.85 Co1 I0.15 N3 P3 Zr1 # Dc = 1.11 Fooo = 1082.66 Mu = 6.65 M = 1021.33 # Found Formula = C50 H86 Cl0.85 Co1 I0.15 N3 P3 Zr1 # Dc = 1.11 FOOO = 1082.66 Mu = 6.65 M = 1021.32 _chemical_formula_sum 'C50 H86 Cl0.85 Co1 I0.15 N3 P3 Zr1' _chemical_formula_moiety 'C50 H86 Cl0.85 Co1 I0.15 N3 P3 Zr1' _chemical_compound_source ? _chemical_formula_weight 1021.32 _cell_measurement_reflns_used 9908 _cell_measurement_theta_min 3 _cell_measurement_theta_max 30 _cell_measurement_temperature 120 _exptl_crystal_description 'prism fragment' _exptl_crystal_colour green _exptl_crystal_size_min 0.319 _exptl_crystal_size_mid 0.403 _exptl_crystal_size_max 0.583 _exptl_crystal_density_diffrn 1.114 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1082.664 _exptl_absorpt_coefficient_mu 0.665 # Sheldrick geometric approximatio 0.76 0.81 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Analytical Absorption (De Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_min 0.77 _exptl_absorpt_correction_T_max 0.81 _diffrn_measurement_device-type 'Bruker Kappa Apex2' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'Apex2 (Bruker AXS, 2006)' _computing_cell_refinement 'Apex2 (Bruker AXS, 2006)' _computing_data_reduction 'Apex2 (Bruker AXS, 2006)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 120 _diffrn_reflns_number 17679 _reflns_number_total 17679 _diffrn_reflns_av_R_equivalents 0.049 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 17679 # Theoretical number of reflections is about 35736 _diffrn_reflns_theta_min 2.067 _diffrn_reflns_theta_max 30.070 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 29.468 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _reflns_limit_h_min -16 _reflns_limit_h_max 17 _reflns_limit_k_min -19 _reflns_limit_k_max 20 _reflns_limit_l_min 0 _reflns_limit_l_max 25 _oxford_diffrn_Wilson_B_factor 1.95 _oxford_diffrn_Wilson_scale 163.70 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.28 _refine_diff_density_max 2.53 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 17679 _refine_ls_number_restraints 1 _refine_ls_number_parameters 542 _oxford_refine_ls_R_factor_ref 0.0943 _refine_ls_wR_factor_ref 0.2032 _refine_ls_goodness_of_fit_ref 0.9847 _refine_ls_shift/su_max 0.0040489 _refine_ls_shift/su_mean 8.1273460 # The values computed from all data _oxford_reflns_number_all 17679 _refine_ls_R_factor_all 0.0943 _refine_ls_wR_factor_all 0.2032 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 12534 _refine_ls_R_factor_gt 0.0669 _refine_ls_wR_factor_gt 0.1773 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment none # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.09P)^2^ +14.84P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Bruker Analytical X-ray Systems, Inc., 2006. Apex2, Version 2 User Manual, M86-E01078, Madison, WI. De Meulenaer, J. & Tompa, H. (1965). Acta Cryst. 19, 1014. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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 _oxford_atom_site_special_shape _atom_site_attached_hydrogens Zr1 Zr 0.78628(3) 0.88565(3) 0.308877(19) 0.0230 1.0000 Uani . . . . . . . Co1 Co 0.98204(4) 0.92711(4) 0.31735(3) 0.0269 1.0000 Uani D . . . . . . Cl1 Cl 1.1312(3) 0.9928(3) 0.3300(2) 0.0324 0.852(2) Uani . . P 1 1 . . I1 I 1.1353(6) 1.0204(5) 0.3258(5) 0.0466 0.148(2) Uani D . P 1 2 . . P1 P 0.96607(7) 0.77588(8) 0.39076(6) 0.0248 1.0000 Uani . . . . . . . P2 P 0.96124(8) 0.93522(10) 0.19503(5) 0.0310 1.0000 Uani . . . . . . . P3 P 0.56559(7) 0.88035(8) 0.34060(5) 0.0227 1.0000 Uani . . . . . . . N1 N 0.8301(2) 0.7637(2) 0.39757(18) 0.0245 1.0000 Uani . . . . . . . N2 N 0.8407(3) 0.8972(3) 0.19149(19) 0.0332 1.0000 Uani . . . . . . . N3 N 0.6293(2) 0.9771(2) 0.31174(17) 0.0236 1.0000 Uani . . . . . . . C1 C 1.0118(3) 0.7681(3) 0.4847(2) 0.0315 1.0000 Uani . . . . . . . C2 C 0.9789(4) 0.8653(4) 0.5093(2) 0.0366 1.0000 Uani . . . . . . . C3 C 1.1390(4) 0.7360(5) 0.4861(3) 0.0477 1.0000 Uani . . . . . . . C4 C 1.0451(3) 0.6676(4) 0.3544(3) 0.0356 1.0000 Uani . . . . . . . C5 C 1.0418(4) 0.5700(4) 0.4080(3) 0.0456 1.0000 Uani . . . . . . . C6 C 1.1641(4) 0.6776(5) 0.3202(3) 0.0482 1.0000 Uani . . . . . . . C7 C 0.7747(3) 0.6887(3) 0.4447(2) 0.0261 1.0000 Uani . . . . . . . C8 C 0.7361(3) 0.6911(3) 0.5199(2) 0.0282 1.0000 Uani . . . . . . . C9 C 0.6832(3) 0.6154(3) 0.5626(3) 0.0339 1.0000 Uani . . . . . . . C10 C 0.6621(3) 0.5399(3) 0.5340(3) 0.0405 1.0000 Uani . . . . . . . C11 C 0.6948(3) 0.5422(3) 0.4579(3) 0.0430 1.0000 Uani . . . . . . . C12 C 0.7485(3) 0.6151(3) 0.4126(3) 0.0336 1.0000 Uani . . . . . . . C13 C 0.7422(3) 0.7742(3) 0.5561(2) 0.0300 1.0000 Uani . . . . . . . C14 C 0.5986(4) 0.4623(4) 0.5802(4) 0.0571 1.0000 Uani . . . . . . . C15 C 0.7753(4) 0.6150(4) 0.3303(3) 0.0430 1.0000 Uani . . . . . . . C16 C 0.9572(4) 1.0612(4) 0.1386(2) 0.0405 1.0000 Uani . . . . . . . C17 C 1.0713(4) 1.0929(5) 0.1159(3) 0.0504 1.0000 Uani . . . . . . . C18 C 0.8842(4) 1.1328(4) 0.1826(3) 0.0433 1.0000 Uani . . . . . . . C19 C 1.0770(3) 0.8581(4) 0.1475(2) 0.0384 1.0000 Uani . . . . . . . C20 C 1.1952(3) 0.8683(5) 0.1612(3) 0.0458 1.0000 Uani . . . . . . . C21 C 1.0699(4) 0.8683(5) 0.0627(2) 0.0493 1.0000 Uani . . . . . . . C22 C 0.7931(3) 0.8852(4) 0.1268(2) 0.0411 1.0000 Uani . . . . . . . C23 C 0.8118(4) 0.7933(5) 0.1077(3) 0.0476 1.0000 Uani . . . . . . . C24 C 0.7618(4) 0.7830(6) 0.0457(3) 0.0608 1.0000 Uani . . . . . . . C25 C 0.6941(4) 0.8589(6) 0.0038(3) 0.0632 1.0000 Uani . . . . . . . C26 C 0.6750(4) 0.9458(6) 0.0252(3) 0.0589 1.0000 Uani . . . . . . . C27 C 0.7212(3) 0.9616(5) 0.0863(2) 0.0448 1.0000 Uani . . . . . . . C28 C 0.8857(5) 0.7067(5) 0.1482(3) 0.0563 1.0000 Uani . . . . . . . C29 C 0.6449(6) 0.8450(8) -0.0642(4) 0.0939 1.0000 Uani . . . . . . . C30 C 0.6878(4) 1.0599(5) 0.1072(3) 0.0496 1.0000 Uani . . . . . . . C31 C 0.4999(3) 0.8802(3) 0.4373(2) 0.0254 1.0000 Uani . . . . . . . C32 C 0.4053(3) 0.9660(3) 0.4449(2) 0.0305 1.0000 Uani . . . . . . . C33 C 0.4630(3) 0.7833(3) 0.4775(3) 0.0347 1.0000 Uani . . . . . . . C34 C 0.4556(3) 0.8756(3) 0.2821(2) 0.0293 1.0000 Uani . . . . . . . C35 C 0.4983(4) 0.8977(4) 0.1991(3) 0.0408 1.0000 Uani . . . . . . . C36 C 0.4248(5) 0.7744(4) 0.3024(3) 0.0513 1.0000 Uani . . . . . . . C37 C 0.6212(3) 1.0756(3) 0.31766(19) 0.0241 1.0000 Uani . . . . . . . C38 C 0.5341(3) 1.1518(3) 0.2948(2) 0.0293 1.0000 Uani . . . . . . . C39 C 0.5477(4) 1.2456(3) 0.2962(2) 0.0341 1.0000 Uani . . . . . . . C40 C 0.6420(4) 1.2673(3) 0.3188(2) 0.0353 1.0000 Uani . . . . . . . C41 C 0.7274(4) 1.1906(3) 0.3412(2) 0.0311 1.0000 Uani . . . . . . . C42 C 0.7185(3) 1.0947(3) 0.34227(19) 0.0247 1.0000 Uani . . . . . . . C43 C 0.4327(4) 1.1344(4) 0.2653(3) 0.0355 1.0000 Uani . . . . . . . C44 C 0.6522(6) 1.3710(4) 0.3198(4) 0.0557 1.0000 Uani . . . . . . . C45 C 0.8085(3) 1.0095(3) 0.3681(2) 0.0249 1.0000 Uani . . . . . . . C46 C 0.4295(15) 1.4075(14) -0.1589(10) 0.1925 1.0000 Uani . . . . . . . C47 C 0.5218(16) 1.3566(14) -0.1266(10) 0.1855 1.0000 Uani . . . . . . . C48 C 0.5072(15) 1.3649(11) -0.0441(9) 0.1571 1.0000 Uani . . . . . . . C49 C 0.6057(14) 1.3052(12) 0.0033(10) 0.1765 1.0000 Uani . . . . . . . C50 C 0.5941(15) 1.3252(12) 0.0845(7) 0.1836 1.0000 Uani . . . . . . . H11 H 0.9760 0.7184 0.5223 0.0378 1.0000 Uiso R . . . . . . H21 H 0.9014 0.8922 0.5028 0.0543 1.0000 Uiso R . . . . . . H22 H 1.0247 0.9115 0.4805 0.0547 1.0000 Uiso R . . . . . . H23 H 0.9891 0.8574 0.5620 0.0549 1.0000 Uiso R . . . . . . H31 H 1.1759 0.7818 0.4482 0.0711 1.0000 Uiso R . . . . . . H32 H 1.1576 0.7368 0.5360 0.0708 1.0000 Uiso