# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_4 _audit_creation_date 12-07-16 _audit_creation_method CRYSTALS_ver_14.41 _oxford_structure_analysis_title 'ZW_570_0ma in P2(1)/c' _vrf_PLAT201_4 ; PLAT201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) ....... 3 RESPONSE: Disordered carbon atoms in the isopropyl groups were refined by using isotropic displacement parameters. ; _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 22.9948(17) _cell_length_b 22.4923(17) _cell_length_c 19.5321(14) _cell_angle_alpha 90 _cell_angle_beta 106.602(4) _cell_angle_gamma 90 _cell_volume 9681.0(13) _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-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' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol 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 8 # Given Formula = C46 H77 Co1 N5 O1 P3 Zr1 # Dc = 1.32 Fooo = 4064.00 Mu = 6.96 M = 1918.45 # Found Formula = C46 H77 Co1 N5 O1 P3 Zr1 # Dc = 1.32 FOOO = 4064.00 Mu = 6.96 M = 1918.45 _chemical_formula_sum 'C46 H77 Co1 N5 O1 P3 Zr1' _chemical_formula_moiety 'C46 H77 Co1 N5 O1 P3 Zr1' _chemical_compound_source ? _chemical_formula_weight 959.22 _cell_measurement_reflns_used 9917 _cell_measurement_theta_min 3 _cell_measurement_theta_max 29 _cell_measurement_temperature 120 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_min 0.160 _exptl_crystal_size_mid 0.340 _exptl_crystal_size_max 0.340 _exptl_crystal_density_diffrn 1.316 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 4064 _exptl_absorpt_coefficient_mu 0.696 # Sheldrick geometric approximatio 0.79 0.89 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Analytical Absorption (De Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_min 0.79 _exptl_absorpt_correction_T_max 0.89 _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 110797 _reflns_number_total 25761 _diffrn_reflns_av_R_equivalents 0.071 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 25761 # Theoretical number of reflections is about 51926 _diffrn_reflns_theta_min 1.848 _diffrn_reflns_theta_max 29.091 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 28.509 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 26 _reflns_limit_h_min -31 _reflns_limit_h_max 30 _reflns_limit_k_min 0 _reflns_limit_k_max 30 _reflns_limit_l_min 0 _reflns_limit_l_max 26 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -1.16 _refine_diff_density_max 1.63 # 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 25761 _refine_ls_number_restraints 0 _refine_ls_number_parameters 1025 _oxford_refine_ls_R_factor_ref 0.0835 _refine_ls_wR_factor_ref 0.1006 _refine_ls_goodness_of_fit_ref 1.0000 _refine_ls_shift/su_max 0.0141503 _refine_ls_shift/su_mean 0.0024257 # The values computed with all filters except I/sigma _oxford_reflns_number_all 25761 _refine_ls_R_factor_all 0.0835 _refine_ls_wR_factor_all 0.1006 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 15829 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_gt 0.0805 # 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 constr #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^ + 9.30P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached 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 _atom_site_attached_hydrogens Zr1 Zr 0.471353(11) 0.668995(11) 0.299413(12) 0.0148 1.0000 Uani . . . . . . Zr101 Zr 0.970095(11) 0.679094(11) 0.288162(12) 0.0151 1.0000 Uani . . . . . . Co1 Co 0.578682(16) 0.676913(15) 0.326872(17) 0.0151 1.0000 Uani . . . . . . Co101 Co 1.078008(15) 0.683949(15) 0.316631(17) 0.0136 1.0000 Uani . . . . . . P1 P 0.54741(3) 0.77085(3) 0.32755(4) 0.0183 1.0000 Uani . . . . . . P2 P 0.55912(3) 0.62811(3) 0.41818(3) 0.0162 1.0000 Uani . . . . . . P3 P 0.54860(3) 0.62877(3) 0.22295(3) 0.0175 1.0000 Uani . . . . . . P101 P 1.04737(3) 0.64131(3) 0.20970(3) 0.0153 1.0000 Uani . . . . . . P102 P 1.04817(3) 0.77755(3) 0.32436(3) 0.0165 1.0000 Uani . . . . . . P103 P 1.05674(3) 0.62912(3) 0.40188(3) 0.0156 1.0000 Uani . . . . . . O1 O 0.36797(8) 0.67688(8) 0.24123(9) 0.0197 1.0000 Uani . . . . . . O101 O 0.86658(9) 0.68948(9) 0.23263(10) 0.0277 1.0000 Uani . . . . . . N1 N 0.47133(10) 0.76415(10) 0.30436(12) 0.0221 1.0000 Uani . . . . . . N2 N 0.48274(10) 0.62507(10) 0.39602(11) 0.0184 1.0000 Uani . . . . . . N3 N 0.47491(10) 0.61176(10) 0.21268(11) 0.0191 1.0000 Uani . . . . . . N4 N 0.66216(11) 0.68012(10) 0.35000(12) 0.0213 1.0000 Uani . . . . . . N5 N 0.71244(12) 0.68225(12) 0.36458(14) 0.0334 1.0000 Uani . . . . . . N101 N 0.97323(10) 0.62455(10) 0.19813(11) 0.0185 1.0000 Uani . . . . . . N102 N 0.97183(10) 0.77394(10) 0.29701(11) 0.0198 1.0000 Uani . . . . . . N103 N 0.98063(10) 0.63517(10) 0.38474(11) 0.0182 1.0000 Uani . . . . . . N104 N 1.16117(11) 0.68809(10) 0.34169(11) 0.0187 1.0000 Uani . . . . . . N105 N 1.21142(11) 0.69110(12) 0.35904(13) 0.0294 1.0000 Uani . . . . . . C1 C 0.42238(12) 0.80403(12) 0.29849(14) 0.0208 1.0000 Uani . . . . . . C2 C 0.39841(13) 0.83771(12) 0.23677(14) 0.0232 1.0000 Uani . . . . . . C3 C 0.34769(13) 0.87328(12) 0.22849(15) 0.0249 1.0000 Uani . . . . . . C4 C 0.31993(13) 0.87482(12) 0.28351(15) 0.0256 1.0000 Uani . . . . . . C5 C 0.34189(13) 0.84198(12) 0.34491(15) 0.0243 1.0000 Uani . . . . . . C6 C 0.39316(13) 0.80664(12) 0.35185(15) 0.0233 1.0000 Uani . . . . . . C7 C 0.32255(15) 0.90856(14) 0.16117(16) 0.0348 1.0000 Uani . . . . . . C8 C 0.31024(16) 0.84198(15) 0.40302(17) 0.0376 1.0000 Uani . . . . . . C9 C 0.56838(13) 0.82309(12) 0.26409(14) 0.0227 1.0000 Uani . . . . . . C10 C 0.54666(15) 0.88799(13) 0.26117(17) 0.0335 1.0000 Uani . . . . . . C11 C 0.63649(14) 0.82198(14) 0.27142(16) 0.0308 1.0000 Uani . . . . . . C12 C 0.56920(14) 0.80999(13) 0.41618(15) 0.0274 1.0000 Uani . . . . . . C13 C 0.53728(16) 0.86832(14) 0.42407(18) 0.0373 1.0000 Uani . . . . . . C14 C 0.63789(15) 0.81759(16) 0.44522(17) 0.0410 1.0000 Uani . . . . . . C15 C 0.43352(12) 0.61521(12) 0.42465(13) 0.0176 1.0000 Uani . . . . . . C16 C 0.39556(12) 0.56628(11) 0.40168(13) 0.0176 1.0000 Uani . . . . . . C17 C 0.34123(12) 0.56061(12) 0.41847(13) 0.0198 1.0000 Uani . . . . . . C18 C 0.32472(13) 0.60409(12) 0.46002(14) 0.0222 1.0000 Uani . . . . . . C19 C 0.36222(13) 0.65327(12) 0.48453(13) 0.0207 1.0000 Uani . . . . . . C20 C 0.41608(12) 0.65800(12) 0.46655(13) 0.0194 1.0000 Uani . . . . . . C21 C 0.29878(13) 0.51042(13) 0.38798(15) 0.0273 1.0000 Uani . . . . . . C22 C 0.34206(15) 0.70155(14) 0.52594(15) 0.0303 1.0000 Uani . . . . . . C23 C 0.58312(12) 0.66188(12) 0.50916(13) 0.0202 1.0000 Uani . . . . . . C24 C 0.56215(13) 0.62921(13) 0.56653(14) 0.0252 1.0000 Uani . . . . . . C25 C 0.65169(14) 0.67220(15) 0.53530(15) 0.0320 1.0000 Uani . . . . . . C26 C 0.58816(13) 0.55089(12) 0.44059(14) 0.0212 1.0000 Uani . . . . . . C27 C 0.65043(13) 0.54411(13) 0.42902(15) 0.0250 1.0000 Uani . . . . . . C28 C 0.54356(15) 0.50345(13) 0.40161(19) 0.0387 1.0000 Uani . . . . . . C29 C 0.43319(12) 0.57591(12) 0.16304(14) 0.0207 1.0000 Uani . . . . . . C30 C 0.43487(14) 0.56512(13) 0.09316(14) 0.0265 1.0000 Uani . . . . . . C31 C 0.39153(15) 0.52942(14) 0.04692(15) 0.0334 1.0000 Uani . . . . . . C32 C 0.34543(15) 0.50497(14) 0.07012(17) 0.0363 1.0000 Uani . . . . . . C33 C 0.34202(14) 0.51489(13) 0.13914(17) 0.0320 1.0000 Uani . . . . . . C34 C 0.38670(13) 0.54947(12) 0.18468(15) 0.0242 1.0000 Uani . . . . . . C35 C 0.39691(18) 0.51728(16) -0.02717(16) 0.0493 1.0000 Uani . . . . . . C36 C 0.29235(15) 0.48787(15) 0.1645(2) 0.0445 1.0000 Uani . . . . . . C37 C 0.54822(14) 0.66646(16) 0.13726(16) 0.0365 1.0000 Uani . . . . . . C38 C 0.60610(16) 0.69934(18) 0.14156(19) 0.0465 1.0000 Uani . . . . . . C39 C 0.49349(15) 0.70761(16) 0.11190(16) 0.0388 1.0000 Uani . . . . . . C40 C 0.65401(14) 0.56448(14) 0.22261(17) 0.0327 1.0000 Uani . . . . . . C41 C 0.5853(3) 0.5615(3) 0.1990(4) 0.0212(14) 0.486(8) Uiso . . P 1 1 . C42 C 0.5644(3) 0.5055(3) 0.2277(3) 0.0256(18) 0.486(8) Uiso . . P 1 1 . C43 C 0.5893(3) 0.5544(2) 0.2280(4) 0.0195(13) 0.514(8) Uiso . . P 1 2 . C44 C 0.5571(3) 0.5050(3) 0.1793(3) 0.0274(17) 0.514(8) Uiso . . P 1 2 . C45 C 0.34499(13) 0.69576(13) 0.16672(14) 0.0240 1.0000 Uani . . . . . . C46 C 0.27725(13) 0.70272(15) 0.15327(15) 0.0308 1.0000 Uani . . . . . . C47 C 0.27112(13) 0.71717(14) 0.22715(15) 0.0275 1.0000 Uani . . . . . . C48 C 0.31811(13) 0.67626(13) 0.27376(15) 0.0251 1.0000 Uani . . . . . . C101 C 0.93297(12) 0.59041(12) 0.14487(13) 0.0195 1.0000 Uani . . . . . . C102 C 0.94136(13) 0.57755(12) 0.07800(14) 0.0220 1.0000 Uani . . . . . . C103 C 0.90016(13) 0.54273(12) 0.02788(14) 0.0236 1.0000 Uani . . . . . . C104 C 0.84900(14) 0.52151(13) 0.04386(15) 0.0284 1.0000 Uani . . . . . . C105 C 0.83886(13) 0.53337(13) 0.10923(15) 0.0284 1.0000 Uani . . . . . . C106 C 0.88129(13) 0.56711(13) 0.15888(14) 0.0239 1.0000 Uani . . . . . . C107 C 0.91070(15) 0.52954(14) -0.04289(15) 0.0337 1.0000 Uani . . . . . . C108 C 0.78322(16) 0.51010(18) 0.12582(18) 0.0480 