R . . . . . . H33 H 1.1622 0.6703 0.4756 0.0708 1.0000 Uiso R . . . . . . H41 H 1.0056 0.6650 0.3120 0.0426 1.0000 Uiso R . . . . . . H51 H 1.0663 0.5178 0.3813 0.0678 1.0000 Uiso R . . . . . . H52 H 0.9676 0.5656 0.4311 0.0678 1.0000 Uiso R . . . . . . H53 H 1.0911 0.5627 0.4462 0.0677 1.0000 Uiso R . . . . . . H61 H 1.1659 0.7439 0.2930 0.0720 1.0000 Uiso R . . . . . . H62 H 1.2130 0.6619 0.3598 0.0719 1.0000 Uiso R . . . . . . H63 H 1.1889 0.6328 0.2862 0.0720 1.0000 Uiso R . . . . . . H91 H 0.6618 0.6169 0.6124 0.0407 1.0000 Uiso R . . . . . . H111 H 0.6798 0.4929 0.4364 0.0521 1.0000 Uiso R . . . . . . H131 H 0.7480 0.8306 0.5189 0.0446 1.0000 Uiso R . . . . . . H132 H 0.6754 0.7850 0.5884 0.0449 1.0000 Uiso R . . . . . . H133 H 0.8047 0.7603 0.5856 0.0449 1.0000 Uiso R . . . . . . H141 H 0.5200 0.4833 0.5749 0.0859 1.0000 Uiso R . . . . . . H142 H 0.6239 0.4030 0.5619 0.0860 1.0000 Uiso R . . . . . . H143 H 0.6115 0.4516 0.6321 0.0859 1.0000 Uiso R . . . . . . H151 H 0.8553 0.5989 0.3200 0.0650 1.0000 Uiso R . . . . . . H152 H 0.7499 0.6780 0.3007 0.0647 1.0000 Uiso R . . . . . . H153 H 0.7402 0.5674 0.3170 0.0652 1.0000 Uiso R . . . . . . H161 H 0.9223 1.0653 0.0929 0.0491 1.0000 Uiso R . . . . . . H171 H 1.1111 1.0821 0.1597 0.0756 1.0000 Uiso R . . . . . . H172 H 1.1134 1.0568 0.0798 0.0759 1.0000 Uiso R . . . . . . H173 H 1.0591 1.1621 0.0939 0.0759 1.0000 Uiso R . . . . . . H181 H 0.8133 1.1113 0.2021 0.0648 1.0000 Uiso R . . . . . . H182 H 0.8679 1.1960 0.1504 0.0650 1.0000 Uiso R . . . . . . H183 H 0.9219 1.1382 0.2237 0.0645 1.0000 Uiso R . . . . . . H191 H 1.0678 0.7910 0.1701 0.0457 1.0000 Uiso R . . . . . . H201 H 1.1954 0.8791 0.2112 0.0688 1.0000 Uiso R . . . . . . H202 H 1.2203 0.9209 0.1253 0.0691 1.0000 Uiso R . . . . . . H203 H 1.2447 0.8087 0.1569 0.0690 1.0000 Uiso R . . . . . . H211 H 1.0852 0.9310 0.0361 0.0737 1.0000 Uiso R . . . . . . H212 H 1.1237 0.8193 0.0431 0.0737 1.0000 Uiso R . . . . . . H213 H 0.9982 0.8607 0.0530 0.0737 1.0000 Uiso R . . . . . . H241 H 0.7756 0.7227 0.0324 0.0731 1.0000 Uiso R . . . . . . H261 H 0.6265 0.9974 -0.0015 0.0708 1.0000 Uiso R . . . . . . H281 H 0.8518 0.6494 0.1567 0.0838 1.0000 Uiso R . . . . . . H282 H 0.8986 0.7169 0.1962 0.0840 1.0000 Uiso R . . . . . . H283 H 0.9575 0.6946 0.1193 0.0838 1.0000 Uiso R . . . . . . H291 H 0.6383 0.7772 -0.0581 0.1409 1.0000 Uiso R . . . . . . H292 H 0.5719 0.8834 -0.0679 0.1411 1.0000 Uiso R . . . . . . H293 H 0.6925 0.8637 -0.1087 0.1410 1.0000 Uiso R . . . . . . H301 H 0.7451 1.0995 0.0873 0.0737 1.0000 Uiso R . . . . . . H302 H 0.6188 1.0925 0.0867 0.0741 1.0000 Uiso R . . . . . . H303 H 0.6770 1.0522 0.1611 0.0737 1.0000 Uiso R . . . . . . H311 H 0.5598 0.8870 0.4649 0.0300 1.0000 Uiso R . . . . . . H321 H 0.3460 0.9638 0.4168 0.0459 1.0000 Uiso R . . . . . . H322 H 0.4347 1.0263 0.4250 0.0458 1.0000 Uiso R . . . . . . H323 H 0.3792 0.9627 0.4966 0.0459 1.0000 Uiso R . . . . . . H331 H 0.5160 0.7295 0.4640 0.0519 1.0000 Uiso R . . . . . . H332 H 0.4596 0.7798 0.5309 0.0517 1.0000 Uiso R . . . . . . H333 H 0.3906 0.7815 0.4641 0.0520 1.0000 Uiso R . . . . . . H341 H 0.3893 0.9239 0.2919 0.0353 1.0000 Uiso R . . . . . . H351 H 0.5229 0.9598 0.1859 0.0604 1.0000 Uiso R . . . . . . H352 H 0.4400 0.8972 0.1690 0.0608 1.0000 Uiso R . . . . . . H353 H 0.5598 0.8477 0.1891 0.0611 1.0000 Uiso R . . . . . . H361 H 0.3907 0.7611 0.3535 0.0771 1.0000 Uiso R . . . . . . H362 H 0.4909 0.7265 0.2972 0.0767 1.0000 Uiso R . . . . . . H363 H 0.3736 0.7694 0.2683 0.0767 1.0000 Uiso R . . . . . . H391 H 0.4905 1.2956 0.2806 0.0410 1.0000 Uiso R . . . . . . H411 H 0.7927 1.2034 0.3552 0.0370 1.0000 Uiso R . . . . . . H431 H 0.3839 1.1948 0.2533 0.0531 1.0000 Uiso R . . . . . . H432 H 0.4534 1.1084 0.2208 0.0532 1.0000 Uiso R . . . . . . H433 H 0.3954 1.0900 0.3021 0.0533 1.0000 Uiso R . . . . . . H441 H 0.7128 1.3916 0.2849 0.0832 1.0000 Uiso R . . . . . . H442 H 0.6649 1.3764 0.3691 0.0833 1.0000 Uiso R . . . . . . H443 H 0.5839 1.4147 0.3062 0.0829 1.0000 Uiso R . . . . . . H451 H 0.7788 0.9706 0.4138 0.0362 1.0000 Uiso R . . . . . . H452 H 0.8679 1.0347 0.3827 0.0370 1.0000 Uiso R . . . . . . H471 H 0.5877 1.3847 -0.1524 0.2191 1.0000 Uiso R . . . . . . H472 H 0.5313 1.2881 -0.1305 0.2191 1.0000 Uiso R . . . . . . H481 H 0.4366 1.3424 -0.0201 0.1873 1.0000 Uiso R . . . . . . H482 H 0.5015 1.4348 -0.0431 0.1873 1.0000 Uiso R . . . . . . H491 H 0.6769 1.3247 -0.0224 0.2111 1.0000 Uiso R . . . . . . H492 H 0.6082 1.2344 0.0065 0.2111 1.0000 Uiso R . . . . . . H501 H 0.6279 1.3824 0.0839 0.2741 1.0000 Uiso R . . . . . . H502 H 0.5160 1.3380 0.1021 0.2741 1.0000 Uiso R . . . . . . H503 H 0.6322 1.2692 0.1174 0.2740 1.0000 Uiso R . . . . . . H461 H 0.4380 1.4023 -0.2103 0.2193 1.0000 Uiso R . . . . . . H462 H 0.4215 1.4741 -0.1558 0.2193 1.0000 Uiso R . . . . . . H463 H 0.3649 1.3819 -0.1343 0.2193 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 Zr1 0.01146(14) 0.0399(2) 0.02088(17) -0.01333(14) 0.00356(11) -0.00744(13) Co1 0.0177(2) 0.0463(3) 0.0203(2) -0.0099(2) 0.00175(17) -0.0132(2) Cl1 0.0205(8) 0.0504(17) 0.0306(9) -0.0120(11) 0.0017(6) -0.0152(9) I1 0.0335(15) 0.067(4) 0.0454(17) -0.003(2) -0.0053(11) -0.031(2) P1 0.0126(4) 0.0380(5) 0.0259(5) -0.0120(4) 0.0016(3) -0.0055(3) P2 0.0136(4) 0.0618(7) 0.0193(4) -0.0125(4) 0.0033(3) -0.0091(4) P3 0.0113(4) 0.0350(5) 0.0247(4) -0.0136(4) 0.0038(3) -0.0064(3) N1 0.0118(12) 0.0354(17) 0.0297(16) -0.0165(13) 0.0035(11) -0.0042(11) N2 0.0135(13) 0.068(3) 0.0229(15) -0.0212(16) 0.0010(11) -0.0073(14) N3 0.0155(13) 0.0352(17) 0.0226(14) -0.0115(13) 0.0026(11) -0.0067(12) C1 0.0207(17) 0.049(2) 0.0267(19) -0.0060(17) -0.0043(14) -0.0106(16) C2 0.040(2) 0.046(3) 0.029(2) -0.0104(18) -0.0040(17) -0.017(2) C3 0.030(2) 0.072(4) 0.047(3) -0.021(3) -0.012(2) -0.005(2) C4 0.0177(17) 0.048(3) 0.042(2) -0.021(2) 0.0010(15) 0.0027(16) C5 0.023(2) 0.044(3) 0.070(3) -0.020(2) -0.002(2) 0.0030(18) C6 0.0178(18) 0.076(4) 0.050(3) -0.023(3) 0.0053(18) -0.001(2) C7 0.0133(14) 0.0267(18) 0.039(2) -0.0121(16) 0.0020(13) -0.0028(13) C8 0.0125(14) 0.0300(19) 0.040(2) -0.0083(16) 0.0028(14) -0.0014(13) C9 0.0173(16) 0.032(2) 0.046(2) -0.0023(18) 0.0042(15) -0.0010(14) C10 0.0169(17) 0.026(2) 0.076(3) -0.007(2) -0.0018(19) -0.0021(14) C11 0.0177(17) 0.031(2) 0.086(4) -0.024(2) -0.001(2) -0.0043(15) C12 0.0162(16) 0.034(2) 0.054(3) -0.0205(19) 0.0002(16) -0.0020(14) C13 0.0234(17) 0.036(2) 0.0293(19) -0.0095(16) 0.0046(14) -0.0044(15) C14 0.027(2) 0.030(2) 0.107(5) 0.001(3) -0.003(3) -0.0081(18) C15 0.028(2) 0.050(3) 0.061(3) -0.036(2) -0.001(2) -0.0056(19) C16 0.0226(18) 0.076(3) 0.0207(18) -0.004(2) 0.0022(14) -0.011(2) C17 0.030(2) 0.081(4) 0.037(2) -0.005(2) 0.0097(18) -0.019(2) C18 0.035(2) 0.064(3) 0.028(2) -0.004(2) 0.0051(17) -0.013(2) C19 0.0180(17) 0.077(3) 0.0214(18) -0.017(2) 0.0023(14) -0.0052(19) C20 0.0146(17) 0.088(4) 0.035(2) -0.017(2) 0.0007(15) -0.006(2) C21 0.024(2) 0.100(4) 0.026(2) -0.024(2) 0.0085(16) -0.008(2) C22 0.0174(17) 0.092(4) 0.0202(18) -0.022(2) 0.0048(13) -0.016(2) C23 0.025(2) 0.096(4) 0.032(2) -0.033(3) 0.0055(17) -0.018(2) C24 0.037(3) 0.121(6) 0.046(3) -0.051(3) 0.011(2) -0.037(3) C25 0.025(2) 0.149(7) 0.030(2) -0.037(3) 0.0023(18) -0.030(3) C26 0.0200(19) 0.141(6) 0.022(2) -0.022(3) 0.0016(15) -0.025(3) C27 0.0169(17) 0.100(4) 0.0204(18) -0.015(2) 0.0061(14) -0.017(2) C28 0.044(3) 0.093(5) 0.044(3) -0.043(3) 0.005(2) -0.015(3) C29 0.044(3) 0.211(10) 0.051(4) -0.062(5) -0.003(3) -0.040(5) C30 0.0209(19) 0.096(4) 0.028(2) -0.004(2) 0.0002(16) -0.010(2) C31 0.0164(15) 0.034(2) 0.0261(17) -0.0102(15) 0.0041(12) -0.0053(14) C32 0.0251(18) 0.038(2) 0.0258(18) -0.0099(16) 0.0052(14) 0.0001(16) C33 0.0217(18) 0.037(2) 0.040(2) -0.0050(18) 0.0087(16) -0.0051(16) C34 0.0163(15) 0.044(2) 0.033(2) -0.0183(17) 0.0005(14) -0.0084(15) C35 0.0239(19) 0.074(3) 0.033(2) -0.025(2) 0.0030(16) -0.016(2) C36 0.053(3) 0.054(3) 0.057(3) -0.001(2) -0.029(3) -0.030(3) C37 0.0239(16) 0.036(2) 0.0148(15) -0.0069(14) 0.0037(12) -0.0113(14) C38 0.0289(19) 0.040(2) 0.0187(16) -0.0055(15) 0.0021(14) -0.0098(16) C39 0.039(2) 0.036(2) 0.0251(19) -0.0024(16) -0.0018(16) -0.0045(18) C40 0.045(2) 0.031(2) 0.030(2) -0.0036(17) -0.0001(17) -0.0116(18) C41 0.034(2) 0.038(2) 0.0251(18) -0.0078(16) -0.0011(15) -0.0147(17) C42 0.0240(17) 0.037(2) 0.0156(15) -0.0082(14) 0.0039(12) -0.0119(15) C43 0.032(2) 0.043(2) 0.031(2) -0.0059(18) -0.0041(16) -0.0051(18) C44 0.066(4) 0.037(3) 0.068(4) -0.007(3) -0.018(3) -0.015(3) C45 0.0220(16) 0.036(2) 0.0192(16) -0.0070(14) 0.0001(12) -0.0106(14) C46 0.174(17) 0.215(18) 0.172(16) 0.002(13) -0.076(13) 0.002(14) C47 0.189(17) 0.234(19) 0.165(14) -0.128(14) -0.064(13) 0.024(14) C48 0.179(16) 0.134(11) 0.162(14) -0.027(10) -0.018(12) -0.037(11) C49 0.136(13) 0.154(13) 0.206(18) 0.015(12) -0.045(12) 0.019(10) C50 0.214(18) 0.220(17) 0.087(8) -0.046(10) -0.043(10) 0.073(14) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.13780(6) 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 Zr1 . Co1 . 2.6036(6) yes Zr1 . P1 . 2.8406(10) yes Zr1 . P2 . 2.8535(10) yes Zr1 . P3 . 2.6935(9) yes Zr1 . N1 . 2.140(4) yes Zr1 . N2 . 2.144(3) yes Zr1 . N3 . 2.106(3) yes Zr1 . C45 . 2.343(4) yes Co1 . Cl1 . 2.262(3) yes Co1 . P1 . 2.3018(12) yes Co1 . P2 . 2.2656(11) yes Co1 . C45 . 2.398(4) yes Co1 . I1 . 2.534(5) yes Co1 . P1 . 2.3018(12) yes Co1 . P2 . 2.2656(11) yes Co1 . C45 . 2.398(4) yes P1 . N1 . 1.688(3) yes P1 . C1 . 1.856(4) yes P1 . C4 . 1.865(4) yes P2 . N2 . 1.677(3) yes P2 . C16 . 1.859(5) yes P2 . C19 . 1.863(4) yes P3 . N3 . 1.662(3) yes P3 . C31 . 1.844(4) yes P3 . C34 . 1.849(4) yes N1 . C7 . 1.435(5) yes N2 . C22 . 1.444(5) yes N3 . C37 . 1.417(5) yes C1 . C2 . 1.516(7) yes C1 . C3 . 1.537(6) yes C1 . H11 . 0.993 no C2 . H21 . 0.966 no C2 . H22 . 0.966 no C2 . H23 . 0.969 no C3 . H31 . 0.968 no C3 . H32 . 0.975 no C3 . H33 . 0.980 no C4 . C5 . 1.518(7) yes C4 . C6 . 1.524(6) yes C4 . H41 . 0.980 no C5 . H51 . 0.960 no C5 . H52 . 0.955 no C5 . H53 . 0.960 no C6 . H61 . 0.969 no C6 . H62 . 0.963 no C6 . H63 . 0.970 no C7 . C8 . 1.401(6) yes C7 . C12 . 1.414(5) yes C8 . C9 . 1.397(6) yes C8 . C13 . 1.499(6) yes C9 . C10 . 1.376(7) yes C9 . H91 . 0.919 no C10 . C11 . 1.392(8) yes C10 . C14 . 1.509(7) yes C11 . C12 . 1.389(7) yes C11 . H111 . 0.935 no C12 . C15 . 1.502(7) yes C13 . H131 . 0.940 no C13 . H132 . 0.950 no C13 . H133 . 0.960 no C14 . H141 . 0.961 no C14 . H142 . 0.960 no C14 . H143 . 0.960 no C15 . H151 . 0.964 no C15 . H152 . 0.960 no C15 . H153 . 0.957 no C16 . C17 . 1.523(6) yes C16 . C18 . 1.521(7) yes C16 . H161 . 0.976 no C17 . H171 . 0.964 no C17 . H172 . 0.963 no C17 . H173 . 0.970 no C18 . H181 . 0.970 no C18 . H182 . 0.963 no C18 . H183 . 0.958 no C19 . C20 . 1.538(6) yes C19 . C21 . 1.543(6) yes C19 . H191 . 0.976 no C20 . H201 . 0.963 no C20 . H202 . 0.950 no C20 . H203 . 0.958 no C21 . H211 . 0.958 no C21 . H212 . 0.960 no C21 . H213 . 0.947 no C22 . C23 . 1.401(8) yes C22 . C27 . 1.401(7) yes C23 . C24 . 1.409(6) yes C23 . C28 . 1.497(9) yes C24 . C25 . 1.380(10) yes C24 . H241 . 0.925 no C25 . C26 . 1.351(10) yes C25 . C29 . 1.522(7) yes C26 . C27 . 1.398(6) yes C26 . H261 . 0.939 no C27 . C30 . 1.502(9) yes C28 . H281 . 0.957 no C28 . H282 . 0.961 no C28 . H283 . 0.969 no C29 . H291 . 0.965 no C29 . H292 . 0.957 no C29 . H293 . 0.953 no C30 . H301 . 0.965 no C30 . H302 . 0.963 no C30 . H303 . 0.964 no C31 . C32 . 1.532(5) yes C31 . C33 . 1.532(6) yes C31 . H311 . 0.976 no C32 . H321 . 0.954 no C32 . H322 . 0.971 no C32 . H323 . 0.953 no C33 . H331 . 0.961 no C33 . H332 . 0.963 no C33 . H333 . 0.957 no C34 . C35 . 1.522(6) yes C34 . C36 . 1.514(6) yes C34 . H341 . 0.983 no C35 . H351 . 0.959 no C35 . H352 . 0.960 no C35 . H353 . 0.962 no C36 . H361 . 0.966 no C36 . H362 . 0.964 no C36 . H363 . 0.965 no C37 . C38 . 1.403(6) yes C37 . C42 . 1.419(5) yes C38 . C39 . 1.384(6) yes C38 . C43 . 1.499(6) yes C39 . C40 . 1.385(6) yes C39 . H391 . 0.924 no C40 . C41 . 1.391(6) yes C40 . C44 . 1.512(7) yes C41 . C42 . 1.389(6) yes C41 . H411 . 0.931 no C42 . C45 . 1.512(6) yes C43 . H431 . 0.950 no C43 . H432 . 0.954 no C43 . H433 . 0.949 no C44 . H441 . 0.957 no C44 . H442 . 0.959 no C44 . H443 . 0.968 no C45 . H451 . 0.963 no C45 . H452 . 0.960 no C46 . C47 . 1.352(19) yes C46 . H461 . 0.950 no C46 . H462 . 0.950 no C46 . H463 . 0.950 no C47 . C48 . 1.526(19) yes C47 . H471 . 0.984 no C47 . H472 . 0.979 no C48 . C49 . 1.580(19) yes C48 . H481 . 0.991 no C48 . H482 . 0.989 no C49 . C50 . 1.56(2) yes C49 . H491 . 0.989 no C49 . H492 . 0.993 no C50 . H501 . 0.979 no C50 . H502 . 0.963 no C50 . H503 . 0.968 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 Co1 . Zr1 . P1 . 49.79(2) yes Co1 . Zr1 . P2 . 48.79(2) yes P1 . Zr1 . P2 . 83.65(3) yes Co1 . Zr1 . P3 . 158.88(3) yes P1 . Zr1 . P3 . 128.54(3) yes P2 . Zr1 . P3 . 146.04(3) yes Co1 . Zr1 . N1 . 85.20(8) yes P1 . Zr1 . N1 . 36.30(8) yes P2 . Zr1 . N1 . 116.56(8) yes P3 . Zr1 . N1 . 92.85(8) yes Co1 . Zr1 . N2 . 84.38(9) yes P1 . Zr1 . N2 . 107.72(9) yes P2 . Zr1 . N2 . 35.79(9) yes P3 . Zr1 . N2 . 113.03(9) yes N1 . Zr1 . N2 . 126.82(13) yes Co1 . Zr1 . N3 . 128.38(9) yes P1 . Zr1 . N3 . 147.01(9) yes P2 . Zr1 . N3 . 120.60(9) yes P3 . Zr1 . N3 . 38.11(9) yes N1 . Zr1 . N3 . 122.32(12) yes Co1 . Zr1 . C45 . 57.72(9) yes P1 . Zr1 . C45 . 83.89(10) yes P2 . Zr1 . C45 . 90.81(9) yes P3 . Zr1 . C45 . 101.97(9) yes N1 . Zr1 . C45 . 98.17(13) yes N2 . Zr1 . N3 . 104.49(13) yes N2 . Zr1 . C45 . 118.81(14) yes N3 . Zr1 . C45 . 74.50(12) yes Zr1 . Co1 . Cl1 . 168.00(10) yes Zr1 . Co1 . P1 . 70.47(3) yes Cl1 . Co1 . P1 . 116.85(11) yes Zr1 . Co1 . P2 . 71.37(3) yes Cl1 . Co1 . P2 . 111.79(11) yes P1 . Co1 . P2 . 112.48(5) yes Zr1 . Co1 . C45 . 55.67(9) yes Cl1 . Co1 . C45 . 112.84(13) yes P1 . Co1 . C45 . 95.66(10) yes P2 . Co1 . C45 . 105.67(9) yes Zr1 . Co1 . I1 . 161.74(19) yes Zr1 . Co1 . P1 . 70.47(3) yes I1 . Co1 . P1 . 123.10(19) yes Zr1 . Co1 . P2 . 71.37(3) yes I1 . Co1 . P2 . 109.57(19) yes P1 . Co1 . P2 . 112.48(5) yes Zr1 . Co1 . C45 . 55.67(9) yes I1 . Co1 . C45 . 108.0(2) yes P1 . Co1 . C45 . 95.66(10) yes P2 . Co1 . C45 . 105.67(9) yes Zr1 . P1 . Co1 . 59.74(3) yes Zr1 . P1 . N1 . 48.61(12) yes Co1 . P1 . N1 . 107.03(13) yes Zr1 . P1 . C1 . 135.51(14) yes Co1 . P1 . C1 . 109.40(15) yes N1 . P1 . C1 . 111.01(17) yes Zr1 . P1 . C4 . 115.99(15) yes Co1 . P1 . C4 . 117.13(16) yes N1 . P1 . C4 . 105.00(18) yes C1 . P1 . C4 . 107.2(2) yes Zr1 . P2 . Co1 . 59.84(3) yes Zr1 . P2 . N2 . 48.37(11) yes Co1 . P2 . N2 . 107.90(12) yes Zr1 . P2 . C16 . 121.45(14) yes Co1 . P2 . C16 . 112.03(16) yes N2 . P2 . C16 . 109.3(2) yes Zr1 . P2 . C19 . 131.65(18) yes Co1 . P2 . C19 . 113.42(14) yes N2 . P2 . C19 . 108.4(2) yes C16 . P2 . C19 . 105.7(2) yes Zr1 . P3 . N3 . 51.43(11) yes Zr1 . P3 . C31 . 119.85(12) yes N3 . P3 . C31 . 108.85(17) yes Zr1 . P3 . C34 . 132.37(13) yes N3 . P3 . C34 . 114.49(19) yes C31 . P3 . C34 . 107.78(17) yes P1 . N1 . Zr1 . 95.09(15) yes P1 . N1 . C7 . 128.6(3) yes Zr1 . N1 . C7 . 136.1(2) yes P2 . N2 . Zr1 . 95.84(15) yes P2 . N2 . C22 . 128.9(3) yes Zr1 . N2 . C22 . 135.2(3) yes P3 . N3 . Zr1 . 90.46(15) yes P3 . N3 . C37 . 