1.0000 Uani . . . . . . C109 C 1.08426(13) 0.57221(12) 0.18744(14) 0.0204 1.0000 Uani . . . . . . C110 C 1.06232(14) 0.51435(12) 0.21249(15) 0.0266 1.0000 Uani . . . . . . C111 C 1.15320(14) 0.57594(14) 0.21367(17) 0.0311 1.0000 Uani . . . . . . C112 C 1.04872(13) 0.68748(12) 0.12950(13) 0.0215 1.0000 Uani . . . . . . C113 C 0.99404(13) 0.72918(13) 0.10812(15) 0.0272 1.0000 Uani . . . . . . C114 C 1.10843(13) 0.72097(13) 0.14161(14) 0.0253 1.0000 Uani . . . . . . C115 C 0.92420(12) 0.80616(11) 0.31222(14) 0.0188 1.0000 Uani . . . . . . C116 C 0.88695(13) 0.84383(12) 0.26156(14) 0.0231 1.0000 Uani . . . . . . C117 C 0.83475(13) 0.86874(12) 0.27154(15) 0.0256 1.0000 Uani . . . . . . C118 C 0.81989(13) 0.85655(13) 0.33359(15) 0.0256 1.0000 Uani . . . . . . C119 C 0.85588(13) 0.81989(13) 0.38661(14) 0.0237 1.0000 Uani . . . . . . C120 C 0.90771(13) 0.79529(12) 0.37488(14) 0.0220 1.0000 Uani . . . . . . C121 C 0.79403(15) 0.90641(14) 0.21420(17) 0.0363 1.0000 Uani . . . . . . C122 C 0.83761(15) 0.80588(16) 0.45292(16) 0.0368 1.0000 Uani . . . . . . C123 C 1.06839(13) 0.81174(12) 0.41508(14) 0.0224 1.0000 Uani . . . . . . C124 C 1.04685(15) 0.87568(13) 0.42078(17) 0.0330 1.0000 Uani . . . . . . C125 C 1.13595(14) 0.80623(14) 0.45446(15) 0.0301 1.0000 Uani . . . . . . C126 C 1.07031(13) 0.83230(12) 0.26426(14) 0.0213 1.0000 Uani . . . . . . C127 C 1.03748(15) 0.89209(13) 0.25056(17) 0.0331 1.0000 Uani . . . . . . C128 C 1.13891(14) 0.84148(14) 0.28414(16) 0.0304 1.0000 Uani . . . . . . C129 C 0.93148(12) 0.60758(12) 0.40242(14) 0.0195 1.0000 Uani . . . . . . C130 C 0.90614(13) 0.63260(13) 0.45248(15) 0.0252 1.0000 Uani . . . . . . C131 C 0.85221(14) 0.60897(15) 0.46227(16) 0.0318 1.0000 Uani . . . . . . C132 C 0.82543(14) 0.56126(15) 0.42070(18) 0.0369 1.0000 Uani . . . . . . C133 C 0.84938(14) 0.53519(14) 0.37148(16) 0.0313 1.0000 Uani . . . . . . C134 C 0.90249(13) 0.55870(12) 0.36264(15) 0.0240 1.0000 Uani . . . . . . C135 C 0.82618(17) 0.63624(18) 0.51706(19) 0.0497 1.0000 Uani . . . . . . C136 C 0.81876(16) 0.48346(16) 0.32674(19) 0.0484 1.0000 Uani . . . . . . C137 C 1.07117(16) 0.54843(14) 0.3957(2) 0.0194(8) 0.861(8) Uiso . . P 1 4 . C138 C 1.04749(16) 0.50533(15) 0.44152(18) 0.0254(10) 0.861(8) Uiso . . P 1 4 . C139 C 1.13902(14) 0.53576(13) 0.40426(16) 0.0282 1.0000 Uani . . . . . . C140 C 1.0846(10) 0.5503(9) 0.4282(14) 0.022(5) 0.139(8) Uiso . . P 1 3 . C141 C 1.0402(11) 0.5028(10) 0.3918(13) 0.032(7) 0.139(8) Uiso . . P 1 3 . C142 C 1.08869(12) 0.65354(12) 0.49591(13) 0.0200 1.0000 Uani . . . . . . C143 C 1.06357(13) 0.62220(14) 0.55136(14) 0.0273 1.0000 Uani . . . . . . C144 C 1.15808(13) 0.65205(15) 0.52062(15) 0.0300 1.0000 Uani . . . . . . C145 C 0.84273(14) 0.71241(15) 0.15996(15) 0.0326 1.0000 Uani . . . . . . C146 C 0.77495(16) 0.7127(2) 0.1478(2) 0.0635 1.0000 Uani . . . . . . C147 C 0.76665(17) 0.71841(18) 0.2209(2) 0.0528 1.0000 Uani . . . . . . C148 C 0.81704(14) 0.68312(16) 0.26518(17) 0.0366 1.0000 Uani . . . . . . H21 H 0.4175 0.8355 0.2011 0.0272 1.0000 Uiso R . . . . . H41 H 0.2861 0.8987 0.2790 0.0306 1.0000 Uiso R . . . . . H61 H 0.4083 0.7842 0.3936 0.0279 1.0000 Uiso R . . . . . H71 H 0.3502 0.9087 0.1316 0.0518 1.0000 Uiso R . . . . . H72 H 0.2842 0.8916 0.1340 0.0531 1.0000 Uiso R . . . . . H73 H 0.3167 0.9496 0.1737 0.0510 1.0000 Uiso R . . . . . H81 H 0.2856 0.8063 0.3990 0.0556 1.0000 Uiso R . . . . . H82 H 0.2856 0.8763 0.3981 0.0560 1.0000 Uiso R . . . . . H83 H 0.3404 0.8425 0.4487 0.0556 1.0000 Uiso R . . . . . H91 H 0.5489 0.8057 0.2182 0.0270 1.0000 Uiso R . . . . . H101 H 0.5497 0.9055 0.2183 0.0494 1.0000 Uiso R . . . . . H102 H 0.5053 0.8900 0.2626 0.0497 1.0000 Uiso R . . . . . H103 H 0.5725 0.9099 0.3004 0.0497 1.0000 Uiso R . . . . . H111 H 0.6590 0.8455 0.3119 0.0456 1.0000 Uiso R . . . . . H112 H 0.6532 0.7824 0.2778 0.0460 1.0000 Uiso R . . . . . H113 H 0.6446 0.8386 0.2298 0.0454 1.0000 Uiso R . . . . . H121 H 0.5572 0.7805 0.4471 0.0333 1.0000 Uiso R . . . . . H131 H 0.5550 0.8998 0.4035 0.0554 1.0000 Uiso R . . . . . H132 H 0.5427 0.8769 0.4743 0.0557 1.0000 Uiso R . . . . . H133 H 0.4951 0.8661 0.4005 0.0568 1.0000 Uiso R . . . . . H141 H 0.6496 0.8524 0.4232 0.0607 1.0000 Uiso R . . . . . H142 H 0.6591 0.7826 0.4355 0.0607 1.0000 Uiso R . . . . . H143 H 0.6480 0.8234 0.4967 0.0612 1.0000 Uiso R . . . . . H161 H 0.4060 0.5376 0.3733 0.0203 1.0000 Uiso R . . . . . H181 H 0.2884 0.6010 0.4715 0.0269 1.0000 Uiso R . . . . . H201 H 0.4412 0.6908 0.4814 0.0224 1.0000 Uiso R . . . . . H211 H 0.2804 0.4958 0.4219 0.0418 1.0000 Uiso R . . . . . H212 H 0.2675 0.5225 0.3468 0.0424 1.0000 Uiso R . . . . . H213 H 0.3193 0.4782 0.3731 0.0417 1.0000 Uiso R . . . . . H221 H 0.3681 0.7351 0.5324 0.0460 1.0000 Uiso R . . . . . H222 H 0.3422 0.6874 0.5721 0.0453 1.0000 Uiso R . . . . . H223 H 0.3024 0.7147 0.5008 0.0462 1.0000 Uiso R . . . . . H231 H 0.5637 0.7007 0.5028 0.0238 1.0000 Uiso R . . . . . H241 H 0.5656 0.6544 0.6064 0.0381 1.0000 Uiso R . . . . . H242 H 0.5866 0.5948 0.5819 0.0382 1.0000 Uiso R . . . . . H243 H 0.5216 0.6167 0.5485 0.0380 1.0000 Uiso R . . . . . H251 H 0.6658 0.6907 0.4988 0.0477 1.0000 Uiso R . . . . . H252 H 0.6618 0.6971 0.5771 0.0480 1.0000 Uiso R . . . . . H253 H 0.6725 0.6346 0.5477 0.0482 1.0000 Uiso R . . . . . H261 H 0.5936 0.5455 0.4910 0.0251 1.0000 Uiso R . . . . . H271 H 0.6484 0.5512 0.3793 0.0372 1.0000 Uiso R . . . . . H272 H 0.6663 0.5042 0.4425 0.0365 1.0000 Uiso R . . . . . H273 H 0.6791 0.5727 0.4575 0.0373 1.0000 Uiso R . . . . . H281 H 0.5310 0.5118 0.3523 0.0583 1.0000 Uiso R . . . . . H282 H 0.5635 0.4659 0.4093 0.0576 1.0000 Uiso R . . . . . H283 H 0.5082 0.5036 0.4187 0.0575 1.0000 Uiso R . . . . . H301 H 0.4652 0.5827 0.0771 0.0309 1.0000 Uiso R . . . . . H321 H 0.3166 0.4810 0.0391 0.0435 1.0000 Uiso R . . . . . H341 H 0.3850 0.5550 0.2318 0.0288 1.0000 Uiso R . . . . . H351 H 0.4195 0.4827 -0.0283 0.0748 1.0000 Uiso R . . . . . H352 H 0.3587 0.5136 -0.0618 0.0744 1.0000 Uiso R . . . . . H353 H 0.4174 0.5488 -0.0432 0.0746 1.0000 Uiso R . . . . . H361 H 0.2610 0.4733 0.1265 0.0678 1.0000 Uiso R . . . . . H362 H 0.3075 0.4560 0.1961 0.0676 1.0000 Uiso R . . . . . H363 H 0.2758 0.5161 0.1888 0.0682 1.0000 Uiso R . . . . . H371 H 0.5474 0.6360 0.1003 0.0447 1.0000 Uiso R . . . . . H381 H 0.6389 0.6683 0.1480 0.0703 1.0000 Uiso R . . . . . H382 H 0.6012 0.7199 0.0951 0.0704 1.0000 Uiso R . . . . . H383 H 0.6154 0.7275 0.1826 0.0699 1.0000 Uiso R . . . . . H392 H 0.4925 0.7335 0.1497 0.0570 1.0000 Uiso R . . . . . H393 H 0.4571 0.6846 0.0974 0.0567 1.0000 Uiso R . . . . . H396 H 0.4979 0.7296 0.0730 0.0585 1.0000 Uiso R . . . . . H421 H 0.5719 0.5588 0.1470 0.0252 0.486(8) Uiso R . P 1 1 . H431 H 0.5792 0.5059 0.2786 0.0379 0.486(8) Uiso R . P 1 1 . H432 H 0.5811 0.4716 0.2096 0.0381 0.486(8) Uiso R . P 1 1 . H433 H 0.5212 0.5025 0.2134 0.0377 0.486(8) Uiso R . P 1 1 . H441 H 0.6525 0.5757 0.1748 0.0485 0.514(8) Uiso R . P 1 2 . H442 H 0.6776 0.5287 0.2350 0.0490 0.514(8) Uiso R . P 1 2 . H443 H 0.6675 0.5977 0.2005 0.0487 0.486(8) Uiso R . P 1 1 . H444 H 0.6742 0.5959 0.2541 0.0487 0.514(8) Uiso R . P 1 2 . H445 H 0.6692 0.5690 0.2739 0.0491 0.486(8) Uiso R . P 1 1 . H446 H 0.6709 0.5285 0.2094 0.0489 0.486(8) Uiso R . P 1 1 . H451 H 0.5933 0.5402 0.2765 0.0230 0.514(8) Uiso R . P 1 2 . H461 H 0.5839 0.4709 0.1861 0.0411 0.514(8) Uiso R . P 1 2 . H462 H 0.5479 0.5179 0.1307 0.0405 0.514(8) Uiso R . P 1 2 . H463 H 0.5211 0.4942 0.1912 0.0406 0.514(8) Uiso R . P 1 2 . H471 H 0.3035 0.6350 0.2725 0.0304 1.0000 Uiso R . . . . . H472 H 0.3328 0.6896 0.3233 0.0296 1.0000 Uiso R . . . . . H481 H 0.2823 0.7583 0.2388 0.0330 1.0000 Uiso R . . . . . H482 H 0.2314 0.7090 0.2312 0.0331 1.0000 Uiso R . . . . . H491 H 0.2610 0.7342 0.1193 0.0381 1.0000 Uiso R . . . . . H492 H 0.2566 0.6660 0.1342 0.0366 1.0000 Uiso R . . . . . H501 H 0.3643 0.7333 0.1601 0.0290 1.0000 Uiso R . . . . . H502 H 0.3536 0.6653 0.1367 0.0286 1.0000 Uiso R . . . . . H1021 H 0.9759 0.5923 0.0668 0.0254 1.0000 Uiso R . . . . . H1041 H 0.8214 0.4979 0.0096 0.0334 1.0000 Uiso R . . . . . H1061 H 0.8750 0.5735 0.2032 0.0288 1.0000 Uiso R . . . . . H1071 H 0.9180 0.5647 -0.0651 0.0519 1.0000 Uiso R . . . . . H1072 H 0.8766 0.5109 -0.0750 0.0516 1.0000 Uiso R . . . . . H1073 H 0.9450 0.5050 -0.0367 0.0515 1.0000 Uiso R . . . . . H1081 H 0.7941 0.4844 0.1658 0.0719 1.0000 Uiso R . . . . . H1082 H 0.7574 0.4887 0.0877 0.0720 1.0000 Uiso R . . . . . H1083 H 0.7612 0.5413 0.1379 0.0728 1.0000 Uiso R . . . . . H1091 H 1.0734 0.5710 0.1360 0.0244 1.0000 Uiso R . . . . . H1101 H 1.0772 0.5099 0.2635 0.0403 1.0000 Uiso R . . . . . H1102 H 1.0192 0.5133 0.1994 0.0405 1.0000 Uiso R . . . . . H1103 H 1.0773 0.4815 0.1904 0.0397 1.0000 Uiso R . . . . . H1111 H 1.1703 0.5406 0.2005 0.0467 1.0000 Uiso R . . . . . H1112 H 1.1672 0.6085 0.1917 0.0469 1.0000 Uiso R . . . . . H1113 H 1.1670 0.5800 0.2651 0.0467 1.0000 Uiso R . . . . . H1121 H 1.0448 