142.6(2) yes Zr1 . N3 . C37 . 120.4(2) yes P1 . C1 . C2 . 111.2(3) yes P1 . C1 . C3 . 111.9(3) yes C2 . C1 . C3 . 108.8(4) yes P1 . C1 . H11 . 109.5 no C2 . C1 . H11 . 108.6 no C3 . C1 . H11 . 106.7 no C1 . C2 . H21 . 111.2 no C1 . C2 . H22 . 110.5 no H21 . C2 . H22 . 108.4 no C1 . C2 . H23 . 110.4 no H21 . C2 . H23 . 107.9 no H22 . C2 . H23 . 108.3 no C1 . C3 . H31 . 108.4 no C1 . C3 . H32 . 107.6 no H31 . C3 . H32 . 110.4 no C1 . C3 . H33 . 111.0 no H31 . C3 . H33 . 109.5 no H32 . C3 . H33 . 109.9 no P1 . C4 . C5 . 115.4(3) yes P1 . C4 . C6 . 114.6(4) yes C5 . C4 . C6 . 111.2(4) yes P1 . C4 . H41 . 104.5 no C5 . C4 . H41 . 105.3 no C6 . C4 . H41 . 104.5 no C4 . C5 . H51 . 110.1 no C4 . C5 . H52 . 110.7 no H51 . C5 . H52 . 108.7 no C4 . C5 . H53 . 109.5 no H51 . C5 . H53 . 108.5 no H52 . C5 . H53 . 109.3 no C4 . C6 . H61 . 109.6 no C4 . C6 . H62 . 109.3 no H61 . C6 . H62 . 109.7 no C4 . C6 . H63 . 109.5 no H61 . C6 . H63 . 109.6 no H62 . C6 . H63 . 109.2 no N1 . C7 . C8 . 121.9(3) yes N1 . C7 . C12 . 119.1(4) yes C8 . C7 . C12 . 118.7(4) yes C7 . C8 . C9 . 118.8(4) yes C7 . C8 . C13 . 123.4(4) yes C9 . C8 . C13 . 117.7(4) yes C8 . C9 . C10 . 123.5(5) yes C8 . C9 . H91 . 117.2 no C10 . C9 . H91 . 119.3 no C9 . C10 . C11 . 116.7(4) yes C9 . C10 . C14 . 122.3(5) yes C11 . C10 . C14 . 120.8(5) yes C10 . C11 . C12 . 122.5(4) yes C10 . C11 . H111 . 118.8 no C12 . C11 . H111 . 118.7 no C7 . C12 . C11 . 119.4(4) yes C7 . C12 . C15 . 121.6(4) yes C11 . C12 . C15 . 119.0(4) yes C8 . C13 . H131 . 109.5 no C8 . C13 . H132 . 108.2 no H131 . C13 . H132 . 109.4 no C8 . C13 . H133 . 112.0 no H131 . C13 . H133 . 109.3 no H132 . C13 . H133 . 108.4 no C10 . C14 . H141 . 108.9 no C10 . C14 . H142 . 108.7 no H141 . C14 . H142 . 109.7 no C10 . C14 . H143 . 110.0 no H141 . C14 . H143 . 109.7 no H142 . C14 . H143 . 109.8 no C12 . C15 . H151 . 108.5 no C12 . C15 . H152 . 110.7 no H151 . C15 . H152 . 109.0 no C12 . C15 . H153 . 109.9 no H151 . C15 . H153 . 109.4 no H152 . C15 . H153 . 109.3 no P2 . C16 . C17 . 114.7(4) yes P2 . C16 . C18 . 109.3(3) yes C17 . C16 . C18 . 108.5(5) yes P2 . C16 . H161 . 108.1 no C17 . C16 . H161 . 108.2 no C18 . C16 . H161 . 107.8 no C16 . C17 . H171 . 109.7 no C16 . C17 . H172 . 109.8 no H171 . C17 . H172 . 110.2 no C16 . C17 . H173 . 107.9 no H171 . C17 . H173 . 109.1 no H172 . C17 . H173 . 110.1 no C16 . C18 . H181 . 110.7 no C16 . C18 . H182 . 110.3 no H181 . C18 . H182 . 107.5 no C16 . C18 . H183 . 109.9 no H181 . C18 . H183 . 109.1 no H182 . C18 . H183 . 109.4 no P2 . C19 . C20 . 114.6(3) yes P2 . C19 . C21 . 114.6(3) yes C20 . C19 . C21 . 109.8(3) yes P2 . C19 . H191 . 105.1 no C20 . C19 . H191 . 106.5 no C21 . C19 . H191 . 105.3 no C19 . C20 . H201 . 110.4 no C19 . C20 . H202 . 110.2 no H201 . C20 . H202 . 109.8 no C19 . C20 . H203 . 108.6 no H201 . C20 . H203 . 107.9 no H202 . C20 . H203 . 109.9 no C19 . C21 . H211 . 110.0 no C19 . C21 . H212 . 110.8 no H211 . C21 . H212 . 108.2 no C19 . C21 . H213 . 111.3 no H211 . C21 . H213 . 109.1 no H212 . C21 . H213 . 107.3 no N2 . C22 . C23 . 119.4(5) yes N2 . C22 . C27 . 121.4(5) yes C23 . C22 . C27 . 119.0(4) yes C22 . C23 . C24 . 118.2(6) yes C22 . C23 . C28 . 123.2(4) yes C24 . C23 . C28 . 118.6(5) yes C23 . C24 . C25 . 123.0(6) yes C23 . C24 . H241 . 118.1 no C25 . C24 . H241 . 118.9 no C24 . C25 . C26 . 117.3(5) yes C24 . C25 . C29 . 121.0(7) yes C26 . C25 . C29 . 121.7(7) yes C25 . C26 . C27 . 123.1(6) yes C25 . C26 . H261 . 118.1 no C27 . C26 . H261 . 118.8 no C22 . C27 . C26 . 119.3(6) yes C22 . C27 . C30 . 122.7(4) yes C26 . C27 . C30 . 117.9(5) yes C23 . C28 . H281 . 110.7 no C23 . C28 . H282 . 110.7 no H281 . C28 . H282 . 108.0 no C23 . C28 . H283 . 110.9 no H281 . C28 . H283 . 108.3 no H282 . C28 . H283 . 108.2 no C25 . C29 . H291 . 109.1 no C25 . C29 . H292 . 109.6 no H291 . C29 . H292 . 108.6 no C25 . C29 . H293 . 109.8 no H291 . C29 . H293 . 109.6 no H292 . C29 . H293 . 110.1 no C27 . C30 . H301 . 110.2 no C27 . C30 . H302 . 109.8 no H301 . C30 . H302 . 108.7 no C27 . C30 . H303 . 109.8 no H301 . C30 . H303 . 109.6 no H302 . C30 . H303 . 108.8 no P3 . C31 . C32 . 114.6(3) yes P3 . C31 . C33 . 114.1(3) yes C32 . C31 . C33 . 110.8(3) yes P3 . C31 . H311 . 104.6 no C32 . C31 . H311 . 106.8 no C33 . C31 . H311 . 105.1 no C31 . C32 . H321 . 109.6 no C31 . C32 . H322 . 108.5 no H321 . C32 . H322 . 109.3 no C31 . C32 . H323 . 109.3 no H321 . C32 . H323 . 110.5 no H322 . C32 . H323 . 109.6 no C31 . C33 . H331 . 110.3 no C31 . C33 . H332 . 107.9 no H331 . C33 . H332 . 109.5 no C31 . C33 . H333 . 109.4 no H331 . C33 . H333 . 109.9 no H332 . C33 . H333 . 109.8 no P3 . C34 . C35 . 110.1(3) yes P3 . C34 . C36 . 108.8(3) yes C35 . C34 . C36 . 109.4(4) yes P3 . C34 . H341 . 109.3 no C35 . C34 . H341 . 109.6 no C36 . C34 . H341 . 109.6 no C34 . C35 . H351 . 110.7 no C34 . C35 . H352 . 109.7 no H351 . C35 . H352 . 110.0 no C34 . C35 . H353 . 109.2 no H351 . C35 . H353 . 109.2 no H352 . C35 . H353 . 107.9 no C34 . C36 . H361 . 111.0 no C34 . C36 . H362 . 109.7 no H361 . C36 . H362 . 109.0 no C34 . C36 . H363 . 109.1 no H361 . C36 . H363 . 109.9 no H362 . C36 . H363 . 108.2 no N3 . C37 . C38 . 126.0(3) yes N3 . C37 . C42 . 112.9(3) yes C38 . C37 . C42 . 120.7(4) yes C37 . C38 . C39 . 117.5(4) yes C37 . C38 . C43 . 121.9(4) yes C39 . C38 . C43 . 120.5(4) yes C38 . C39 . C40 . 123.5(4) yes C38 . C39 . H391 . 117.2 no C40 . C39 . H391 . 119.4 no C39 . C40 . C41 . 118.1(4) yes C39 . C40 . C44 . 121.3(5) yes C41 . C40 . C44 . 120.6(4) yes C40 . C41 . C42 . 121.5(4) yes C40 . C41 . H411 . 119.8 no C42 . C41 . H411 . 118.7 no C37 . C42 . C41 . 118.7(4) yes C37 . C42 . C45 . 118.5(3) yes C41 . C42 . C45 . 122.8(3) yes C38 . C43 . H431 . 108.7 no C38 . C43 . H432 . 110.5 no H431 . C43 . H432 . 108.5 no C38 . C43 . H433 . 110.1 no H431 . C43 . H433 . 109.8 no H432 . C43 . H433 . 109.2 no C40 . C44 . H441 . 110.8 no C40 . C44 . H442 . 110.4 no H441 . C44 . H442 . 108.8 no C40 . C44 . H443 . 110.3 no H441 . C44 . H443 . 108.5 no H442 . C44 . H443 . 107.9 no C42 . C45 . Zr1 . 105.6(2) yes C42 . C45 . Co1 . 138.3(2) yes Zr1 . C45 . Co1 . 66.61(10) yes C42 . C45 . H451 . 108.2 no Zr1 . C45 . H451 . 86.2 no Co1 . C45 . H451 . 111.8 no C42 . C45 . H452 . 108.0 no Zr1 . C45 . H452 . 138.8 no Co1 . C45 . H452 . 72.5 no H451 . C45 . H452 . 104.9 no C47 . C46 . H461 . 108.6 no C47 . C46 . H462 . 109.6 no H461 . C46 . H462 . 109.5 no C47 . C46 . H463 . 110.1 no H461 . C46 . H463 . 109.5 no H462 . C46 . H463 . 109.5 no C46 . C47 . C48 . 108.3(16) yes C46 . C47 . H471 . 109.0 no C48 . C47 . H471 . 109.8 no C46 . C47 . H472 . 110.0 no C48 . C47 . H472 . 110.2 no H471 . C47 . H472 . 109.6 no C47 . C48 . C49 . 114.9(15) yes C47 . C48 . H481 . 108.9 no C49 . C48 . H481 . 108.3 no C47 . C48 . H482 . 107.1 no C49 . C48 . H482 . 108.3 no H481 . C48 . H482 . 109.2 no C48 . C49 . C50 . 113.1(13) yes C48 . C49 . H491 . 108.4 no C50 . C49 . H491 . 107.4 no C48 . C49 . H492 . 109.3 no C50 . C49 . H492 . 108.9 no H491 . C49 . H492 . 109.7 no C49 . C50 . H501 . 109.5 no C49 . C50 . H502 . 109.2 no H501 . C50 . H502 . 108.9 no C49 . C50 . H503 . 109.6 no H501 . C50 . H503 . 109.2 no H502 . C50 . H503 . 