0.6604 0.0887 0.0256 1.0000 Uiso R . . . . . H1131 H 0.9909 0.7523 0.1482 0.0409 1.0000 Uiso R . . . . . H1132 H 0.9988 0.7554 0.0714 0.0409 1.0000 Uiso R . . . . . H1133 H 0.9574 0.7072 0.0901 0.0401 1.0000 Uiso R . . . . . H1141 H 1.1176 0.7427 0.1860 0.0379 1.0000 Uiso R . . . . . H1142 H 1.1406 0.6937 0.1432 0.0377 1.0000 Uiso R . . . . . H1143 H 1.1053 0.7481 0.1019 0.0382 1.0000 Uiso R . . . . . H1161 H 0.8963 0.8514 0.2197 0.0274 1.0000 Uiso R . . . . . H1181 H 0.7848 0.8730 0.3396 0.0316 1.0000 Uiso R . . . . . H1201 H 0.9324 0.7703 0.4098 0.0256 1.0000 Uiso R . . . . . H1211 H 0.7608 0.9213 0.2276 0.0557 1.0000 Uiso R . . . . . H1212 H 0.7789 0.8849 0.1716 0.0550 1.0000 Uiso R . . . . . H1213 H 0.8147 0.9396 0.2033 0.0556 1.0000 Uiso R . . . . . H1221 H 0.8620 0.7746 0.4803 0.0558 1.0000 Uiso R . . . . . H1222 H 0.7970 0.7927 0.4406 0.0554 1.0000 Uiso R . . . . . H1223 H 0.8410 0.8399 0.4814 0.0560 1.0000 Uiso R . . . . . H1231 H 1.0462 0.7873 0.4405 0.0271 1.0000 Uiso R . . . . . H1241 H 1.0719 0.9046 0.4057 0.0499 1.0000 Uiso R . . . . . H1242 H 1.0056 0.8817 0.3933 0.0497 1.0000 Uiso R . . . . . H1243 H 1.0512 0.8845 0.4705 0.0500 1.0000 Uiso R . . . . . H1251 H 1.1432 0.8145 0.5042 0.0449 1.0000 Uiso R . . . . . H1252 H 1.1499 0.7669 0.4486 0.0447 1.0000 Uiso R . . . . . H1253 H 1.1589 0.8353 0.4368 0.0451 1.0000 Uiso R . . . . . H1261 H 1.0590 0.8119 0.2191 0.0262 1.0000 Uiso R . . . . . H1271 H 1.0429 0.9094 0.2078 0.0498 1.0000 Uiso R . . . . . H1272 H 0.9945 0.8876 0.2438 0.0499 1.0000 Uiso R . . . . . H1273 H 1.0532 0.9192 0.2894 0.0498 1.0000 Uiso R . . . . . H1281 H 1.1604 0.8042 0.2960 0.0451 1.0000 Uiso R . . . . . H1282 H 1.1516 0.8688 0.3235 0.0452 1.0000 Uiso R . . . . . H1283 H 1.1496 0.8588 0.2439 0.0460 1.0000 Uiso R . . . . . H1301 H 0.9245 0.6647 0.4796 0.0284 1.0000 Uiso R . . . . . H1321 H 0.7899 0.5456 0.4271 0.0443 1.0000 Uiso R . . . . . H1341 H 0.9193 0.5405 0.3291 0.0295 1.0000 Uiso R . . . . . H1351 H 0.7949 0.6637 0.4949 0.0745 1.0000 Uiso R . . . . . H1352 H 0.8560 0.6599 0.5516 0.0724 1.0000 Uiso R . . . . . H1353 H 0.8099 0.6073 0.5419 0.0746 1.0000 Uiso R . . . . . H1361 H 0.7795 0.4957 0.2974 0.0733 1.0000 Uiso R . . . . . H1362 H 0.8135 0.4513 0.3583 0.0732 1.0000 Uiso R . . . . . H1363 H 0.8428 0.4697 0.2960 0.0735 1.0000 Uiso R . . . . . H1371 H 1.0486 0.5385 0.3463 0.0228 0.861(8) Uiso R . P 1 4 . H1381 H 1.0079 0.5171 0.4433 0.0376 0.861(8) Uiso R . P 1 4 . H1382 H 1.0734 0.5060 0.4900 0.0368 0.861(8) Uiso R . P 1 4 . H1383 H 1.0461 0.4652 0.4228 0.0378 0.861(8) Uiso R . P 1 4 . H1391 H 1.1748 0.5507 0.4385 0.0419 0.139(8) Uiso R . P 1 3 . H1392 H 1.1424 0.4933 0.4009 0.0421 0.139(8) Uiso R . P 1 3 . H1393 H 1.1555 0.5655 0.3793 0.0417 0.861(8) Uiso R . P 1 4 . H1394 H 1.1356 0.5534 0.3585 0.0420 0.139(8) Uiso R . P 1 3 . H1395 H 1.1423 0.4972 0.3838 0.0424 0.861(8) Uiso R . P 1 4 . H1396 H 1.1621 0.5347 0.4533 0.0417 0.861(8) Uiso R . P 1 4 . H1401 H 1.0942 0.5453 0.4801 0.0261 0.139(8) Uiso R . P 1 3 . H1411 H 1.0134 0.4938 0.4199 0.0460 0.139(8) Uiso R . P 1 3 . H1412 H 1.0167 0.5167 0.3456 0.0460 0.139(8) Uiso R . P 1 3 . H1413 H 1.0619 0.4675 0.3862 0.0461 0.139(8) Uiso R . P 1 3 . H1421 H 1.0759 0.6946 0.4943 0.0235 1.0000 Uiso R . . . . . H1431 H 1.0206 0.6205 0.5363 0.0405 1.0000 Uiso R . . . . . H1432 H 1.0792 0.5825 0.5613 0.0408 1.0000 Uiso R . . . . . H1433 H 1.0758 0.6444 0.5943 0.0407 1.0000 Uiso R . . . . . H1441 H 1.1723 0.6745 0.5633 0.0444 1.0000 Uiso R . . . . . H1442 H 1.1743 0.6693 0.4855 0.0446 1.0000 Uiso R . . . . . H1443 H 1.1730 0.6119 0.5302 0.0446 1.0000 Uiso R . . . . . H1451 H 0.8587 0.7513 0.1567 0.0392 1.0000 Uiso R . . . . . H1452 H 0.8553 0.6863 0.1281 0.0394 1.0000 Uiso R . . . . . H1461 H 0.7579 0.7449 0.1170 0.0759 1.0000 Uiso R . . . . . H1462 H 0.7583 0.6754 0.1280 0.0770 1.0000 Uiso R . . . . . H1471 H 0.7717 0.7605 0.2348 0.0642 1.0000 Uiso R . . . . . H1472 H 0.7272 0.7040 0.2221 0.0629 1.0000 Uiso R . . . . . H1481 H 0.8294 0.6974 0.3125 0.0447 1.0000 Uiso R . . . . . H1482 H 0.8053 0.6417 0.2646 0.0451 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 0.00975(13) 0.01538(12) 0.01939(12) -0.00090(9) 0.00430(9) 0.00005(10) Zr101 0.00962(13) 0.01900(13) 0.01669(11) -0.00351(9) 0.00364(9) 0.00021(10) Co1 0.00988(18) 0.01498(17) 0.02079(17) -0.00032(13) 0.00483(13) -0.00007(14) Co101 0.00994(18) 0.01507(17) 0.01574(15) -0.00159(13) 0.00368(13) 0.00015(14) P1 0.0137(4) 0.0148(3) 0.0263(3) -0.0014(3) 0.0057(3) -0.0011(3) P2 0.0120(3) 0.0176(3) 0.0187(3) -0.0011(2) 0.0040(3) -0.0009(3) P3 0.0125(4) 0.0193(3) 0.0215(3) -0.0006(3) 0.0062(3) 0.0019(3) P101 0.0121(3) 0.0185(3) 0.0159(3) -0.0030(2) 0.0050(2) 0.0003(3) P102 0.0138(4) 0.0157(3) 0.0199(3) -0.0017(2) 0.0050(3) 0.0009(3) P103 0.0118(3) 0.0163(3) 0.0196(3) -0.0003(2) 0.0059(3) 0.0003(3) O1 0.0119(10) 0.0241(10) 0.0224(9) 0.0035(7) 0.0037(7) 0.0031(8) O101 0.0118(10) 0.0369(12) 0.0318(10) -0.0060(9) 0.0019(8) 0.0037(9) N1 0.0139(12) 0.0149(11) 0.0371(13) -0.0012(9) 0.0065(10) 0.0011(9) N2 0.0125(12) 0.0216(12) 0.0215(11) 0.0013(9) 0.0058(9) -0.0034(9) N3 0.0137(12) 0.0227(12) 0.0220(11) -0.0049(9) 0.0069(9) -0.0010(9) N4 0.0188(13) 0.0187(12) 0.0269(11) 0.0018(9) 0.0076(10) 0.0004(10) N5 0.0136(14) 0.0404(16) 0.0451(15) 0.0020(12) 0.0066(11) -0.0025(12) N101 0.0147(12) 0.0218(11) 0.0197(10) -0.0078(9) 0.0063(9) -0.0027(9) N102 0.0149(12) 0.0201(11) 0.0241(11) -0.0022(9) 0.0051(9) 0.0046(10) N103 0.0126(12) 0.0204(12) 0.0236(11) 0.0007(9) 0.0085(9) 0.0003(9) N104 0.0167(13) 0.0207(12) 0.0185(10) 0.0011(9) 0.0046(9) 0.0010(10) N105 0.0151(14) 0.0398(15) 0.0338(13) 0.0030(11) 0.0077(11) -0.0010(11) C1 0.0136(14) 0.0168(13) 0.0314(14) -0.0041(11) 0.0053(11) 0.0002(11) C2 0.0240(16) 0.0200(14) 0.0283(14) -0.0011(11) 0.0116(12) -0.0015(12) C3 0.0222(16) 0.0164(13) 0.0331(15) 0.0007(11) 0.0032(12) -0.0005(12) C4 0.0172(15) 0.0186(14) 0.0414(16) -0.0006(12) 0.0089(12) 0.0034(11) C5 0.0201(16) 0.0180(14) 0.0365(15) -0.0018(11) 0.0106(12) 0.0011(12) C6 0.0210(16) 0.0205(14) 0.0280(14) 0.0024(11) 0.0066(12) -0.0003(12) C7 0.038(2) 0.0257(16) 0.0378(17) 0.0035(13) 0.0063(14) 0.0099(14) C8 0.036(2) 0.0386(19) 0.0451(19) 0.0048(15) 0.0233(16) 0.0108(16) C9 0.0208(16) 0.0180(14) 0.0282(14) 0.0021(11) 0.0053(11) -0.0024(11) C10 0.0348(19) 0.0219(15) 0.0463(18) 0.0034(13) 0.0155(15) 0.0010(14) C11 0.0239(17) 0.0307(17) 0.0400(17) 0.0084(13) 0.0129(13) -0.0023(13) C12 0.0314(18) 0.0219(15) 0.0303(15) -0.0053(12) 0.0109(13) -0.0044(13) C13 0.036(2) 0.0296(17) 0.0470(19) -0.0162(14) 0.0128(15) -0.0021(15) C14 0.032(2) 0.042(2) 0.0397(18) -0.0168(15) -0.0049(14) 0.0032(16) C15 0.0127(14) 0.0224(14) 0.0173(12) 0.0027(10) 0.0038(10) -0.0007(11) C16 0.0170(14) 0.0193(13) 0.0166(12) -0.0015(10) 0.0048(10) 0.0007(11) C17 0.0154(14) 0.0217(14) 0.0190(12) 0.0031(10) -0.0007(10) -0.0020(11) C18 0.0152(14) 0.0309(15) 0.0215(13) 0.0032(11) 0.0066(11) 0.0000(12) C19 0.0189(15) 0.0257(14) 0.0181(12) 0.0015(10) 0.0063(11) 0.0013(11) C20 0.0192(15) 0.0192(13) 0.0190(12) -0.0003(10) 0.0044(11) -0.0039(11) C21 0.0190(15) 0.0292(16) 0.0322(15) -0.0038(12) 0.0047(12) -0.0086(12) C22 0.0324(18) 0.0311(17) 0.0316(15) -0.0027(12) 0.0159(13) 0.0001(14) C23 0.0190(15) 0.0209(14) 0.0193(12) -0.0028(10) 0.0032(10) -0.0001(11) C24 0.0254(17) 0.0292(16) 0.0196(13) -0.0008(11) 0.0043(11) 0.0005(13) C25 0.0241(17) 0.0446(19) 0.0249(14) -0.0085(13) 0.0034(12) -0.0088(14) C26 0.0210(15) 0.0191(13) 0.0238(13) 0.0025(10) 0.0068(11) 0.0031(11) C27 0.0202(16) 0.0260(15) 0.0277(14) 0.0028(11) 0.0053(12) 0.0054(12) C28 0.0282(19) 0.0203(16) 0.067(2) -0.0110(15) 0.0127(16) -0.0032(13) C29 0.0159(15) 0.0179(13) 0.0251(13) -0.0012(10) 0.0005(11) 0.0040(11) C30 0.0251(17) 0.0258(15) 0.0241(14) 0.0019(11) -0.0001(12) 0.0035(12) C31 0.038(2) 0.0264(16) 0.0263(15) -0.0037(12) -0.0049(13) 0.0053(14) C32 0.0302(19) 0.0242(16) 0.0405(18) -0.0049(13) -0.0122(14) -0.0029(14) C33 0.0237(17) 0.0176(14) 0.0466(18) 0.0002(13) -0.0029(14) 0.0013(12) C34 0.0199(16) 0.0211(14) 0.0310(15) -0.0017(11) 0.0065(12) 0.0031(12) C35 0.066(3) 0.042(2) 0.0276(16) -0.0129(15) -0.0052(16) -0.0023(19) C36 0.0252(19) 0.0320(19) 0.070(2) -0.0043(17) 0.0040(17) -0.0088(15) C37 0.0243(18) 0.058(2) 0.0291(15) 0.0053(15) 0.0110(13) -0.0029(16) C38 0.037(2) 0.058(2) 0.047(2) 0.0104(17) 0.0149(17) -0.0066(18) C39 0.0260(18) 0.057(2) 0.0307(16) 0.0222(15) 0.0037(13) -0.0040(16) C40 0.0239(18) 0.0317(17) 0.0443(18) 0.0058(14) 0.0129(14) 0.0109(14) C45 0.0198(16) 0.0297(16) 0.0218(13) 0.0050(11) 0.0049(11) 0.0007(12) C46 0.0173(16) 0.0455(19) 0.0274(15) 0.0048(13) 0.0029(12) 0.0036(14) C47 0.0135(15) 0.0367(17) 0.0328(15) 0.0018(13) 0.0074(12) 0.0065(13) C48 0.0157(15) 0.0319(16) 0.0284(14) 0.0022(12) 0.0073(11) 0.0006(12) C101 0.0152(14) 0.0199(13) 0.0208(12) -0.0035(10) 0.0011(10) 0.0001(11) C102 0.0200(15) 0.0221(14) 0.0237(13) -0.0051(11) 0.0059(11) 0.0002(11) C103 0.0240(16) 0.0240(15) 0.0210(13) -0.0039(11) 0.0035(11) 