110.3 no # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.500 0.000 586 70 ' ' _platon_squeeze_details ; During the structure solution, electron density difference maps revealed that there were considerable disordered solvent molecules. One pentane molecule was located and successfully refined. From history, the remaining solvate was likely pentane or toluene in a volume of 588.8 \%A3 per unit cell (19.3%); the remaining peaks could not be modeled successfully. It appeared that the cavity area contained about two pentane molecules, located near the center of symmetry at (0, 1/2, 0). Modeling with or without restraints was unsuccessful, as was step by step acquisition of peaks using successive electron density difference maps. Thus, the structure factors were modified using the PLATON SQUEEZE technique, in order to produce a ?solvate-free? structure factor set (only for the second independent pentane molecule.) PLATON reported a total electron density of 70 e- per unit cell, likely representing two pentane molecules, consistent with our earlier observations. Use of the SQUEEZE technique resulted in a decrease of ca 1.3 % in R. ; #===END data_8 _database_code_depnum_ccdc_archive 'CCDC 776343' #TrackingRef '- combined_rev.cif' _audit_creation_date 10-01-31 _audit_creation_method CRYSTALS_ver_14.01 _oxford_structure_analysis_title 'CMT35_0m in P-1' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 11.4036(3) _cell_length_b 12.3007(3) _cell_length_c 18.7536(5) _cell_angle_alpha 94.3420(10) _cell_angle_beta 105.8890(10) _cell_angle_gamma 108.4810(10) _cell_volume 2361.24(11) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' 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 C 4.2.6.8 and 6.1.1.4' Co 0.3494 0.9721 12.2841 4.2791 7.3409 0.2784 4.0034 13.5359 2.3488 71.1692 1.0118 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Zr -2.9673 0.5597 17.8765 1.2762 10.9480 11.9160 5.4173 0.1176 3.6572 87.6627 2.0693 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C45 H79 Co1 N3 P3 Zr1 # Dc = 1.27 Fooo = 964.00 Mu = 7.06 M = 905.22 # Found Formula = C45 H79 Co1 N3 P3 Zr1 # Dc = 1.27 FOOO = 964.00 Mu = 7.06 M = 905.22 _chemical_formula_sum 'C45 H79 Co1 N3 P3 Zr1' _chemical_formula_moiety 'C45 H79 Co1 N3 P3 Zr1' _chemical_compound_source ? _chemical_formula_weight 905.22 _cell_measurement_reflns_used 9855 _cell_measurement_theta_min 3 _cell_measurement_theta_max 30 _cell_measurement_temperature 100 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_min 0.070 _exptl_crystal_size_mid 0.138 _exptl_crystal_size_max 0.302 _exptl_crystal_density_diffrn 1.273 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 964 _exptl_absorpt_coefficient_mu 0.706 # Sheldrick geometric approximatio 0.91 0.95 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Analytical Absorption (De Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_min 0.91 _exptl_absorpt_correction_T_max 0.95 _diffrn_measurement_device-type 'Bruker Kappa Apex2' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'Apex2 (Bruker AXS, 2006)' _computing_cell_refinement 'Apex2 (Bruker AXS, 2006)' _computing_data_reduction 'Apex2 (Bruker AXS, 2006)' _computing_structure_solution 'CRYSTALS (Betteridge et al., 2003)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 100 _diffrn_reflns_number 66346 _reflns_number_total 13803 _diffrn_reflns_av_R_equivalents 0.046 # Number of reflections without Friedels Law is 13891 # Number of reflections with Friedels Law is 13803 # Theoretical number of reflections is about 13851 _diffrn_reflns_theta_min 1.147 _diffrn_reflns_theta_max 30.061 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.061 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _reflns_limit_h_min -16 _reflns_limit_h_max 15 _reflns_limit_k_min -17 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 26 _oxford_diffrn_Wilson_B_factor 1.04 _oxford_diffrn_Wilson_scale 2.68 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.58 _refine_diff_density_max 0.74 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 13778 _refine_ls_number_restraints 0 _refine_ls_number_parameters 499 _oxford_refine_ls_R_factor_ref 0.0399 _refine_ls_wR_factor_ref 0.0655 _refine_ls_goodness_of_fit_ref 0.9591 _refine_ls_shift/su_max 0.0008121 _refine_ls_shift/su_mean 0.0081071 # The values computed from all data _oxford_reflns_number_all 13778 _refine_ls_R_factor_all 0.0399 _refine_ls_wR_factor_all 0.0655 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 10842 _refine_ls_R_factor_gt 0.0272 _refine_ls_wR_factor_gt 0.0612 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment none # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.03P)^2^ + 1.08P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Bruker Analytical X-ray Systems, Inc., 2006. Apex2, Version 2 User Manual, M86-E01078, Madison, WI. De Meulenaer, J. & Tompa, H. (1965). Acta Cryst. 19, 1014. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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 _oxford_atom_site_special_shape _atom_site_attached_hydrogens Zr1 Zr 0.140181(13) 0.237323(11) 0.247693(7) 0.0097 1.0000 Uani . . . . . . . Co1 Co 0.230477(18) 0.081965(16) 0.260591(10) 0.0102 1.0000 Uani . . . . . . . P1 P 0.36821(4) 0.22696(3) 0.23061(2) 0.0114 1.0000 Uani . . . . . . . P2 P 0.15391(4) 0.09386(3) 0.35460(2) 0.0115 1.0000 Uani . . . . . . . P3 P 0.23632(9) -0.08277(6) 0.21131(5) 0.0130 0.958(6) Uani . . P 1 1 . . P301 P 0.206(3) -0.1002(17) 0.2258(13) 0.022(4) 0.042(6) Uiso . . P 1 2 . . N1 N 0.31577(11) 0.34368(10) 0.23319(7) 0.0120 1.0000 Uani . . . . . . . N2 N 0.10901(11) 0.21557(10) 0.35125(7) 0.0117 1.0000 Uani . . . . . . . N3 N -0.03480(12) 0.21668(11) 0.16251(7) 0.0140 1.0000 Uani . . . . . . . C1 C 0.38302(16) 0.20309(13) 0.13442(9) 0.0173 1.0000 Uani . . . . . . . C2 C 0.24919(16) 0.13508(14) 0.07644(9) 0.0211 1.0000 Uani . . . . . . . C3 C 0.47589(17) 0.13793(14) 0.12905(10) 0.0230 1.0000 Uani . . . . . . . C4 C 0.53972(14) 0.26725(13) 0.29122(9) 0.0156 1.0000 Uani . . . . . . . C5 C 0.64001(15) 0.36843(13) 0.27293(10) 0.0201 1.0000 Uani . . . . . . . C6 C 0.55694(15) 0.28109(14) 0.37578(9) 0.0192 1.0000 Uani . . . . . . . C7 C 0.36851(14) 0.45408(12) 0.21143(8) 0.0122 1.0000 Uani . . . . . . . C8 C 0.31805(14) 0.47365(12) 0.13768(8) 0.0142 1.0000 Uani . . . . . . . C9 C 0.37672(15) 0.57915(13) 0.11735(8) 0.0162 1.0000 Uani . . . . . . . C10 C 0.48309(15) 0.66848(12) 0.16678(9) 0.0161 1.0000 Uani . . . . . . . C11 C 0.52405(14) 0.65243(12) 0.24051(8) 0.0153 1.0000 Uani . . . . . . . C12 C 0.46661(14) 0.54959(12) 0.26440(8) 0.0132 1.0000 Uani . . . . . . . C13 C 0.19990(16) 0.38791(14) 0.07888(9) 0.0219 1.0000 Uani . . . . . . . C14 C 0.54699(17) 0.77907(14) 0.14120(10) 0.0238 1.0000 Uani . . . . . . . C15 C 0.50717(15) 0.54897(13) 0.34749(8) 0.0173 1.0000 Uani . . . . . . . C16 C 0.00405(14) -0.02677(12) 0.35194(9) 0.0161 1.0000 Uani . . . . . . . C17 C -0.09626(15) -0.06042(14) 0.27357(9) 0.0204 1.0000 Uani . . . . . . . C18 C 0.03188(17) -0.13554(14) 0.37376(11) 0.0250 1.0000 Uani . . . . . . . C19 C 0.26426(15) 0.11957(14) 0.45362(8) 0.0166 1.0000 Uani . . . . . . . C20 C 0.35290(16) 0.04728(15) 0.46793(9) 0.0226 1.0000 Uani . . . . . . . C21 C 0.19560(18) 0.11164(16) 0.51425(9) 0.0245 1.0000 Uani . . . . . . . C22 C 0.07579(14) 0.27200(12) 0.40801(8) 0.0123 1.0000 Uani . . . . . . . C23 C -0.05369(14) 0.23963(12) 0.40947(8) 0.0141 1.0000 Uani . . . . . . . C24 C -0.07835(15) 0.28900(13) 0.47082(9) 0.0161 1.0000 Uani . . . . . . . C25 C 0.01841(16) 0.37219(13) 0.52890(8) 0.0166 1.0000 Uani . . . . . . . C26 C 0.14262(15) 0.41242(13) 0.52211(8) 0.0162 1.0000 Uani . . . . . . . C27 C 0.17238(14) 0.36586(12) 0.46241(8) 0.0146 1.0000 Uani . . . . . . . C28 C -0.16791(15) 0.15790(14) 0.34572(9) 0.0196 1.0000 Uani . . . . . . . C29 C -0.00956(17) 0.42130(14) 0.59588(9) 0.0205 1.0000 Uani . . . . . . . C30 C 0.30578(16) 0.42055(14) 0.45565(9) 0.0225 1.0000 Uani . . . . . . . C31 C -0.10762(14) 0.28880(12) 0.14446(8) 0.0126 1.0000 Uani . . . . . . . C32 C -0.22604(14) 0.25307(13) 0.08486(8) 0.0151 1.0000 Uani . . . . . . . C33 C -0.29403(15) 0.32914(14) 0.07077(9) 0.0178 1.0000 Uani . . . . . . . C34 C -0.25004(16) 0.44034(14) 0.11286(9) 0.0192 1.0000 Uani . . . . . . . C35 C -0.13288(15) 0.47485(13) 0.17101(9) 0.0177 1.0000 Uani . . . . . . . C36 C -0.06154(14) 0.40155(12) 0.18728(8) 0.0138 1.0000 Uani . . . . . . . C37 C -0.27847(16) 0.13301(14) 0.03811(9) 0.0214 1.0000 Uani . . . . . . . C38 C -0.32831(18) 0.51950(16) 0.09773(11) 0.0282 1.0000 Uani . . . . . . . C39 C 0.06464(15) 0.44127(13) 0.25053(9) 0.0167 1.0000 Uani . . . . . . . C40 C 0.34848(15) -0.15349(13) 0.26267(9) 0.0186 1.0000 Uani . . . . . . . C41 C 0.48710(16) -0.06564(14) 0.29603(10) 0.0226 1.0000 Uani . . . . . . . C42 C 0.30246(18) -0.21475(15) 0.32293(10) 0.0260 1.0000 Uani . . . . . . . C43 C 0.08459(15) -0.20956(13) 0.16167(9) 0.0199 1.0000 Uani . . . . . . . C44 C -0.00711(17) -0.16981(15) 0.10210(10) 0.0259 1.0000 Uani . . . . . . . C45 C 0.10919(18) -0.31198(14) 0.12423(10) 0.0257 1.0000 Uani . . . . . . . H1 H 0.337(2) 0.085(2) 0.3159(13) 0.044(6) 1.0000 Uiso . . . . . . . H2 H 0.1056(19) 0.0765(17) 0.1986(11) 0.027(5) 1.0000 Uiso . . . . . . . H3 H 0.2786(18) -0.0760(16) 0.1522(10) 0.021(5) 1.0000 Uiso . . . . . . . H4 H -0.0688(19) 0.1561(18) 0.1339(11) 0.023(5) 1.0000 Uiso . . . . . . . H11 H 0.4169 0.2791 0.1225 0.0211 1.0000 Uiso R . . . . . . H21 H 0.2222 0.0540 0.0808 0.0316 1.0000 Uiso R . . . . . . H22 H 0.1830 0.1652 0.0829 0.0308 1.0000 Uiso R . . . . . . H23 H 0.2526 0.1400 0.0248 0.0306 1.0000 Uiso R . . . . . . H31 H 0.4677 0.1186 0.0759 0.0347 1.0000 Uiso R . . . . . . H32 H 0.4534 0.0666 0.1485 0.0349 1.0000 Uiso R . . . . . . H33 H 0.5644 0.1813 0.1560 0.0338 1.0000 Uiso R . . . . . . H41 H 0.5581 0.1989 0.2780 0.0176 1.0000 Uiso R . . . . . . H51 H 0.6363 0.4406 0.2900 0.0291 1.0000 Uiso R . . . . . . H52 H 0.6254 0.3619 0.2196 0.0303 1.0000 Uiso R . . . . . . H53 H 0.7277 0.3690 0.2951 0.0305 1.0000 Uiso R . . . . . . H61 H 0.5272 0.2071 0.3899 0.0311 1.0000 Uiso R . . . . . . H62 H 0.5142 0.3269 0.3914 0.0316 1.0000 Uiso R . . . . . . H63 H 0.6456 0.3184 0.4045 0.0310 1.0000 Uiso R . . . . . . H91 H 0.3411 0.5911 0.0696 0.0183 1.0000 Uiso R . . . . . . H111 H 0.5910 0.7128 0.2763 0.0173 1.0000 Uiso R . . . . . . H131 H 0.2230 0.3392 0.0463 0.0338 1.0000 Uiso R . . . . . . H132 H 0.1433 0.3381 0.1011 0.0321 1.0000 Uiso R . . . . . . H133 H 0.1531 0.4288 0.0475 0.0339 1.0000 Uiso R . . . . . . H141 H 0.6105 0.8365 0.1819 0.0368 1.0000 Uiso R . . . . . . H142 H 0.4845 0.8112 0.1171 0.0376 1.0000 Uiso R . . . . . . H143 H 0.5885 0.7674 0.1055 0.0377 1.0000 Uiso R . . . . . . H151 H 0.5979 0.5832 0.3698 0.0278 1.0000 Uiso R . . . . . . H152 H 0.4800 0.4725 0.3582 0.0264 1.0000 Uiso R . . . . . . H153 H 0.4703 0.5931 0.3711 0.0269 1.0000 Uiso R . . . . . . H161 H -0.0300 0.0029 0.3885 0.0189 1.0000 Uiso R . . . . . . H171 H -0.0684 -0.1021 0.2387 0.0300 1.0000 Uiso R . . . . . . H172 H -0.1061 0.0077 0.2537 0.0295 1.0000 Uiso R . . . . . . H173 H -0.1796 -0.1118 0.2763 0.0316 1.0000 Uiso R . . . . . . H181 H 0.0743 -0.1594 0.3414 0.0357 1.0000 Uiso R . . . . . . H182 H 0.0868 -0.1224 0.4255 0.0363 1.0000 Uiso R . . . . . . H183 H -0.0494 -0.1983 0.3675 0.0371 1.0000 Uiso R . . . . . . H191 H 0.3217 0.2001 0.4594 0.0193 1.0000 Uiso R . . . . . . H201 H 0.3045 -0.0317 0.4689 0.0333 1.0000 Uiso R . . . . . . H202 H 0.3965 0.0468 0.4303 0.0326 1.0000 Uiso R . . . . . . H203 H 0.4189 0.0793 0.5165 0.0331 1.0000 Uiso R . . . . . . H211 H 0.2604 0.1428 0.5629 0.0371 1.0000 Uiso R . . . . . . H212 H 0.1462 0.0310 0.5138 0.0364 1.0000 Uiso R . . . . . . H213 H 0.1352 0.1533 0.5072 0.0352 1.0000 Uiso R . . . . . . H241 H -0.1624 0.2662 0.4725 0.0190 1.0000 Uiso R . . . . . . H261 H 0.2081 0.4722 0.5578 0.0196 1.0000 Uiso R . . . . . . H281 H -0.1844 0.0776 0.3512 0.0282 1.0000 Uiso R . . . . . . H282 H -0.1526 0.1673 0.2987 0.0276 1.0000 Uiso R . . . . . . H283 H -0.2454 0.1742 0.3447 0.0286 1.0000 Uiso R . . . . . . H291 H 0.0096 0.5006 0.6001 0.0311 1.0000 Uiso R . . . . . . H292 H 0.0401 0.4086 0.6416 0.0319 1.0000 Uiso R . . . . . . H293 H -0.0983 0.3883 0.5918 0.0317 1.0000 Uiso R . . . . . . H301 H 0.3102 0.4055 0.4081 0.0367 1.0000 Uiso R . . . . . . H302 H 0.3419 0.5005 0.4736 0.0364 1.0000 Uiso R . . . . . . H303 H 0.3655 0.3906 0.4848 0.0371 1.0000 Uiso R . . . . . . H331 H -0.3756 0.3028 0.0318 0.0202 1.0000 Uiso R . . . . . . H351 H -0.1015 0.5483 0.2000 0.0204 1.0000 Uiso R . . . . . . H371 H -0.2163 0.1213 0.0147 0.0309 1.0000 Uiso R . . . . . . H372 H -0.3587 0.1217 -0.0007 0.0316 1.0000 Uiso R . . . . . . H373 H -0.2954 0.0737 0.0693 0.0319 1.0000 Uiso R . . . . . . H381 H -0.3969 0.5033 0.1188 0.0452 1.0000 Uiso R . . . . . . H382 H -0.2755 0.5957 0.1168 0.0456 1.0000 Uiso R . . . . . . H383 H -0.3664 0.5186 0.0458 0.0451 1.0000 Uiso R . . . . . . H391 H 0.1356 0.4373 0.2317 0.0235 1.0000 Uiso R . . . . . . H392 H 0.0878 0.5218 0.2742 0.0238 1.0000 Uiso R . . . . . . H393 H 0.0608 0.3947 0.2892 0.0245 1.0000 Uiso R . . . . . . H401 H 0.3468 -0.2120 0.2248 0.0209 1.0000 Uiso R . . . . . . H411 H 0.5180 -0.0300 0.2567 0.0333 1.0000 Uiso R . . . . . . H412 H 0.5464 -0.1044 0.3193 0.0337 1.0000 Uiso R . . . . . . H413 H 0.4920 -0.0061 0.3334 0.0330 1.0000 Uiso R . . . . . . H421 H 0.3582 -0.2553 0.3439 0.0393 1.0000 Uiso R . . . . . . H422 H 0.3036 -0.1610 0.3628 0.0370 1.0000 Uiso R . . . . . . H423 H 0.2159 -0.2700 0.3032 0.0380 1.0000 Uiso R . . . . . . H431 H 0.0399 -0.2375 0.1986 0.0239 1.0000 Uiso R . . . . . . H441 H -0.0913 -0.2312 0.0785 0.0384 1.0000 Uiso R . . . . . . H442 H -0.0197 -0.1023 0.1229 0.0378 1.0000 Uiso R . . . . . . H443 H 0.0304 -0.1512 0.0626 0.0366 1.0000 Uiso R . . . . . . H451 H 0.1578 -0.2852 0.0917 0.0351 1.0000 Uiso R . . . . . . H452 H 0.0262 -0.3710 0.0962 0.0363 1.0000 Uiso R . . . . . . H453 H 0.1559 -0.3455 0.1608 0.0372 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 Zr1 0.01072(6) 0.00952(6) 0.01001(6) 0.00212(5) 0.00306(5) 0.00502(5) Co1 0.01075(9) 0.00956(8) 0.01109(9) 0.00206(7) 0.00320(7) 0.00469(7) P1 0.01216(16) 0.01089(15) 0.01263(16) 0.00250(13) 0.00502(13) 0.00508(13) P2 0.01276(16) 0.01207(16) 0.01205(16) 0.00412(13) 0.00472(13) 0.00625(13) P3 0.0139(3) 0.0101(2) 0.0159(3) 0.00160(17) 0.0053(2) 0.00520(19) N1 0.0135(6) 0.0105(5) 0.0130(6) 0.0024(4) 0.0048(5) 0.0050(4) N2 0.0128(5) 0.0121(5) 0.0124(5) 0.0020(4) 0.0051(4) 0.0063(4) N3 0.0152(6) 0.0121(6) 0.0139(6) -0.0003(5) 0.0010(5) 0.0075(5) C1 0.0245(8) 0.0141(7) 0.0177(7) 0.0045(6) 0.0119(6) 0.0077(6) C2 0.0283(8) 0.0217(7) 0.0134(7) 0.0021(6) 0.0059(6) 0.0095(6) C3 0.0263(8) 0.0195(7) 0.0286(9) 0.0020(6) 0.0179(7) 0.0077(6) C4 0.0118(6) 0.0138(6) 0.0223(7) 0.0036(6) 0.0054(6) 0.0058(5) C5 0.0143(7) 0.0185(7) 0.0287(8) 0.0035(6) 0.0091(6) 0.0054(6) C6 0.0175(7) 0.0188(7) 0.0182(7) 0.0030(6) 0.0002(6) 0.0071(6) C7 0.0132(6) 0.0116(6) 0.0143(6) 0.0031(5) 0.0065(5) 0.0058(5) C8 0.0150(7) 0.0141(6) 0.0153(7) 0.0033(5) 0.0052(5) 0.0069(5) C9 0.0199(7) 0.0167(7) 0.0148(7) 0.0058(5) 0.0057(6) 0.0093(6) C10 0.0184(7) 0.0125(6) 0.0212(7) 0.0056(6) 0.0092(6) 0.0076(5) C11 0.0157(7) 0.0123(6) 0.0183(7) 0.0017(5) 0.0056(6) 0.0055(5) C12 0.0145(7) 0.0132(6) 0.0139(6) 0.0025(5) 0.0048(5) 0.0073(5) C13 0.0235(8) 0.0189(7) 0.0165(7) 0.0054(6) 0.0002(6) 0.0031(6) C14 0.0274(9) 0.0166(7) 0.0241(8) 0.0075(6) 0.0079(7) 0.0026(6) C15 0.0205(7) 0.0151(7) 0.0151(7) 0.0024(5) 0.0044(6) 0.0059(6) C16 0.0169(7) 0.0137(6) 0.0215(7) 