0.0021(12) C104 0.0263(17) 0.0254(15) 0.0280(14) -0.0089(12) -0.0012(12) -0.0035(13) C105 0.0196(16) 0.0323(17) 0.0306(15) -0.0066(12) 0.0026(12) -0.0071(13) C106 0.0201(15) 0.0308(16) 0.0204(13) -0.0040(11) 0.0051(11) -0.0028(12) C107 0.038(2) 0.0356(18) 0.0248(14) -0.0110(13) 0.0043(13) 0.0001(15) C108 0.032(2) 0.072(3) 0.0414(19) -0.0142(18) 0.0123(16) -0.0273(19) C109 0.0206(15) 0.0224(14) 0.0197(12) -0.0032(10) 0.0081(11) 0.0033(11) C110 0.0308(18) 0.0230(15) 0.0267(14) -0.0028(11) 0.0094(12) 0.0020(13) C111 0.0241(18) 0.0288(17) 0.0449(18) -0.0004(13) 0.0168(14) 0.0043(13) C112 0.0221(15) 0.0277(15) 0.0149(11) 0.0001(10) 0.0056(10) 0.0003(12) C113 0.0208(16) 0.0313(16) 0.0260(14) 0.0059(12) 0.0010(12) 0.0029(13) C114 0.0188(15) 0.0333(16) 0.0253(14) 0.0028(12) 0.0085(11) 0.0033(12) C115 0.0145(14) 0.0153(13) 0.0256(13) -0.0025(10) 0.0042(11) 0.0006(10) C116 0.0238(16) 0.0191(14) 0.0254(13) 0.0015(11) 0.0057(12) 0.0029(12) C117 0.0199(16) 0.0177(14) 0.0346(15) -0.0012(11) 0.0004(12) 0.0053(11) C118 0.0166(15) 0.0266(15) 0.0336(15) -0.0038(12) 0.0071(12) 0.0055(12) C119 0.0201(15) 0.0250(15) 0.0266(13) -0.0063(11) 0.0077(11) -0.0009(12) C120 0.0180(15) 0.0227(14) 0.0240(13) 0.0022(11) 0.0041(11) 0.0050(11) C121 0.0272(19) 0.0350(18) 0.0439(18) 0.0080(14) 0.0060(14) 0.0147(14) C122 0.0308(19) 0.050(2) 0.0331(16) -0.0010(15) 0.0146(14) 0.0043(16) C123 0.0233(16) 0.0216(14) 0.0230(13) -0.0028(11) 0.0081(11) -0.0012(12) C124 0.037(2) 0.0245(16) 0.0391(17) -0.0118(13) 0.0125(14) -0.0007(14) C125 0.0279(18) 0.0343(17) 0.0247(14) -0.0067(12) 0.0024(12) -0.0038(14) C126 0.0200(15) 0.0205(14) 0.0245(13) 0.0034(11) 0.0083(11) 0.0020(11) C127 0.0331(19) 0.0254(16) 0.0446(18) 0.0102(13) 0.0169(15) 0.0058(14) C128 0.0255(17) 0.0288(16) 0.0375(16) 0.0082(13) 0.0101(13) -0.0037(13) C129 0.0148(14) 0.0197(13) 0.0236(13) 0.0052(10) 0.0048(11) 0.0027(11) C130 0.0216(16) 0.0277(15) 0.0295(14) 0.0059(12) 0.0126(12) 0.0076(12) C131 0.0238(17) 0.0428(19) 0.0350(16) 0.0167(14) 0.0184(13) 0.0148(14) C132 0.0144(16) 0.042(2) 0.052(2) 0.0244(16) 0.0047(14) -0.0025(14) C133 0.0181(16) 0.0310(17) 0.0384(17) 0.0131(13) -0.0024(13) -0.0057(13) C134 0.0178(15) 0.0224(14) 0.0297(14) 0.0048(11) 0.0033(12) 0.0015(12) C135 0.044(2) 0.066(3) 0.052(2) 0.0182(19) 0.0337(18) 0.022(2) C136 0.037(2) 0.040(2) 0.054(2) 0.0111(16) -0.0101(17) -0.0183(17) C139 0.0271(17) 0.0265(16) 0.0357(16) 0.0047(12) 0.0165(13) 0.0098(13) C142 0.0185(15) 0.0239(14) 0.0174(12) 0.0001(10) 0.0045(10) 0.0017(11) C143 0.0229(16) 0.0349(17) 0.0233(14) 0.0051(12) 0.0054(12) -0.0015(13) C144 0.0192(16) 0.0463(19) 0.0221(14) 0.0047(13) 0.0020(12) -0.0023(14) C145 0.0238(17) 0.0389(18) 0.0304(15) -0.0030(13) 0.0004(13) 0.0063(14) C146 0.020(2) 0.109(4) 0.053(2) 0.000(2) -0.0040(17) 0.025(2) C147 0.027(2) 0.056(3) 0.077(3) 0.005(2) 0.0172(19) 0.0088(18) C148 0.0150(16) 0.051(2) 0.0439(18) -0.0088(16) 0.0091(13) -0.0011(15) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.0360787(17) 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 . 2.3778(5) yes Zr1 . P1 . 2.8390(7) yes Zr1 . P2 . 2.7613(7) yes Zr1 . P3 . 2.7785(7) yes Zr1 . O1 . 2.3303(18) yes Zr1 . N1 . 2.142(2) yes Zr1 . N2 . 2.079(2) yes Zr1 . N3 . 2.148(2) yes Zr101 . Co101 . 2.3854(5) yes Zr101 . P101 . 2.7901(7) yes Zr101 . P102 . 2.8109(7) yes Zr101 . P103 . 2.7636(7) yes Zr101 . O101 . 2.3285(19) yes Zr101 . N101 . 2.162(2) yes Zr101 . N102 . 2.140(2) yes Zr101 . N103 . 2.081(2) yes Co1 . P1 . 2.2331(8) yes Co1 . P2 . 2.2464(8) yes Co1 . P3 . 2.2290(8) yes Co1 . N4 . 1.844(2) yes Co101 . P101 . 2.2221(7) yes Co101 . P102 . 2.2326(8) yes Co101 . P103 . 2.2356(7) yes Co101 . N104 . 1.836(2) yes P1 . N1 . 1.684(2) yes P1 . C9 . 1.868(3) yes P1 . C12 . 1.878(3) yes P2 . N2 . 1.686(2) yes P2 . C23 . 1.865(3) yes P2 . C26 . 1.867(3) yes P3 . N3 . 1.692(2) yes P3 . C37 . 1.874(3) yes P3 . C41 . 1.855(6) yes P3 . N3 . 1.692(2) yes P3 . C37 . 1.874(3) yes P3 . C43 . 1.905(6) yes P101 . N101 . 1.697(2) yes P101 . C109 . 1.880(3) yes P101 . C112 . 1.887(3) yes P102 . N102 . 1.684(2) yes P102 . C123 . 1.865(3) yes P102 . C126 . 1.870(3) yes P103 . N103 . 1.691(2) yes P103 . C140 . 1.91(2) yes P103 . C142 . 1.856(3) yes P103 . N103 . 1.691(2) yes P103 . C137 . 1.855(3) yes P103 . C142 . 1.856(3) yes O1 . C45 . 1.462(3) yes O1 . C48 . 1.461(3) yes O101 . C145 . 1.462(3) yes O101 . C148 . 1.462(4) yes N1 . C1 . 1.418(3) yes N2 . C15 . 1.416(3) yes N3 . C29 . 1.407(3) yes N4 . N5 . 1.110(3) yes N101 . C101 . 1.407(3) yes N102 . C115 . 1.414(3) yes N103 . C129 . 1.416(3) yes N104 . N105 . 1.109(3) yes C1 . C2 . 1.397(4) yes C1 . C6 . 1.393(4) yes C2 . C3 . 1.385(4) yes C2 . H21 . 0.926 no C3 . C4 . 1.398(4) yes C3 . C7 . 1.503(4) yes C4 . C5 . 1.376(4) yes C4 . H41 . 0.928 no C5 . C6 . 1.396(4) yes C5 . C8 . 1.513(4) yes C6 . H61 . 0.938 no C7 . H71 . 0.973 no C7 . H72 . 0.968 no C7 . H73 . 0.974 no C8 . H81 . 0.973 no C8 . H82 . 0.946 no C8 . H83 . 0.961 no C9 . C10 . 1.539(4) yes C9 . C11 . 1.532(4) yes C9 . H91 . 0.962 no C10 . H101 . 0.947 no C10 . H102 . 0.960 no C10 . H103 . 0.961 no C11 . H111 . 0.969 no C11 . H112 . 0.963 no C11 . H113 . 0.960 no C12 . C13 . 1.532(4) yes C12 . C14 . 1.528(4) yes C12 . H121 . 0.988 no C13 . H131 . 0.960 no C13 . H132 . 0.973 no C13 . H133 . 0.949 no C14 . H141 . 0.968 no C14 . H142 . 0.973 no C14 . H143 . 0.973 no C15 . C16 . 1.397(4) yes C15 . C20 . 1.394(4) yes C16 . C17 . 1.385(4) yes C16 . H161 . 0.926 no C17 . C18 . 1.391(4) yes C17 . C21 . 1.500(4) yes C18 . C19 . 1.400(4) yes C18 . H181 . 0.927 no C19 . C20 . 1.385(4) yes C19 . C22 . 1.504(4) yes C20 . H201 . 0.931 no C21 . H211 . 0.941 no C21 . H212 . 0.953 no C21 . H213 . 0.954 no C22 . H221 . 0.948 no C22 . H222 . 0.955 no C22 . H223 . 0.951 no C23 . C24 . 1.529(4) yes C23 . C25 . 1.530(4) yes C23 . H231 . 0.972 no C24 . H241 . 0.947 no C24 . H242 . 0.953 no C24 . H243 . 0.940 no C25 . H251 . 0.959 no C25 . H252 . 0.961 no C25 . H253 . 0.969 no C26 . C27 . 1.520(4) yes C26 . C28 . 1.524(4) yes C26 . H261 . 0.965 no C27 . H271 . 0.971 no C27 . H272 . 0.976 no C27 . H273 . 0.973 no C28 . H281 . 0.942 no C28 . H282 . 0.953 no C28 . H283 . 0.964 no C29 . C30 . 1.398(4) yes C29 . C34 . 1.390(4) yes C30 . C31 . 1.393(4) yes C30 . H301 . 0.931 no C31 . C32 . 1.381(5) yes C31 . C35 . 1.512(4) yes C32 . C33 . 1.391(4) yes C32 . H321 . 0.932 no C33 . C34 . 1.389(4) yes C33 . C36 . 1.497(5) yes C34 . H341 . 0.942 no C35 . H351 . 0.940 no C35 . H352 . 0.946 no C35 . H353 . 0.952 no C36 . H361 . 0.932 no C36 . H362 . 0.945 no C36 . H363 . 0.935 no C37 . C38 . 1.504(5) yes C37 . C39 . 1.526(5) yes C37 . H371 . 0.992 no C38 . H381 . 1.008 no C38 . H382 . 0.996 no C38 . H383 . 0.995 no C39 . H392 . 0.946 no C39 . H393 . 0.955 no C39 . H396 . 0.937 no C40 . C41 . 1.516(7) yes C40 . H443 . 0.957 no C40 . H445 . 0.967 no C40 . H446 . 0.964 no C40 . C43 . 1.537(6) yes C40 . H441 . 0.959 no C40 . H442 . 0.963 no C40 . H444 . 0.964 no C41 . C42 . 1.512(9) yes C41 . H421 . 0.974 no C42 . H431 . 0.954 no C42 . H432 . 0.965 no C42 . H433 . 0.954 no C43 . C44 . 1.513(8) yes C43 . H451 . 0.978 no C44 . H461 . 0.968 no C44 . H462 . 0.957 no C44 . H463 . 0.954 no C45 . C46 . 1.512(4) yes C45 . H501 . 0.979 no C45 . H502 . 0.959 no C46 . C47 . 1.524(4) yes C46 . H491 . 0.969 no C46 . H492 . 0.973 no C47 . C48 . 1.510(4) yes C47 . H481 . 0.970 no C47 . H482 . 0.957 no C48 . H471 . 0.985 no C48 . H472 . 0.977 no C101 . C102 . 1.404(4) yes C101 . C106 . 1.396(4) yes C102 . C103 . 1.393(4) yes C102 . H1021 . 0.943 no C103 . C104 . 1.385(4) yes C103 . C107 . 1.500(4) yes C104 . C105 . 1.388(4) yes C104 . H1041 . 0.943 no C105 . C106 . 1.388(4) yes C105 . C108 . 1.501(4) yes C106 . H1061 . 0.928 no C107 . H1071 . 0.941 no C107 . H1072 . 0.951 no C107 . H1073 . 0.942 no C108 . H1081 . 0.946 no C108 . H1082 . 0.940 no C108 . H1083 . 0.935 no C109 . C110 . 1.526(4) yes C109 . C111 . 1.523(4) yes C109 . H1091 . 0.964 no C110 . H1101 . 0.961 no C110 . H1102 . 0.952 no C110 . H1103 . 0.968 no C111 . H1111 . 0.955 no C111 . H1112 . 0.951 no C111 . H1113 . 0.968 no C112 . C113 . 1.528(4) yes C112 . C114 . 1.524(4) yes C112 . H1121 . 0.987 no C113 . H1131 . 0.960 no C113 . H1132 . 0.958 no C113 . H1133 . 0.954 no C114 . H1141 . 0.964 no C114 . H1142 . 0.954 no C114 . H1143 . 0.973 no C115 . C116 . 1.395(4) yes C115 . C120 . 1.402(4) yes C116 . C117 . 1.388(4) yes C116 . H1161 . 0.918 no C117 . C118 . 1.377(4) yes C117 . C121 . 1.500(4) yes C118 . C119 . 1.396(4) yes C118 . H1181 . 0.925 no C119 . C120 . 1.391(4) yes C119 . C122 . 1.505(4) yes C120 . H1201 . 0.939 no C121 . H1211 . 0.937 no C121 . H1212 . 0.939 no C121 . H1213 . 0.942 no C122 . H1221 . 0.961 no C122 . H1222 . 0.944 no C122 . H1223 . 0.936 no C123 . C124 . 1.535(4) yes C123 . C125 . 1.529(4) yes C123 . H1231 . 0.975 no C124 . H1241 . 0.970 no C124 . H1242 . 0.956 no C124 . H1243 . 0.968 no C125 . H1251 . 0.956 no C125 . H1252 . 0.958 no C125 . H1253 . 0.963 no C126 . C127 . 1.528(4) yes C126 . C128 . 1.527(4) yes C126 . H1261 . 0.961 no C127 . H1271 . 0.962 no C127 . H1272 . 0.964 no C127 . H1273 . 0.960 no C128 . H1281 . 0.966 no C128 . H1282 . 0.963 no C128 . H1283 . 0.971 no C129 . C130 . 1.392(4) yes C129 . C134 . 1.400(4) yes C130 . C131 . 1.411(4) yes C130 . H1301 . 0.922 no C131 . C132 . 1.380(5) yes C131 . C135 . 1.499(4) yes C132 . C133 . 1.369(5) yes C132 . H1321 . 0.930 no C133 . C134 . 1.386(4) yes C133 . C136 . 1.504(4) yes C134 . H1341 . 0.943 no C135 . H1351 . 0.953 no C135 . H1352 . 0.971 no C135 . H1353 . 0.950 no C136 . H1361 . 0.962 no C136 . H1362 . 0.980 no C136 . H1363 . 0.975 no C137 . C138 . 1.522(5) yes C137 . C139 . 1.547(4) yes C137 . H1371 . 0.983 no C138 . H1381 . 0.957 no C138 . H1382 . 0.963 no C138 . H1383 . 0.971 no C139 . C140 . 1.49(2) yes C139 . H1391 . 0.960 no C139 . H1392 . 0.961 no C139 . H1394 . 0.961 no C139 . H1393 . 0.967 no C139 . H1395 . 0.966 no C139 . H1396 . 0.954 no C140 . C141 . 1.51(3) yes C140 . H1401 . 0.981 no C141 . H1411 . 0.958 no C141 . H1412 . 0.960 no C141 . H1413 . 0.962 no C142 . C143 . 1.537(4) yes C142 . C144 . 1.530(4) yes C142 . H1421 . 0.966 no C143 . H1431 . 0.947 no C143 . H1432 . 0.961 no C143 . H1433 . 0.946 no C144 . H1441 . 0.949 no C144 . H1442 . 0.952 no C144 . H1443 . 0.966 no C145 . C146 . 1.508(5) yes C145 . H1451 . 0.958 no C145 . H1452 . 0.959 no C146 . C147 . 1.498(5) yes C146 . H1461 . 0.951 no C146 . H1462 . 0.956 no C147 . C148 . 1.466(5) yes C147 . H1471 . 0.983 no C147 . H1472 . 0.969 no C148 . H1481 . 0.942 no C148 . H1482 . 0.969 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 . 49.729(17) yes Co1 . Zr1 . P2 . 51.176(17) yes P1 . Zr1 . P2 . 81.04(2) yes Co1 . Zr1 . P3 . 50.496(17) yes P1 . Zr1 . P3 . 85.05(2) yes P2 . Zr1 . P3 . 85.24(2) yes Co1 . Zr1 . O1 . 162.32(4) yes P1 . Zr1 . O1 . 121.28(5) yes P2 . Zr1 . O1 . 146.51(5) yes P3 . Zr1 . O1 . 118.84(5) yes Co1 . Zr1 . N1 . 85.91(6) yes P1 . Zr1 . N1 . 36.22(6) yes P2 . Zr1 . N1 . 107.72(6) yes P3 . Zr1 . N1 . 110.98(7) yes O1 . Zr1 . N1 . 86.14(8) yes Co1 . Zr1 . N2 . 88.71(6) yes P1 . Zr1 . N2 . 107.28(6) yes P2 . Zr1 . N2 . 37.54(6) yes P3 . Zr1 . N2 . 113.51(6) yes O1 . Zr1 . N2 . 108.97(7) yes Co1 . Zr1 . N3 . 87.24(6) yes P1 . Zr1 . N3 . 118.43(6) yes P2 . Zr1 . N3 . 106.23(6) yes P3 . Zr1 . N3 . 37.50(6) yes O1 . Zr1 . N3 . 85.66(7) yes N1 . Zr1 . N2 . 115.81(9) yes N1 . Zr1 . N3 . 129.41(9) yes N2 . Zr1 . N3 . 114.06(9) yes Co101 . Zr101 . P101 . 50.106(16) yes Co101 . Zr101 . P102 . 50.074(17) yes P101 . Zr101 . P102 . 85.23(2) yes Co101 . Zr101 . P103 . 50.819(17) yes P101 . Zr101 . P103 . 83.77(2) yes P102 . Zr101 . P103 . 81.74(2) yes Co101 . Zr101 . O101 . 163.92(5) yes P101 . Zr101 . O101 . 120.09(5) yes P102 . Zr101 . O101 . 122.18(5) yes P103 . Zr101 . O101 . 145.23(5) yes Co101 . Zr101 . N101 . 86.64(6) yes P101 . Zr101 . N101 . 37.44(6) yes P102 . Zr101 . N101 . 118.96(6) yes P103 . Zr101 . N101 . 103.83(6) yes O101 . Zr101 . N101 . 86.86(8) yes Co101 . Zr101 . N102 . 86.64(6) yes P101 . Zr101 . N102 . 110.36(6) yes P102 . Zr101 . N102 . 36.72(6) yes P103 . Zr101 . N102 . 110.37(6) yes O101 . Zr101 . N102 . 86.02(8) yes Co101 . Zr101 . N103 . 88.08(6) yes P101 . Zr101 . N103 . 115.20(6) yes P102 . Zr101 . N103 . 104.20(6) yes P103 . Zr101 . N103 . 37.63(6) yes O101 . Zr101 . N103 . 107.98(8) yes N101 . Zr101 . N102 . 128.84(8) yes N101 . Zr101 . N103 . 116.46(8) yes N102 . Zr101 . N103 . 113.91(8) yes Zr1 . Co1 . P1 . 75.94(2) yes Zr1 . Co1 . P2 . 73.27(2) yes P1 . Co1 . P2 . 108.65(3) yes Zr1 . Co1 . P3 . 74.11(2) yes P1 . Co1 . P3 . 116.64(3) yes P2 . Co1 . P3 . 113.90(3) yes Zr1 . Co1 . N4 . 177.68(7) yes P1 . Co1 . N4 . 106.02(7) yes P2 . Co1 . N4 . 104.79(7) yes P3 . Co1 . N4 . 105.82(7) yes Zr101 . Co101 . P101 . 74.44(2) yes Zr101 . Co101 . P102 . 74.91(2) yes P101 . Co101 . P102 . 116.71(3) yes Zr101 . Co101 . P103 . 73.38(2) yes P101 . Co101 . P103 . 112.58(3) yes P102 . Co101 . P103 . 109.45(3) yes Zr101 . Co101 . N104 . 178.08(7) yes P101 . Co101 . N104 . 107.39(7) yes P102 . Co101 . N104 . 104.54(7) yes P103 . Co101 . N104 . 105.21(7) yes Zr1 . P1 . Co1 . 54.336(19) yes Zr1 . P1 . N1 . 48.74(8) yes Co1 . P1 . N1 . 103.02(8) yes Zr1 . P1 . C9 . 129.83(9) yes Co1 . P1 . C9 . 116.52(9) yes N1 . P1 . C9 . 108.85(12) yes Zr1 . P1 . C12 . 122.95(10) yes Co1 . P1 . C12 . 116.58(10) yes N1 . P1 . C12 . 105.83(13) yes C9 . P1 . C12 . 105.38(13) yes Zr1 . P2 . Co1 . 55.554(18) yes Zr1 . P2 . N2 . 48.71(7) yes Co1 . P2 . N2 . 104.25(8) yes Zr1 . P2 . C23 . 127.66(9) yes Co1 . P2 . C23 . 119.05(9) yes N2 . P2 . C23 . 105.31(12) yes Zr1 . P2 . C26 . 129.29(9) yes Co1 . P2 . C26 . 120.09(9) yes N2 . P2 . C26 . 107.40(12) yes C23 . P2 . C26 . 99.60(12) yes Zr1 . P3 . Co1 . 55.394(19) yes Zr1 . P3 . N3 . 50.58(7) yes Co1 . P3 . N3 . 104.92(8) yes Zr1 . P3 . C37 . 119.48(11) yes Co1 . P3 . C37 . 120.97(12) yes N3 . P3 . C37 . 104.32(13) yes Zr1 . P3 . C41 . 143.9(2) yes Co1 . P3 . C41 . 125.5(2) yes N3 . P3 . C41 . 107.3(2) yes C37 . P3 . C41 . 91.7(3) yes Zr1 . P3 . Co1 . 55.394(19) yes Zr1 . P3 . N3 . 50.58(7) yes Co1 . P3 . N3 . 104.92(8) yes Zr1 . P3 . C37 . 119.48(11) yes Co1 . P3 . C37 . 120.97(12) yes N3 . P3 . C37 . 104.32(13) yes Zr1 . P3 . C43 . 129.7(2) yes Co1 . P3 . C43 . 111.0(2) yes N3 . P3 . C43 . 105.57(19) yes C37 . P3 . C43 . 108.7(2) yes Zr101 . P101 . Co101 . 55.451(18) yes Zr101 . P101 . N101 . 50.77(7) yes Co101 . P101 . N101 . 104.93(7) yes Zr101 . P101 . C109 . 141.17(9) yes Co101 . P101 . C109 . 122.09(9) yes N101 . P101 . C109 . 106.74(12) yes Zr101 . P101 . C112 . 116.90(9) yes Co101 . P101 . C112 . 117.82(9) yes N101 . P101 . C112 . 105.42(12) yes C109 . P101 . C112 . 98.48(12) yes Zr101 . P102 . Co101 . 55.019(19) yes Zr101 . P102 . N102 . 49.42(8) yes Co101 . P102 . N102 . 104.22(8) yes Zr101 . P102 . C123 . 122.13(9) yes Co101 . P102 . C123 . 117.08(9) yes N102 . P102 . C123 . 105.99(12) yes Zr101 . P102 . C126 . 129.05(9) yes Co101 . P102 . C126 . 115.76(9) yes N102 . P102 . C126 . 106.18(12) yes C123 . P102 . C126 . 106.63(12) yes Zr101 . P103 . Co101 . 55.802(18) yes Zr101 . P103 . N103 . 48.73(7) yes Co101 . P103 . N103 . 104.03(8) yes Zr101 . P103 . C140 . 134.8(8) yes Co101 . P103 . C140 . 125.9(7) yes N103 . P103 . C140 . 112.2(7) yes Zr101 . P103 . C142 . 131.74(9) yes Co101 . P103 . C142 . 117.70(9) yes N103 . P103 . C142 . 105.48(12) yes C140 . P103 . C142 . 90.1(8) yes Zr101 . P103 . Co101 . 55.802(18) yes Zr101 . P103 . N103 . 48.73(7) yes Co101 . P103 . N103 . 104.03(8) yes Zr101 . P103 . C137 . 116.55(13) yes Co101 . P103 . C137 . 114.21(12) yes N103 . P103 . C137 . 105.08(13) yes Zr101 . P103 . C142 . 131.74(9) yes Co101 . P103 . C142 . 117.70(9) yes N103 . P103 . C142 . 105.48(12) yes C137 . P103 . C142 . 109.04(15) yes Zr1 . O1 . C45 . 122.39(15) yes Zr1 . O1 . C48 . 127.24(14) yes C45 . O1 . C48 . 109.29(19) yes Zr101 . O101 . C145 . 122.53(17) yes Zr101 . O101 . C148 . 127.41(17) yes C145 . O101 . C148 . 109.5(2) yes P1 . N1 . Zr1 . 95.04(10) yes P1 . N1 . C1 . 134.82(19) yes Zr1 . N1 . C1 . 129.69(18) yes P2 . N2 . Zr1 . 93.75(10) yes P2 . N2 . C15 . 142.81(18) yes Zr1 . N2 . C15 . 121.69(16) yes P3 . N3 . Zr1 . 91.92(10) yes P3 . N3 . C29 . 132.37(19) yes Zr1 . N3 . C29 . 135.64(18) yes Co1 . N4 . N5 . 179.3(2) yes P101 . N101 . Zr101 . 91.80(9) yes P101 . N101 . C101 . 130.07(18) yes Zr101 . N101 . C101 . 138.02(18) yes P102 . N102 . Zr101 . 93.86(10) yes P102 . N102 . C115 . 135.10(18) yes Zr101 . N102 . C115 . 122.02(17) yes P103 . N103 . Zr101 . 93.64(10) yes P103 . N103 . C129 . 140.32(18) yes Zr101 . N103 . C129 . 122.33(16) yes Co101 . N104 . N105 . 177.7(2) yes N1 . C1 . C2 . 121.4(3) yes N1 . C1 . C6 . 120.5(2) yes C2 . C1 . C6 . 117.8(3) yes C1 . C2 . C3 . 121.7(3) yes C1 . C2 . H21 . 117.8 no C3 . C2 . H21 . 120.5 no C2 . C3 . C4 . 118.6(3) yes C2 . C3 . C7 . 120.5(3) yes C4 . C3 . C7 . 120.9(3) yes C3 . C4 . C5 . 121.5(3) yes C3 . C4 . H41 . 119.7 no C5 . C4 . H41 . 118.8 no C4 . C5 . C6 . 118.7(3) yes C4 . C5 . C8 . 121.2(3) yes C6 . C5 . C8 . 120.1(3) yes C5 . C6 . C1 . 121.7(3) yes C5 . C6 . H61 . 119.0 no C1 . C6 . H61 . 119.3 no C3 . C7 . H71 . 111.6 no C3 . C7 . H72 . 109.5 no H71 . C7 . H72 . 109.0 no C3 . C7 . H73 . 109.1 no H71 . C7 . H73 . 107.8 no H72 . C7 . H73 . 109.9 no C5 . C8 . H81 . 109.4 no C5 . C8 . H82 . 109.1 no H81 . C8 . H82 . 110.2 no C5 . C8 . H83 . 108.8 no H81 . C8 . H83 . 109.5 no H82 . C8 . H83 . 109.7 no P1 . C9 . C10 . 118.6(2) yes P1 . C9 . C11 . 112.24(19) yes C10 . C9 . C11 . 109.3(2) yes P1 . C9 . H91 . 102.9 no C10 . C9 . H91 . 106.9 no C11 . C9 . H91 . 105.7 no C9 . C10 . H101 . 108.8 no C9 . C10 . H102 . 110.9 no H101 . C10 . H102 . 109.3 no C9 . C10 . H103 . 109.7 no H101 . C10 . H103 . 108.0 no H102 . C10 . H103 . 110.1 no C9 . C11 . H111 . 111.2 no C9 . C11 . H112 . 112.7 no H111 . C11 . H112 . 107.4 no C9 . C11 . H113 . 110.9 no H111 . C11 . H113 . 