0.0060(6) 0.0100(6) 0.0063(5) C17 0.0166(7) 0.0166(7) 0.0251(8) 0.0006(6) 0.0069(6) 0.0025(6) C18 0.0266(9) 0.0185(7) 0.0374(10) 0.0143(7) 0.0163(8) 0.0107(7) C19 0.0187(7) 0.0204(7) 0.0130(6) 0.0050(6) 0.0047(6) 0.0097(6) C20 0.0232(8) 0.0311(9) 0.0189(7) 0.0100(7) 0.0052(6) 0.0168(7) C21 0.0339(9) 0.0334(9) 0.0156(7) 0.0104(7) 0.0105(7) 0.0208(8) C22 0.0161(7) 0.0135(6) 0.0109(6) 0.0042(5) 0.0056(5) 0.0083(5) C23 0.0143(7) 0.0130(6) 0.0167(7) 0.0043(5) 0.0046(5) 0.0069(5) C24 0.0163(7) 0.0177(7) 0.0202(7) 0.0074(6) 0.0102(6) 0.0093(6) C25 0.0257(8) 0.0162(7) 0.0155(7) 0.0067(6) 0.0111(6) 0.0128(6) C26 0.0214(7) 0.0134(6) 0.0130(7) 0.0010(5) 0.0047(6) 0.0059(6) C27 0.0152(7) 0.0154(6) 0.0145(7) 0.0040(5) 0.0056(5) 0.0062(5) C28 0.0139(7) 0.0215(7) 0.0223(8) -0.0003(6) 0.0034(6) 0.0077(6) C29 0.0320(9) 0.0197(7) 0.0179(7) 0.0047(6) 0.0145(7) 0.0139(7) C30 0.0181(7) 0.0231(8) 0.0217(8) -0.0030(6) 0.0087(6) 0.0007(6) C31 0.0142(6) 0.0144(6) 0.0125(6) 0.0053(5) 0.0062(5) 0.0070(5) C32 0.0150(7) 0.0192(7) 0.0127(6) 0.0048(5) 0.0050(5) 0.0073(6) C33 0.0146(7) 0.0267(8) 0.0165(7) 0.0103(6) 0.0058(6) 0.0106(6) C34 0.0219(8) 0.0242(8) 0.0224(8) 0.0140(6) 0.0129(6) 0.0155(6) C35 0.0230(8) 0.0166(7) 0.0209(7) 0.0075(6) 0.0131(6) 0.0108(6) C36 0.0146(7) 0.0148(6) 0.0143(6) 0.0042(5) 0.0062(5) 0.0064(5) C37 0.0178(7) 0.0232(8) 0.0185(7) -0.0011(6) -0.0001(6) 0.0072(6) C38 0.0332(10) 0.0337(9) 0.0331(9) 0.0157(8) 0.0152(8) 0.0260(8) C39 0.0203(7) 0.0132(6) 0.0172(7) 0.0016(5) 0.0042(6) 0.0085(6) C40 0.0208(7) 0.0155(7) 0.0224(8) 0.0029(6) 0.0065(6) 0.0107(6) C41 0.0194(8) 0.0213(8) 0.0284(9) 0.0027(7) 0.0040(7) 0.0120(6) C42 0.0321(9) 0.0215(8) 0.0310(9) 0.0102(7) 0.0116(8) 0.0153(7) C43 0.0203(8) 0.0149(7) 0.0218(8) -0.0008(6) 0.0070(6) 0.0034(6) C44 0.0231(8) 0.0219(8) 0.0246(8) -0.0040(7) -0.0009(7) 0.0064(7) C45 0.0299(9) 0.0155(7) 0.0294(9) -0.0025(7) 0.0098(7) 0.0060(7) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.125626(18) 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 Zr1 . Co1 . 2.4397(2) yes Zr1 . P1 . 2.7460(4) yes Zr1 . P2 . 2.7745(4) yes Zr1 . N1 . 2.1180(12) yes Zr1 . N2 . 2.0895(12) yes Zr1 . N3 . 2.1142(12) yes Zr1 . C39 . 2.9005(15) yes Zr1 . H2 . 1.987(19) no Co1 . P1 . 2.1963(4) yes Co1 . P2 . 2.1856(4) yes Co1 . P3 . 2.1910(5) yes Co1 . H1 . 1.36(2) no Co1 . H2 . 1.551(19) no Co1 . P1 . 2.1963(4) yes Co1 . P2 . 2.1856(4) yes Co1 . P301 . 2.194(15) yes Co1 . H1 . 1.36(2) no Co1 . H2 . 1.551(19) no P1 . N1 . 1.7236(12) yes P1 . C1 . 1.8673(15) yes P1 . C4 . 1.8563(15) yes P2 . N2 . 1.7292(12) yes P2 . C16 . 1.8598(15) yes P2 . C19 . 1.8737(15) yes P3 . C40 . 1.8649(16) yes P3 . C43 . 1.8655(17) yes P3 . H3 . 1.322(19) no P301 . C40 . 1.913(17) yes P301 . C43 . 1.686(17) yes N1 . C7 . 1.4397(17) yes N2 . C22 . 1.4263(18) yes N3 . C31 . 1.3964(18) yes N3 . H4 . 0.80(2) no C1 . C2 . 1.535(2) yes C1 . C3 . 1.536(2) yes C1 . H11 . 0.961 no C2 . H21 . 0.963 no C2 . H22 . 0.972 no C2 . H23 . 0.986 no C3 . H31 . 0.978 no C3 . H32 . 0.962 no C3 . H33 . 0.947 no C4 . C5 . 1.534(2) yes C4 . C6 . 1.533(2) yes C4 . H41 . 0.960 no C5 . H51 . 0.939 no C5 . H52 . 0.961 no C5 . H53 . 0.969 no C6 . H61 . 0.951 no C6 . H62 . 0.932 no C6 . H63 . 0.945 no C7 . C8 . 1.416(2) yes C7 . C12 . 1.4142(19) yes C8 . C9 . 1.393(2) yes C8 . C13 . 1.501(2) yes C9 . C10 . 1.387(2) yes C9 . H91 . 0.921 no C10 . C11 . 1.384(2) yes C10 . C14 . 1.508(2) yes C11 . C12 . 1.397(2) yes C11 . H111 . 0.932 no C12 . C15 . 1.501(2) yes C13 . H131 . 0.966 no C13 . H132 . 0.949 no C13 . H133 . 0.963 no C14 . H141 . 0.947 no C14 . H142 . 0.948 no C14 . H143 . 0.946 no C15 . H151 . 0.940 no C15 . H152 . 0.949 no C15 . H153 . 0.937 no C16 . C17 . 1.525(2) yes C16 . C18 . 1.530(2) yes C16 . H161 . 0.976 no C17 . H171 . 0.979 no C17 . H172 . 0.968 no C17 . H173 . 0.977 no C18 . H181 . 0.956 no C18 . H182 . 0.969 no C18 . H183 . 0.971 no C19 . C20 . 1.530(2) yes C19 . C21 . 1.540(2) yes C19 . H191 . 0.978 no C20 . H201 . 0.957 no C20 . H202 . 0.969 no C20 . H203 . 0.966 no C21 . H211 . 0.961 no C21 . H212 . 0.971 no C21 . H213 . 0.969 no C22 . C23 . 1.411(2) yes C22 . C27 . 1.410(2) yes C23 . C24 . 1.397(2) yes C23 . C28 . 1.507(2) yes C24 . C25 . 1.381(2) yes C24 . H241 . 0.919 no C25 . C26 . 1.390(2) yes C25 . C29 . 1.507(2) yes C26 . C27 . 1.390(2) yes C26 . H261 . 0.922 no C27 . C30 . 1.501(2) yes C28 . H281 . 0.964 no C28 . H282 . 0.953 no C28 . H283 . 0.961 no C29 . H291 . 0.921 no C29 . H292 . 0.944 no C29 . H293 . 0.942 no C30 . H301 . 0.914 no C30 . H302 . 0.931 no C30 . H303 . 0.940 no C31 . C32 . 1.410(2) yes C31 . C36 . 1.408(2) yes C32 . C33 . 1.390(2) yes C32 . C37 . 1.505(2) yes C33 . C34 . 1.389(2) yes C33 . H331 . 0.951 no C34 . C35 . 1.388(2) yes C34 . C38 . 1.510(2) yes C35 . C36 . 1.392(2) yes C35 . H351 . 0.924 no C36 . C39 . 1.499(2) yes C37 . H371 . 0.970 no C37 . H372 . 0.962 no C37 . H373 . 0.974 no C38 . H381 . 0.944 no C38 . H382 . 0.918 no C38 . H383 . 0.950 no C39 . H391 . 0.981 no C39 . H392 . 0.975 no C39 . H393 . 0.960 no C40 . C41 . 1.527(2) yes C40 . C42 . 1.524(2) yes C40 . H401 . 0.964 no C40 . C41 . 1.527(2) yes C40 . C42 . 1.524(2) yes C40 . H401 . 0.964 no C41 . H411 . 0.977 no C41 . H412 . 0.975 no C41 . H413 . 0.952 no C42 . H421 . 0.950 no C42 . H422 . 0.954 no C42 . H423 . 0.954 no C43 . C44 . 1.532(2) yes C43 . C45 . 1.535(2) yes C43 . H431 . 0.988 no C43 . C44 . 1.532(2) yes C43 . C45 . 1.535(2) yes C43 . H431 . 0.988 no C44 . H441 . 0.972 no C44 . H442 . 0.958 no C44 . H443 . 0.960 no C45 . H451 . 0.943 no C45 . H452 . 0.966 no C45 . H453 . 0.951 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 Co1 . Zr1 . P1 . 49.684(9) yes Co1 . Zr1 . P2 . 49.049(9) yes P1 . Zr1 . P2 . 89.898(11) yes Co1 . Zr1 . N1 . 88.20(3) yes P2 . Zr1 . N1 . 118.54(3) yes Co1 . Zr1 . N2 . 87.20(3) yes P1 . Zr1 . N2 . 118.16(3) yes N1 . Zr1 . N2 . 125.37(5) yes Co1 . Zr1 . N3 . 121.90(3) yes P1 . Zr1 . N3 . 128.01(4) yes P2 . Zr1 . N3 . 122.85(4) yes N1 . Zr1 . N3 . 116.87(5) yes N2 . Zr1 . N3 . 111.41(5) yes Co1 . Zr1 . C39 . 171.86(3) yes P1 . Zr1 . C39 . 126.44(3) yes P2 . Zr1 . C39 . 128.09(3) yes N1 . Zr1 . C39 . 87.57(4) yes N2 . Zr1 . C39 . 89.59(4) yes P1 . Zr1 . H2 . 71.8(6) no P2 . Zr1 . H2 . 69.9(6) no N1 . Zr1 . H2 . 106.3(6) no N2 . Zr1 . H2 . 103.7(6) no N3 . Zr1 . C39 . 66.24(4) yes N3 . Zr1 . H2 . 82.6(6) no C39 . Zr1 . H2 . 148.8(6) no Zr1 . Co1 . P1 . 72.430(11) yes Zr1 . Co1 . P2 . 73.487(11) yes P1 . Co1 . P2 . 125.761(16) yes Zr1 . Co1 . P3 . 148.937(16) yes P1 . Co1 . P3 . 109.07(4) yes P2 . Co1 . P3 . 121.76(4) yes Zr1 . Co1 . H1 . 125.9(10) no P1 . Co1 . H1 . 84.4(9) no P2 . Co1 . H1 . 82.9(10) no P3 . Co1 . H1 . 84.5(10) no Zr1 . Co1 . H2 . 54.4(7) no P1 . Co1 . H2 . 97.3(7) no P2 . Co1 . H2 . 95.7(7) no P3 . Co1 . H2 . 95.4(7) no H1 . Co1 . H2 . 178.3(12) no Zr1 . Co1 . P1 . 72.430(11) yes Zr1 . Co1 . P2 . 73.487(11) yes P1 . Co1 . P2 . 125.761(16) yes Zr1 . Co1 . P301 . 148.4(4) yes P1 . Co1 . P301 . 122.1(10) yes P2 . Co1 . P301 . 109.0(9) yes Zr1 . Co1 . H1 . 125.9(10) no P1 . Co1 . H1 . 84.4(9) no P2 . Co1 . H1 . 82.9(10) no P301 . Co1 . H1 . 85.2(10) no P1 . Co1 . H2 . 97.3(7) no P2 . Co1 . H2 . 95.7(7) no P301 . Co1 . H2 . 94.4(8) no H1 . Co1 . H2 . 178.3(12) no Zr1 . P1 . Co1 . 57.885(10) yes Zr1 . P1 . N1 . 50.47(4) yes Co1 . P1 . N1 . 107.83(4) yes Zr1 . P1 . C1 . 120.18(5) yes Co1 . P1 . C1 . 116.65(5) yes N1 . P1 . C1 . 105.18(6) yes Zr1 . P1 . C4 . 136.77(5) yes Co1 . P1 . C4 . 113.78(5) yes N1 . P1 . C4 . 111.34(6) yes C1 . P1 . C4 . 101.71(7) yes Zr1 . P2 . Co1 . 57.464(10) yes Zr1 . P2 . N2 . 48.79(4) yes Co1 . P2 . N2 . 105.76(4) yes Zr1 . P2 . C16 . 119.32(5) yes Co1 . P2 . C16 . 117.34(5) yes N2 . P2 . C16 . 104.60(6) yes Zr1 . P2 . C19 . 132.02(5) yes Co1 . P2 . C19 . 119.63(5) yes N2 . P2 . C19 . 103.57(6) yes C16 . P2 . C19 . 104.18(7) yes Co1 . P3 . C40 . 122.42(5) yes Co1 . P3 . C43 . 121.80(7) yes C40 . P3 . C43 . 102.67(8) yes Co1 . P3 . H3 . 113.9(8) no C40 . P3 . H3 . 95.6(8) no C43 . P3 . H3 . 94.1(8) no Co1 . P301 . C40 . 119.9(9) yes Co1 . P301 . C43 . 131.8(8) yes C40 . P301 . C43 . 107.9(7) yes P1 . N1 . Zr1 . 90.66(5) yes P1 . N1 . C7 . 127.73(9) yes Zr1 . N1 . C7 . 139.46(9) yes P2 . N2 . Zr1 . 92.71(5) yes P2 . N2 . C22 . 126.99(9) yes Zr1 . N2 . C22 . 140.12(9) yes Zr1 . N3 . C31 . 133.16(10) yes Zr1 . N3 . H4 . 116.6(14) no C31 . N3 . H4 . 110.3(14) no P1 . C1 . C2 . 110.64(11) yes P1 . C1 . C3 . 113.72(11) yes C2 . C1 . C3 . 108.36(13) yes P1 . C1 . H11 . 106.3 no C2 . C1 . H11 . 109.3 no C3 . C1 . H11 . 108.4 no C1 . C2 . H21 . 110.5 no C1 . C2 . H22 . 111.8 no H21 . C2 . H22 . 108.4 no C1 . C2 . H23 . 110.6 no H21 . C2 . H23 . 107.7 no H22 . C2 . H23 . 107.7 no C1 . C3 . H31 . 108.3 no C1 . C3 . H32 . 110.9 no H31 . C3 . H32 . 108.3 no C1 . C3 . H33 . 113.7 no H31 . C3 . H33 . 108.6 no H32 . C3 . H33 . 106.9 no P1 . C4 . C5 . 115.95(11) yes P1 . C4 . C6 . 113.85(10) yes C5 . C4 . C6 . 111.72(12) yes P1 . C4 . H41 . 101.3 no C5 . C4 . H41 . 105.8 no C6 . C4 . H41 . 106.9 no C4 . C5 . H51 . 111.6 no C4 . C5 . H52 . 111.4 no H51 . C5 . H52 . 107.2 no C4 . C5 . H53 . 111.2 no H51 . C5 . H53 . 108.9 no H52 . C5 . H53 . 106.3 no C4 . C6 . H61 . 110.6 no C4 . C6 . H62 . 114.0 no H61 . C6 . H62 . 108.4 no C4 . C6 . H63 . 110.9 no H61 . C6 . H63 . 107.7 no H62 . C6 . H63 . 105.1 no N1 . C7 . C8 . 121.34(12) yes N1 . C7 . C12 . 121.14(12) yes C8 . C7 . C12 . 117.38(12) yes C7 . C8 . C9 . 119.67(13) yes C7 . C8 . C13 . 123.82(13) yes C9 . C8 . C13 . 116.48(13) yes C8 . C9 . C10 . 122.90(14) yes C8 . C9 . H91 . 118.4 no C10 . C9 . H91 . 118.6 no C9 . C10 . C11 . 116.81(13) yes C9 . C10 . C14 . 120.97(14) yes C11 . C10 . C14 . 122.18(14) yes C10 . C11 . C12 . 122.53(14) yes C10 . C11 . H111 . 119.4 no C12 . C11 . H111 . 118.1 no C7 . C12 . C11 . 119.91(13) yes C7 . C12 . C15 . 122.68(13) yes C11 . C12 . C15 . 117.29(13) yes C8 . C13 . H131 . 111.8 no C8 . C13 . H132 . 111.4 no H131 . C13 . H132 . 107.5 no C8 . C13 . H133 . 109.8 no H131 . C13 . H133 . 107.3 no H132 . C13 . H133 . 108.9 no C10 . C14 . H141 . 112.0 no C10 . C14 . H142 . 110.9 no H141 . C14 . H142 . 107.7 no C10 . C14 . H143 . 113.1 no H141 . C14 . H143 . 107.2 no H142 . C14 . H143 . 105.6 no C12 . C15 . H151 . 111.8 no C12 . C15 . H152 . 111.9 no H151 . C15 . H152 . 108.4 no C12 . C15 . H153 . 109.6 no H151 . C15 . H153 . 106.6 no H152 . C15 . H153 . 108.3 no P2 . C16 . C17 . 110.87(10) yes P2 . C16 . C18 . 112.39(11) yes C17 . C16 . C18 . 108.34(13) yes P2 . C16 . H161 . 105.9 no C17 . C16 . H161 . 110.2 no C18 . C16 . H161 . 109.2 no C16 . C17 . H171 . 110.0 no C16 . C17 . H172 . 111.3 no H171 . C17 . H172 . 107.4 no C16 . C17 . H173 . 109.0 no H171 . C17 . H173 . 108.7 no H172 . C17 . H173 . 110.3 no C16 . C18 . H181 . 109.1 no C16 . C18 . H182 . 112.6 no H181 . C18 . H182 . 108.5 no C16 . C18 . H183 . 109.8 no H181 . C18 . H183 . 108.5 no H182 . C18 . H183 . 108.2 no P2 . C19 . C20 . 115.95(11) yes P2 . C19 . C21 . 114.70(11) yes C20 . C19 . C21 . 109.01(12) yes P2 . C19 . H191 . 101.5 no C20 . C19 . H191 . 106.0 no C21 . C19 . H191 . 108.8 no C19 . C20 . H201 . 110.9 no C19 . C20 . H202 . 112.7 no H201 . C20 . H202 . 108.2 no C19 . C20 . H203 . 109.2 no H201 . C20 . H203 . 107.7 no H202 . C20 . H203 . 108.0 no C19 . C21 . H211 . 108.8 no C19 . C21 . H212 . 110.4 no H211 . C21 . H212 . 108.3 no C19 . C21 . H213 . 113.1 no H211 . C21 . H213 . 108.9 no H212 . C21 . H213 . 107.1 no N2 . C22 . C23 . 121.55(12) yes N2 . C22 . C27 . 119.97(13) yes C23 . C22 . C27 . 118.42(13) yes C22 . C23 . C24 . 118.96(13) yes C22 . C23 . C28 . 122.69(13) yes C24 . C23 . C28 . 118.29(13) yes C23 . C24 . C25 . 122.62(14) yes C23 . C24 . H241 . 119.0 no C25 . C24 . H241 . 118.4 no C24 . C25 . C26 . 117.39(13) yes C24 . C25 . C29 . 121.74(14) yes C26 . C25 . C29 . 120.83(14) yes C25 . C26 . C27 . 122.10(14) yes C25 . C26 . H261 . 119.8 no C27 . C26 . H261 . 118.1 no C22 . C27 . C26 . 119.65(13) yes C22 . C27 . C30 . 121.45(13) yes C26 . C27 . C30 . 118.85(13) yes C23 . C28 . H281 . 111.8 no C23 . C28 . H282 . 110.3 no H281 . C28 . H282 . 108.6 no C23 . C28 . H283 . 109.9 no H281 . C28 . H283 . 107.5 no H282 . C28 . H283 . 108.5 no C25 . C29 . H291 . 111.5 no C25 . C29 . H292 . 112.0 no H291 . C29 . H292 . 106.8 no C25 . C29 . H293 . 111.4 no H291 . C29 . H293 . 106.6 no H292 . C29 . H293 . 108.2 no C27 . C30 . H301 . 114.1 no C27 . C30 . H302 . 113.2 no H301 . C30 . H302 . 109.6 no C27 . C30 . H303 . 111.4 no H301 . C30 . H303 . 103.3 no H302 . C30 . H303 . 104.4 no N3 . C31 . C32 . 122.51(13) yes N3 . C31 . C36 . 118.97(13) yes C32 . C31 . C36 . 118.52(13) yes C31 . C32 . C33 . 119.30(14) yes C31 . C32 . C37 . 119.96(13) yes C33 . C32 . C37 . 120.74(13) yes C32 . C33 . C34 . 122.76(14) yes C32 . C33 . H331 . 118.5 no C34 . C33 . H331 . 118.7 no C33 . C34 . C35 . 117.41(14) yes C33 . C34 . C38 . 121.48(15) yes C35 . C34 . C38 . 121.08(15) yes C34 . C35 . C36 . 121.84(14) yes C34 . C35 . H351 . 119.2 no C36 . C35 . H351 . 118.9 no C31 . C36 . C35 . 120.17(13) yes C31 . C36 . C39 . 119.23(13) yes C35 . C36 . C39 . 120.59(13) yes C32 . C37 . H371 . 110.8 no C32 . C37 . H372 . 110.5 no H371 . C37 . H372 . 108.8 no C32 . C37 . H373 . 110.6 no H371 . C37 . H373 . 107.8 no H372 . C37 . H373 . 108.3 no C34 . C38 . H381 . 114.0 no C34 . C38 . H382 . 110.4 no H381 . C38 . H382 . 107.2 no C34 . C38 . H383 . 114.0 no H381 . C38 . H383 . 106.2 no H382 . C38 . H383 . 104.4 no C36 . C39 . Zr1 . 102.35(9) yes C36 . C39 . H391 . 110.4 no Zr1 . C39 . H391 . 57.6 no C36 . C39 . H392 . 111.3 no Zr1 . C39 . H392 . 146.3 no H391 . C39 . H392 . 107.4 no C36 . C39 . H393 . 112.0 no Zr1 . C39 . H393 . 58.7 no H391 . C39 . H393 . 108.3 no H392 . C39 . H393 . 107.2 no P3 . C40 . C41 . 110.75(11) yes P3 . C40 . C42 . 112.89(12) yes C41 . C40 . C42 . 111.03(14) yes P3 . C40 . H401 . 105.0 no C41 . C40 . H401 . 109.1 no C42 . C40 . H401 . 107.8 no P301 . C40 . C41 . 119.9(7) yes P301 . C40 . C42 . 97.8(11) yes C41 . C40 . C42 . 111.03(14) yes P301 . C40 . H401 . 110.2 no C41 . C40 . H401 . 109.1 no C42 . C40 . H401 . 107.8 no C40 . C41 . H411 . 110.7 no C40 . C41 . H412 . 110.3 no H411 . C41 . H412 . 107.1 no C40 . C41 . H413 . 111.3 no H411 . C41 . H413 . 109.1 no H412 . C41 . H413 . 108.2 no C40 . C42 . H421 . 109.4 no C40 . C42 . H422 . 111.9 no H421 . C42 . H422 . 108.1 no C40 . C42 . H423 . 112.3 no H421 . C42 . H423 . 107.8 no H422 . C42 . H423 . 107.2 no P3 . C43 . C44 . 109.30(11) yes P3 . C43 . C45 . 113.63(12) yes C44 . C43 . C45 . 109.41(14) yes P3 . C43 . H431 . 108.6 no C44 . C43 . H431 . 107.5 no C45 . C43 . H431 . 108.2 no P301 . C43 . C44 . 114.5(6) yes P301 . C43 . C45 . 121.5(7) yes C44 . C43 . C45 . 109.41(14) yes P301 . C43 . H431 . 93.5 no C44 . C43 . H431 . 107.5 no C45 . C43 . H431 . 108.2 no C43 . C44 . H441 . 112.1 no C43 . C44 . H442 . 111.6 no H441 . C44 . H442 . 109.3 no C43 . C44 . H443 . 108.6 no H441 . C44 . H443 . 106.3 no H442 . C44 . H443 . 108.8 no C43 . C45 . H451 . 109.1 no C43 . C45 . H452 . 108.7 no H451 . C45 . H452 . 110.3 no C43 . C45 . H453 . 111.3 no H451 . C45 . H453 . 109.1 no H452 . C45 . H453 . 108.4 no Zr1 . H2 . Co1 . 86.3(9) no #===END