106.8 no H112 . C11 . H113 . 107.5 no P1 . C12 . C13 . 119.0(2) yes P1 . C12 . C14 . 111.7(2) yes C13 . C12 . C14 . 109.9(2) yes P1 . C12 . H121 . 101.6 no C13 . C12 . H121 . 106.7 no C14 . C12 . H121 . 106.8 no C12 . C13 . H131 . 108.5 no C12 . C13 . H132 . 110.2 no H131 . C13 . H132 . 109.1 no C12 . C13 . H133 . 111.0 no H131 . C13 . H133 . 109.5 no H132 . C13 . H133 . 108.5 no C12 . C14 . H141 . 108.4 no C12 . C14 . H142 . 111.1 no H141 . C14 . H142 . 110.3 no C12 . C14 . H143 . 108.3 no H141 . C14 . H143 . 109.7 no H142 . C14 . H143 . 108.9 no N2 . C15 . C16 . 119.6(2) yes N2 . C15 . C20 . 121.3(2) yes C16 . C15 . C20 . 118.3(2) yes C15 . C16 . C17 . 121.3(2) yes C15 . C16 . H161 . 119.7 no C17 . C16 . H161 . 118.9 no C16 . C17 . C18 . 119.2(2) yes C16 . C17 . C21 . 120.3(2) yes C18 . C17 . C21 . 120.4(3) yes C17 . C18 . C19 . 120.7(3) yes C17 . C18 . H181 . 120.2 no C19 . C18 . H181 . 119.1 no C18 . C19 . C20 . 118.8(2) yes C18 . C19 . C22 . 120.0(3) yes C20 . C19 . C22 . 121.1(3) yes C15 . C20 . C19 . 121.6(2) yes C15 . C20 . H201 . 118.2 no C19 . C20 . H201 . 120.1 no C17 . C21 . H211 . 110.9 no C17 . C21 . H212 . 111.6 no H211 . C21 . H212 . 108.2 no C17 . C21 . H213 . 111.7 no H211 . C21 . H213 . 108.0 no H212 . C21 . H213 . 106.2 no C19 . C22 . H221 . 111.5 no C19 . C22 . H222 . 110.4 no H221 . C22 . H222 . 107.9 no C19 . C22 . H223 . 110.1 no H221 . C22 . H223 . 107.2 no H222 . C22 . H223 . 109.6 no P2 . C23 . C24 . 115.67(19) yes P2 . C23 . C25 . 112.08(19) yes C24 . C23 . C25 . 109.8(2) yes P2 . C23 . H231 . 104.1 no C24 . C23 . H231 . 107.2 no C25 . C23 . H231 . 107.4 no C23 . C24 . H241 . 110.2 no C23 . C24 . H242 . 109.8 no H241 . C24 . H242 . 108.8 no C23 . C24 . H243 . 110.9 no H241 . C24 . H243 . 109.0 no H242 . C24 . H243 . 108.0 no C23 . C25 . H251 . 110.6 no C23 . C25 . H252 . 110.4 no H251 . C25 . H252 . 109.1 no C23 . C25 . H253 . 109.9 no H251 . C25 . H253 . 108.5 no H252 . C25 . H253 . 108.3 no P2 . C26 . C27 . 110.33(19) yes P2 . C26 . C28 . 112.9(2) yes C27 . C26 . C28 . 112.6(2) yes P2 . C26 . H261 . 106.8 no C27 . C26 . H261 . 106.6 no C28 . C26 . H261 . 107.2 no C26 . C27 . H271 . 110.7 no C26 . C27 . H272 . 110.3 no H271 . C27 . H272 . 109.2 no C26 . C27 . H273 . 111.2 no H271 . C27 . H273 . 107.2 no H272 . C27 . H273 . 108.3 no C26 . C28 . H281 . 109.7 no C26 . C28 . H282 . 108.5 no H281 . C28 . H282 . 109.4 no C26 . C28 . H283 . 109.8 no H281 . C28 . H283 . 108.0 no H282 . C28 . H283 . 111.3 no N3 . C29 . C30 . 124.7(3) yes N3 . C29 . C34 . 117.9(2) yes C30 . C29 . C34 . 117.4(3) yes C29 . C30 . C31 . 121.3(3) yes C29 . C30 . H301 . 119.2 no C31 . C30 . H301 . 119.6 no C30 . C31 . C32 . 119.4(3) yes C30 . C31 . C35 . 119.1(3) yes C32 . C31 . C35 . 121.5(3) yes C31 . C32 . C33 . 121.0(3) yes C31 . C32 . H321 . 119.2 no C33 . C32 . H321 . 119.7 no C32 . C33 . C34 . 118.3(3) yes C32 . C33 . C36 . 121.0(3) yes C34 . C33 . C36 . 120.7(3) yes C29 . C34 . C33 . 122.5(3) yes C29 . C34 . H341 . 119.5 no C33 . C34 . H341 . 118.0 no C31 . C35 . H351 . 111.7 no C31 . C35 . H352 . 112.7 no H351 . C35 . H352 . 108.5 no C31 . C35 . H353 . 111.3 no H351 . C35 . H353 . 106.3 no H352 . C35 . H353 . 106.0 no C33 . C36 . H361 . 111.6 no C33 . C36 . H362 . 110.5 no H361 . C36 . H362 . 108.1 no C33 . C36 . H363 . 110.5 no H361 . C36 . H363 . 107.9 no H362 . C36 . H363 . 108.1 no P3 . C37 . C38 . 113.2(2) yes P3 . C37 . C39 . 110.9(2) yes C38 . C37 . C39 . 110.8(3) yes P3 . C37 . H371 . 109.4 no C38 . C37 . H371 . 102.3 no C39 . C37 . H371 . 109.9 no C37 . C38 . H381 . 106.5 no C37 . C38 . H382 . 108.0 no H381 . C38 . H382 . 108.7 no C37 . C38 . H383 . 109.9 no H381 . C38 . H383 . 111.1 no H382 . C38 . H383 . 112.4 no C37 . C39 . H392 . 108.8 no C37 . C39 . H393 . 109.8 no H392 . C39 . H393 . 110.5 no C37 . C39 . H396 . 108.2 no H392 . C39 . H396 . 109.9 no H393 . C39 . H396 . 109.5 no C41 . C40 . H443 . 110.0 no C41 . C40 . H445 . 110.9 no H443 . C40 . H445 . 108.5 no C41 . C40 . H446 . 110.3 no H443 . C40 . H446 . 109.0 no H445 . C40 . H446 . 108.1 no C43 . C40 . H441 . 109.9 no C43 . C40 . H442 . 110.2 no H441 . C40 . H442 . 109.0 no C43 . C40 . H444 . 111.3 no H441 . C40 . H444 . 107.7 no H442 . C40 . H444 . 108.6 no C40 . C41 . P3 . 113.4(4) yes C40 . C41 . C42 . 109.7(5) yes P3 . C41 . C42 . 111.7(5) yes C40 . C41 . H421 . 108.2 no P3 . C41 . H421 . 106.4 no C42 . C41 . H421 . 107.1 no C41 . C42 . H431 . 108.8 no C41 . C42 . H432 . 108.9 no H431 . C42 . H432 . 109.2 no C41 . C42 . H433 . 111.3 no H431 . C42 . H433 . 109.6 no H432 . C42 . H433 . 109.0 no C40 . C43 . P3 . 109.8(3) yes C40 . C43 . C44 . 112.0(5) yes P3 . C43 . C44 . 117.9(4) yes C40 . C43 . H451 . 106.8 no P3 . C43 . H451 . 104.3 no C44 . C43 . H451 . 105.1 no C43 . C44 . H461 . 108.6 no C43 . C44 . H462 . 109.3 no H461 . C44 . H462 . 109.2 no C43 . C44 . H463 . 109.7 no H461 . C44 . H463 . 109.2 no H462 . C44 . H463 . 110.8 no O1 . C45 . C46 . 105.3(2) yes O1 . C45 . H501 . 109.5 no C46 . C45 . H501 . 111.8 no O1 . C45 . H502 . 108.7 no C46 . C45 . H502 . 110.5 no H501 . C45 . H502 . 110.8 no C45 . C46 . C47 . 103.1(2) yes C45 . C46 . H491 . 111.7 no C47 . C46 . H491 . 111.7 no C45 . C46 . H492 . 110.2 no C47 . C46 . H492 . 112.1 no H491 . C46 . H492 . 107.9 no C46 . C47 . C48 . 101.4(2) yes C46 . C47 . H481 . 109.6 no C48 . C47 . H481 . 110.1 no C46 . C47 . H482 . 112.7 no C48 . C47 . H482 . 111.6 no H481 . C47 . H482 . 111.1 no C47 . C48 . O1 . 104.3(2) yes C47 . C48 . H471 . 112.2 no O1 . C48 . H471 . 107.6 no C47 . C48 . H472 . 113.3 no O1 . C48 . H472 . 109.7 no H471 . C48 . H472 . 109.5 no N101 . C101 . C102 . 124.3(2) yes N101 . C101 . C106 . 118.5(2) yes C102 . C101 . C106 . 117.1(2) yes C101 . C102 . C103 . 121.5(3) yes C101 . C102 . H1021 . 119.5 no C103 . C102 . H1021 . 119.0 no C102 . C103 . C104 . 119.1(3) yes C102 . C103 . C107 . 120.2(3) yes C104 . C103 . C107 . 120.7(3) yes C103 . C104 . C105 . 121.2(3) yes C103 . C104 . H1041 . 118.5 no C105 . C104 . H1041 . 120.3 no C104 . C105 . C106 . 118.6(3) yes C104 . C105 . C108 . 120.6(3) yes C106 . C105 . C108 . 120.8(3) yes C101 . C106 . C105 . 122.4(3) yes C101 . C106 . H1061 . 119.5 no C105 . C106 . H1061 . 118.1 no C103 . C107 . H1071 . 110.9 no C103 . C107 . H1072 . 112.1 no H1071 . C107 . H1072 . 106.8 no C103 . C107 . H1073 . 110.3 no H1071 . C107 . H1073 . 107.4 no H1072 . C107 . H1073 . 109.2 no C105 . C108 . H1081 . 110.6 no C105 . C108 . H1082 . 113.0 no H1081 . C108 . H1082 . 107.4 no C105 . C108 . H1083 . 110.5 no H1081 . C108 . H1083 . 106.5 no H1082 . C108 . H1083 . 108.6 no P101 . C109 . C110 . 114.75(19) yes P101 . C109 . C111 . 111.82(19) yes C110 . C109 . C111 . 110.3(2) yes P101 . C109 . H1091 . 105.4 no C110 . C109 . H1091 . 107.4 no C111 . C109 . H1091 . 106.7 no C109 . C110 . H1101 . 111.6 no C109 . C110 . H1102 . 110.5 no H1101 . C110 . H1102 . 108.1 no C109 . C110 . H1103 . 108.5 no H1101 . C110 . H1103 . 108.4 no H1102 . C110 . H1103 . 109.7 no C109 . C111 . H1111 . 109.4 no C109 . C111 . H1112 . 110.2 no H1111 . C111 . H1112 . 107.5 no C109 . C111 . H1113 . 110.8 no H1111 . C111 . H1113 . 108.7 no H1112 . C111 . H1113 . 110.1 no P101 . C112 . C113 . 110.93(19) yes P101 . C112 . C114 . 111.77(18) yes C113 . C112 . C114 . 111.9(2) yes P101 . C112 . H1121 . 108.2 no C113 . C112 . H1121 . 106.2 no C114 . C112 . H1121 . 107.5 no C112 . C113 . H1131 . 110.9 no C112 . C113 . H1132 . 108.8 no H1131 . C113 . H1132 . 109.1 no C112 . C113 . H1133 . 110.7 no H1131 . C113 . H1133 . 108.6 no H1132 . C113 . H1133 . 108.8 no C112 . C114 . H1141 . 110.3 no C112 . C114 . H1142 . 110.1 no H1141 . C114 . H1142 . 109.1 no C112 . C114 . H1143 . 109.1 no H1141 . C114 . H1143 . 110.3 no H1142 . C114 . H1143 . 108.0 no N102 . C115 . C116 . 121.2(2) yes N102 . C115 . C120 . 120.9(2) yes C116 . C115 . C120 . 117.4(3) yes C115 . C116 . C117 . 121.7(3) yes C115 . C116 . H1161 . 119.5 no C117 . C116 . H1161 . 118.7 no C116 . C117 . C118 . 119.0(3) yes C116 . C117 . C121 . 120.2(3) yes C118 . C117 . C121 . 120.7(3) yes C117 . C118 . C119 . 121.8(3) yes C117 . C118 . H1181 . 118.5 no C119 . C118 . H1181 . 119.7 no C118 . C119 . C120 . 117.8(3) yes C118 . C119 . C122 . 120.7(3) yes C120 . C119 . C122 . 121.4(3) yes C115 . C120 . C119 . 122.2(2) yes C115 . C120 . H1201 . 118.7 no C119 . C120 . H1201 . 119.1 no C117 . C121 . H1211 . 112.2 no C117 . C121 . H1212 . 111.4 no H1211 . C121 . H1212 . 107.8 no C117 . C121 . H1213 . 111.7 no H1211 . C121 . H1213 . 106.4 no H1212 . C121 . H1213 . 107.1 no C119 . C122 . H1221 . 111.7 no C119 . C122 . H1222 . 110.2 no H1221 . C122 . H1222 . 106.9 no C119 . C122 . H1223 . 110.1 no H1221 . C122 . H1223 . 109.3 no H1222 . C122 . H1223 . 108.5 no P102 . C123 . C124 . 117.2(2) yes P102 . C123 . C125 . 112.72(19) yes C124 . C123 . C125 . 110.0(2) yes P102 . C123 . H1231 . 103.1 no C124 . C123 . H1231 . 105.3 no C125 . C123 . H1231 . 107.5 no C123 . C124 . H1241 . 112.0 no C123 . C124 . H1242 . 112.3 no H1241 . C124 . H1242 . 108.4 no C123 . C124 . H1243 . 108.8 no H1241 . C124 . H1243 . 105.5 no H1242 . C124 . H1243 . 109.6 no C123 . C125 . H1251 . 110.6 no C123 . C125 . H1252 . 109.9 no H1251 . C125 . H1252 . 109.4 no C123 . C125 . H1253 . 110.2 no H1251 . C125 . H1253 . 106.3 no H1252 . C125 . H1253 . 110.4 no P102 . C126 . C127 . 118.7(2) yes P102 . C126 . C128 . 112.10(18) yes C127 . C126 . C128 . 110.4(2) yes P102 . C126 . H1261 . 102.2 no C127 . C126 . H1261 . 105.6 no C128 . C126 . H1261 . 106.6 no C126 . C127 . H1271 . 109.1 no C126 . C127 . H1272 . 111.6 no H1271 . C127 . H1272 . 107.8 no C126 . C127 . H1273 . 111.3 no H1271 . C127 . H1273 . 108.5 no H1272 . C127 . H1273 . 108.3 no C126 . C128 . H1281 . 111.3 no C126 . C128 . H1282 . 110.2 no H1281 . C128 . H1282 . 110.2 no C126 . C128 . H1283 . 109.3 no H1281 . C128 . H1283 . 108.2 no H1282 . C128 . H1283 . 107.5 no N103 . C129 . C130 . 121.2(2) yes N103 . C129 . C134 . 119.7(2) yes C130 . C129 . C134 . 118.6(3) yes C129 . C130 . C131 . 120.2(3) yes C129 . C130 . H1301 . 120.3 no C131 . C130 . H1301 . 119.5 no C130 . C131 . C132 . 118.4(3) yes C130 . C131 . C135 . 119.2(3) yes C132 . C131 . C135 . 122.4(3) yes C131 . C132 . C133 . 123.0(3) yes C131 . C132 . H1321 . 118.5 no C133 . C132 . H1321 . 118.5 no C132 . C133 . C134 . 118.0(3) yes C132 . C133 . C136 . 121.6(3) yes C134 . C133 . C136 . 120.4(3) yes C129 . C134 . C133 . 121.8(3) yes C129 . C134 . H1341 . 120.1 no C133 . C134 . H1341 . 118.1 no C131 . C135 . H1351 . 110.2 no C131 . C135 . H1352 . 111.9 no H1351 . C135 . H1352 . 104.6 no C131 . C135 . H1353 . 112.4 no H1351 . C135 . H1353 . 108.6 no H1352 . C135 . H1353 . 108.9 no C133 . C136 . H1361 . 109.2 no C133 . C136 . H1362 . 109.0 no H1361 . C136 . H1362 . 108.8 no C133 . C136 . H1363 . 110.5 no H1361 . C136 . H1363 . 109.0 no H1362 . C136 . H1363 . 110.3 no P103 . C137 . C138 . 119.0(2) yes P103 . C137 . C139 . 111.5(2) yes C138 . C137 . C139 . 109.8(3) yes P103 . C137 . H1371 . 103.4 no C138 . C137 . H1371 . 104.9 no C139 . C137 . H1371 . 107.3 no C137 . C138 . H1381 . 110.4 no C137 . C138 . H1382 . 110.1 no H1381 . C138 . H1382 . 106.7 no C137 . C138 . H1383 . 110.5 no H1381 . C138 . H1383 . 109.9 no H1382 . C138 . H1383 . 109.2 no C140 . C139 . H1391 . 109.5 no C140 . C139 . H1392 . 109.3 no H1391 . C139 . H1392 . 109.0 no C140 . C139 . H1394 . 110.4 no H1391 . C139 . H1394 . 109.2 no H1392 . C139 . H1394 . 109.4 no C137 . C139 . H1393 . 110.3 no C137 . C139 . H1395 . 108.4 no H1393 . C139 . H1395 . 108.9 no C137 . C139 . H1396 . 111.6 no H1393 . C139 . H1396 . 109.7 no H1395 . C139 . H1396 . 107.9 no P103 . C140 . C139 . 111.5(12) yes P103 . C140 . C141 . 113.7(17) yes C139 . C140 . C141 . 102.3(17) yes P103 . C140 . H1401 . 110.2 no C139 . C140 . H1401 . 109.7 no C141 . C140 . H1401 . 109.2 no C140 . C141 . H1411 . 109.9 no C140 . C141 . H1412 . 109.5 no H1411 . C141 . H1412 . 109.1 no C140 . C141 . H1413 . 109.6 no H1411 . C141 . H1413 . 109.2 no H1412 . C141 . H1413 . 109.5 no P103 . C142 . C143 . 116.08(19) yes P103 . C142 . C144 . 112.84(19) yes C143 . C142 . C144 . 109.6(2) yes P103 . C142 . H1421 . 102.7 no C143 . C142 . H1421 . 106.8 no C144 . C142 . H1421 . 108.1 no C142 . C143 . H1431 . 111.6 no C142 . C143 . H1432 . 111.9 no H1431 . C143 . H1432 . 108.8 no C142 . C143 . H1433 . 107.9 no H1431 . C143 . H1433 . 108.4 no H1432 . C143 . H1433 . 108.2 no C142 . C144 . H1441 . 109.4 no C142 . C144 . H1442 . 110.6 no H1441 . C144 . H1442 . 108.0 no C142 . C144 . H1443 . 111.3 no H1441 . C144 . H1443 . 108.2 no H1442 . C144 . H1443 . 109.3 no O101 . C145 . C146 . 103.8(3) yes O101 . C145 . H1451 . 110.0 no C146 . C145 . H1451 . 112.6 no O101 . C145 . H1452 . 108.3 no C146 . C145 . H1452 . 113.0 no H1451 . C145 . H1452 . 108.9 no C145 . C146 . C147 . 104.9(3) yes C145 . C146 . H1461 . 108.9 no C147 . C146 . H1461 . 113.2 no C145 . C146 . H1462 . 109.6 no C147 . C146 . H1462 . 108.4 no H1461 . C146 . H1462 . 111.5 no C146 . C147 . C148 . 102.8(3) yes C146 . C147 . H1471 . 108.1 no C148 . C147 . H1471 . 110.3 no C146 . C147 . H1472 . 111.6 no C148 . C147 . H1472 . 113.1 no H1471 . C147 . H1472 . 110.6 no C147 . C148 . O101 . 105.8(3) yes C147 . C148 . H1481 . 111.1 no O101 . C148 . H1481 . 109.9 no C147 . C148 . H1482 . 110.1 no O101 . C148 . H1482 . 109.7 no H1481 . C148 . H1482 . 110.1 no _iucr_refine_instructions_details_constraints ; # # Punched on 16/07/12 at 14:56:14 # #LIST 12 BLOCK CONT SCALE CONT ZR ( 1 ,X'S,U'S) UNTIL C ( 40 ) CONT C ( 41 ,X'S,U[ISO]) UNTIL C ( 44 ) CONT C ( 45 ,X'S,U'S) UNTIL C ( 136 ) CONT C ( 137 ,X'S,U[ISO]) UNTIL C ( 138 ) CONT C ( 139 ,X'S,U'S) CONT C ( 140 ,X'S,U[ISO]) UNTIL C ( 141 ) CONT C ( 142 ,X'S,U'S) UNTIL C ( 148 ) SUMFIX PART(1001, OCC) AND PART(1002, OCC) SUMFIX PART(1003, OCC) AND PART(1004, OCC) RIDE C ( 2,X'S) H ( 21,X'S) RIDE C ( 4,X'S) H ( 41,X'S) RIDE C ( 6,X'S) H ( 61,X'S) RIDE C ( 7,X'S) H ( 71,X'S) H ( 72,X'S) H ( 73,X'S) RIDE C ( 8,X'S) H ( 81,X'S) H ( 82,X'S) H ( 83,X'S) RIDE C ( 9,X'S) H ( 91,X'S) RIDE C ( 10,X'S) H ( 101,X'S) H ( 102,X'S) H ( 103,X'S) RIDE C ( 11,X'S) H ( 111,X'S) H ( 112,X'S) H ( 113,X'S) RIDE C ( 12,X'S) H ( 121,X'S) RIDE C ( 13,X'S) H ( 131,X'S) H ( 132,X'S) H ( 133,X'S) RIDE C ( 14,X'S) H ( 141,X'S) H ( 142,X'S) H ( 143,X'S) RIDE C ( 16,X'S) H ( 161,X'S) RIDE C ( 18,X'S) H ( 181,X'S) RIDE C ( 20,X'S) H ( 201,X'S) RIDE C ( 21,X'S) H ( 211,X'S) H ( 212,X'S) H ( 213,X'S) RIDE C ( 22,X'S) H ( 221,X'S) H ( 222,X'S) H ( 223,X'S) RIDE C ( 23,X'S) H ( 231,X'S) RIDE C ( 24,X'S) H ( 241,X'S) H ( 242,X'S) H ( 243,X'S) RIDE C ( 25,X'S) H ( 251,X'S) H ( 252,X'S) H ( 253,X'S) RIDE C ( 26,X'S) H ( 261,X'S) RIDE C ( 27,X'S) H ( 271,X'S) H ( 272,X'S) H ( 273,X'S) RIDE C ( 28,X'S) H ( 281,X'S) H ( 282,X'S) H ( 283,X'S) RIDE C ( 30,X'S) H ( 301,X'S) RIDE C ( 32,X'S) H ( 321,X'S) RIDE C ( 34,X'S) H ( 341,X'S) RIDE C ( 35,X'S) H ( 351,X'S) H ( 352,X'S) H ( 353,X'S) RIDE C ( 36,X'S) H ( 361,X'S) H ( 362,X'S) H ( 363,X'S) RIDE C ( 37,X'S) H ( 371,X'S) RIDE C ( 38,X'S) H ( 381,X'S) H ( 382,X'S) H ( 383,X'S) RIDE C ( 39,X'S) H ( 392,X'S) H ( 393,X'S) H ( 396,X'S) RIDE C ( 40,X'S) H ( 443,X'S) H ( 445,X'S) H ( 446,X'S) CONT H ( 441,X'S) H ( 442,X'S) H ( 444,X'S) RIDE C ( 41,X'S) H ( 421,X'S) RIDE C ( 42,X'S) H ( 431,X'S) H ( 432,X'S) H ( 433,X'S) RIDE C ( 43,X'S) H ( 451,X'S) RIDE C ( 44,X'S) H ( 461,X'S) H ( 462,X'S) H ( 463,X'S) RIDE C ( 45,X'S) H ( 501,X'S) H ( 502,X'S) RIDE C ( 46,X'S) H ( 491,X'S) H ( 492,X'S) RIDE C ( 47,X'S) H ( 481,X'S) H ( 482,X'S) RIDE C ( 48,X'S) H ( 471,X'S) H ( 472,X'S) RIDE C ( 102,X'S) H (1021,X'S) RIDE C ( 104,X'S) H (1041,X'S) RIDE C ( 106,X'S) H (1061,X'S) RIDE C ( 107,X'S) H (1071,X'S) H (1072,X'S) H (1073,X'S) RIDE C ( 108,X'S) H (1081,X'S) H (1082,X'S) H (1083,X'S) RIDE C ( 109,X'S) H (1091,X'S) RIDE C ( 110,X'S) H (1101,X'S) H (1102,X'S) H (1103,X'S) RIDE C ( 111,X'S) H (1111,X'S) H (1112,X'S) H (1113,X'S) RIDE C ( 112,X'S) H (1121,X'S) RIDE C ( 113,X'S) H (1131,X'S) H (1132,X'S) H (1133,X'S) RIDE C ( 114,X'S) H (1141,X'S) H (1142,X'S) H (1143,X'S) RIDE C ( 116,X'S) H (1161,X'S) RIDE C ( 118,X'S) H (1181,X'S) RIDE C ( 120,X'S) H (1201,X'S) RIDE C ( 121,X'S) H (1211,X'S) H (1212,X'S) H (1213,X'S) RIDE C ( 122,X'S) H (1221,X'S) H (1222,X'S) H (1223,X'S) RIDE C ( 123,X'S) H (1231,X'S) RIDE C ( 124,X'S) H (1241,X'S) H (1242,X'S) H (1243,X'S) RIDE C ( 125,X'S) H (1251,X'S) H (1252,X'S) H (1253,X'S) RIDE C ( 126,X'S) H (1261,X'S) RIDE C ( 127,X'S) H (1271,X'S) H (1272,X'S) H (1273,X'S) RIDE C ( 128,X'S) H (1281,X'S) H (1282,X'S) H (1283,X'S) RIDE C ( 130,X'S) H (1301,X'S) RIDE C ( 132,X'S) H (1321,X'S) RIDE C ( 134,X'S) H (1341,X'S) RIDE C ( 135,X'S) H (1351,X'S) H (1352,X'S) H (1353,X'S) RIDE C ( 136,X'S) H (1361,X'S) H (1362,X'S) H (1363,X'S) RIDE C ( 137,X'S) H (1371,X'S) RIDE C ( 138,X'S) H (1381,X'S) H (1382,X'S) H (1383,X'S) RIDE C ( 139,X'S) H (1391,X'S) H (1392,X'S) H (1394,X'S) CONT H (1393,X'S) H (1395,X'S) H (1396,X'S) RIDE C ( 140,X'S) H (1401,X'S) RIDE C ( 141,X'S) H (1411,X'S) H (1412,X'S) H (1413,X'S) RIDE C ( 142,X'S) H (1421,X'S) RIDE C ( 143,X'S) H (1431,X'S) H (1432,X'S) H (1433,X'S) RIDE C ( 144,X'S) H (1441,X'S) H (1442,X'S) H (1443,X'S) RIDE C ( 145,X'S) H (1451,X'S) H (1452,X'S) RIDE C ( 146,X'S) H (1461,X'S) H (1462,X'S) RIDE C ( 147,X'S) H (1471,X'S) H (1472,X'S) RIDE C ( 148,X'S) H (1481,X'S) H (1482,X'S) END ; _iucr_refine_instructions_details_restraints ; # # Punched on 16/07/12 at 14:56:14 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; _database_code_depnum_ccdc_archive 'CCDC 953851' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_5 _audit_creation_date 13-04-15 _audit_creation_method CRYSTALS_ver_14.41 _oxford_structure_analysis_title 'ZW_595_0m in P2(1)/n' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 12.0391(3) _cell_length_b 19.7151(5) _cell_length_c 21.9331(6) _cell_angle_alpha 90 _cell_angle_beta 97.6840(10) _cell_angle_gamma 90 _cell_volume 5159.1(2) _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall -P2yn 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' Br -0.2901 2.4595 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328 2.9557 '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 4 # Given Formula = C42 H69 Br2 Co1 N3 P3 Zr1 # Dc = 1.31 Fooo = 2096.00 Mu = 21.94 M = 1018.91 # Found Formula = C42 H69 Br2 Co1 N3 P3 Zr1 # Dc = 1.31 FOOO = 2096.00 Mu = 21.94 M = 1018.91 _chemical_formula_sum 'C42 H69 Br2 Co1 N3 P3 Zr1' _chemical_formula_moiety 'C42 H69 Br2 Co1 N3 P3 Zr1' _chemical_compound_source ? _chemical_formula_weight 1018.91 _cell_measurement_reflns_used 9875 _cell_measurement_theta_min 3 _cell_measurement_theta_max 28 _cell_measurement_temperature 135 _exptl_crystal_description 'prism fragment' _exptl_crystal_colour yellow _exptl_crystal_size_min 0.184 _exptl_crystal_size_mid 0.276 _exptl_crystal_size_max 0.279 _exptl_crystal_density_diffrn 1.312 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 2096 _exptl_absorpt_coefficient_mu 2.194 # Sheldrick geometric approximatio 0.55 0.67 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Analytical Absorption (De Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_min 0.55 _exptl_absorpt_correction_T_max 0.67 _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 135 _diffrn_reflns_number 12445 _reflns_number_total 12445 _diffrn_reflns_av_R_equivalents 0.042 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 12445 # Theoretical number of reflections is about 24923 _diffrn_reflns_theta_min 1.394 _diffrn_reflns_theta_max 28.004 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.004 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 28 _reflns_limit_h_min -15 _reflns_limit_h_max 15 _reflns_limit_k_min 0 _reflns_limit_k_max 26 _reflns_limit_l_min 0 _reflns_limit_l_max 28 _oxford_diffrn_Wilson_B_factor 1.74 _oxford_diffrn_Wilson_scale 221.77 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -1.07 _refine_diff_density_max 1.30 # 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 12445 _refine_ls_number_restraints 0 _refine_ls_number_parameters 469 _oxford_refine_ls_R_factor_ref 0.0440 _refine_ls_wR_factor_ref 0.0713 _refine_ls_goodness_of_fit_ref 0.9491 _refine_ls_shift/su_max 0.0019913 _refine_ls_shift/su_mean 0.0000439 # The values computed with all filters except I/sigma _oxford_reflns_number_all 12445 _refine_ls_R_factor_all 0.0440 _refine_ls_wR_factor_all 0.0713 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 9631 _refine_ls_R_factor_gt 0.0291 _refine_ls_wR_factor_gt 0.0669 # 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 constr #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^ + 4.30P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached 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 _atom_site_attached_hydrogens Zr1 Zr 0.393304(15) 0.171029(10) 0.601817(9) 0.0156 1.0000 Uani . . . . . . Br1 Br -0.030450(18) 0.159874(15) 0.546538(12) 0.0381 1.0000 Uani . . . . . . Br2 Br 0.270321(18) 0.149548(12) 0.494752(10) 0.0274 1.0000 Uani . . . . . . Co1 Co 0.16209(2) 0.166252(15) 0.584719(13) 0.0202 1.0000 Uani . . . . . . P1 P 0.22175(5) 0.26588(3) 0.63082(3) 0.0235 1.0000 Uani . . . . . . P2 P 0.23193(4) 0.07935(3) 0.64755(2) 0.0196 1.0000 Uani . . . . . . P3 P 0.61598(4) 0.15719(3) 0.61494(2) 0.0180 1.0000 Uani . . . . . . N1 N 0.36200(14) 0.26060(9) 0.64749(8) 0.0211 1.0000 Uani . . . . . . N2 N 0.37329(14) 0.08454(9) 0.65569(8) 0.0201 1.0000 Uani . . . . . . N3 N 0.53508(14) 0.19470(9) 0.55666(8) 0.0188 1.0000 Uani . . . . . . C1 C 0.43418(17) 0.30503(11) 0.68588(10) 0.0239 1.0000 Uani . . . . . . C2 C 0.46448(19) 0.36841(11) 0.66546(12) 0.0290 1.0000 Uani . . . . . . C3 C 0.5384(2) 0.40965(13) 0.70363(13) 0.0366 1.0000 Uani . . . . . . C4 C 0.5801(2) 0.38668(15) 0.76196(14) 0.0427 1.0000 Uani . . . . . . C5 C 0.5510(2) 0.32400(15) 0.78333(12) 0.0389 1.0000 Uani . . . . . . C6 C 0.47765(19) 0.28324(13) 0.74452(11) 0.0300 1.0000 Uani . . . . . . C7 C 0.5737(3) 0.47710(14) 0.67982(16) 0.0541 1.0000 Uani . . . . . . C8 C 0.5974(3) 0.29977(19) 0.84680(13) 0.0586 1.0000 Uani . . . . . . C9 C 0.1901(2) 0.34519(13) 0.58685(14) 0.0388 1.0000 Uani . . . . . . C10 C 0.0639(3) 0.35898(18) 0.5741(2) 0.0716 1.0000 Uani . . . . . . C11 C 0.2422(3) 0.34359(14) 0.52795(14) 0.0511 1.0000 Uani . . . . . . C12 C 0.16600(19) 0.27928(13) 0.70516(12) 0.0319 1.0000 Uani . . . . . . C13 C 0.1988(2) 0.34614(14) 0.73773(15) 0.0446 1.0000 Uani . . . . . . C14 C 0.0382(2) 0.27028(15) 0.69993(15) 0.0466 1.0000 Uani . . . . . . C15 C 0.44800(17) 0.04119(11) 0.69404(10) 0.0225 1.0000 Uani . . . . . . C16 C 0.47254(18) -0.02387(11) 0.67565(11) 0.0256 1.0000 Uani . . . . . . C17 C 0.55207(19) -0.06412(12) 0.71154(12) 0.0321 1.0000 Uani . . . . . . C18 C 0.6022(2) -0.03907(13) 0.76728(12) 0.0371 1.0000 Uani . . . . . . C19 C 0.5782(2) 0.02568(14) 0.78747(11) 0.0363 1.0000 Uani . . . . . . C20 C 0.50268(19) 0.06554(13) 0.74990(11) 0.0295 1.0000 Uani . . . . . . C21 C 0.5859(2) -0.13104(13) 0.68625(15) 0.0434 1.0000 Uani . . . . . . C22 C 0.6355(3) 0.05366(18) 0.84791(14) 0.0589 1.0000 Uani . . . . . . C23 C 0.1915(2) 0.08296(12) 0.72672(11) 0.0303 1.0000 Uani . . . . . . C24 C 0.2216(2) 0.02065(14) 0.76626(12) 0.0385 1.0000 Uani . . . . . . C25 C 0.0674(2) 0.10044(15) 0.72557(13) 0.0445 1.0000 Uani . . . . . . C26 C 0.19255(19) -0.00712(12) 0.61952(11) 0.0279 1.0000 Uani . . . . . . C27 C 0.0669(2) -0.02164(14) 0.61774(13) 0.0399 1.0000 Uani . . . . . . C28 C 0.2264(2) -0.01778(13) 0.55619(12) 0.0365 1.0000 Uani . . . . . . C29 C 0.56311(18) 0.22140(11) 0.50074(9) 0.0215 1.0000 Uani . . . . . . C30 C 0.48251(18) 0.26038(11) 0.46434(10) 0.0255 1.0000 Uani . . . . . . C31 C 0.5027(2) 0.28819(12) 0.40891(11) 0.0292 1.0000 Uani . . . . . . C32 C 0.6047(2) 0.27630(14) 0.38873(11) 0.0353 1.0000 Uani . . . . . . C33 C 0.6876(2) 0.23769(15) 0.42336(12) 0.0409 1.0000 Uani . . . . . . C34 C 0.6655(2) 0.21112(13) 0.47943(11) 0.0328 1.0000 Uani . . . . . . C35 C 0.4134(2) 0.33037(15) 0.37242(13) 0.0452 1.0000 Uani . . . . . . C36 C 0.7995(3) 0.2258(2) 0.40114(16) 0.0766 1.0000 Uani . . . . . . C37 C 0.68344(18) 0.08122(11) 0.58746(10) 0.0233 1.0000 Uani . . . . . . C38 C 0.5933(2) 0.03894(12) 0.54988(11) 0.0295 1.0000 Uani . . . . . . C39 C 0.7471(2) 0.04133(13) 0.64078(12) 0.0349 1.0000 Uani . . . . . . C40 C 0.73532(17) 0.21020(11) 0.64866(10) 0.0246 1.0000 Uani . . . . . . C41 C 0.7192(2) 0.28474(12) 0.63287(13) 0.0361 1.0000 Uani . . . . . . C42 C 0.7537(2) 0.19925(16) 0.71844(11) 0.0407 1.0000 Uani . . . . . . H21 H 0.4368 0.3824 0.6246 0.0343 1.0000 Uiso R . . . . . H41 H 0.6298 0.4140 0.7869 0.0512 1.0000 Uiso R . . . . . H61 H 0.4575 0.2408 0.7588 0.0352 1.0000 Uiso R . . . . . H71 H 0.6159 0.4709 0.6463 0.0804 1.0000 Uiso R . . . . . H72 H 0.5095 0.5040 0.6651 0.0811 1.0000 Uiso R . . . . . H73 H 0.6174 0.5014 0.7115 0.0807 1.0000 Uiso R . . . . . H81 H 0.5727 0.2548 0.8545 0.0885 1.0000 Uiso R . . . . . H82 H 0.5726 0.3274 0.8786 0.0886 1.0000 Uiso R . . . . . H83 H 0.6763 0.2989 0.8517 0.0884 1.0000 Uiso R . . . . . H91 H 0.2216 0.3833 0.6118 0.0461 1.0000 Uiso R . . . . . H101 H 0.0344 0.3690 0.6124 0.1071 1.0000 Uiso R . . . . . H102 H 0.0531 0.3969 0.5463 0.1060 1.0000 Uiso R . . . . . H103 H 0.0263 0.3198 0.5552 0.1065 1.0000 Uiso R . . . . . H111 H 0.2072 0.3088 0.5019 0.0760 1.0000 Uiso R . . . . . H112 H 0.2302 0.3859 0.5072 0.0767 1.0000 Uiso R . . . . . H113 H 0.3209 0.3353 0.5349 0.0766 1.0000 Uiso R . . . . . H121 H 0.2013 0.2429 0.7317 0.0373 1.0000 Uiso R . . . . . H131 H 0.2781 0.3513 0.7435 0.0663 1.0000 Uiso R . . . . . H132 H 0.1716 0.3472 0.7768 0.0668 1.0000 Uiso R . . . . . H133 H 0.1678 0.3838 0.7126 0.0664 1.0000 Uiso R . . . . . H141 H 0.0134 0.2368 0.6691 0.0698 1.0000 Uiso R . . . . . H142 H 0.0186 0.2555 0.7404 0.0698 1.0000 Uiso R . . . . . H143 H 0.0037 0.3145 0.6882 0.0695 1.0000 Uiso R . . . . . H161 H 0.4378 -0.0405 0.6373 0.0302 1.0000 Uiso R . . . . . H181 H 0.6541 -0.0647 0.7925 0.0442 1.0000 Uiso R . . . . . H201 H 0.4877 0.1096 0.7619 0.0346 1.0000 Uiso R . . . . . H211 H 0.6310 -0.1557 0.7178 0.0649 1.0000 Uiso R . . . . . H212 H 0.6286 -0.1238 0.6529 0.0652 1.0000 Uiso R . . . . . H213 H 0.5240 -0.1580 0.6718 0.0652 1.0000 Uiso R . . . . . H221 H 0.6231 0.0229 0.8793 0.0892 1.0000 Uiso R . . . . . H222 H 0.7136 0.0573 0.8493 0.0888 1.0000 Uiso R . . . . . H223 H 0.6055 0.0960 0.8583 0.0883 1.0000 Uiso R . . . . . H231 H 0.2360 0.1205 0.7469 0.0351 1.0000 Uiso R . . . . . H241 H 0.2061 0.0288 0.8081 0.0580 1.0000 Uiso R . . . . . H242 H 0.3003 0.0095 0.7687 0.0576 1.0000 Uiso R . . . . . H243 H 0.1792 -0.0181 0.7491 0.0575 1.0000 Uiso R . . . . . H251 H 0.0253 0.0587 0.7148 0.0668 1.0000 Uiso R . . . . . H252 H 0.0549 0.1166 0.7658 0.0666 1.0000 Uiso R . . . . . H253 H 0.0457 0.1358 0.6949 0.0676 1.0000 Uiso R . . . . . H261 H 0.2327 -0.0401 0.6476 0.0330 1.0000 Uiso R . . . . . H271 H 0.0448 -0.0262 0.6593 0.0594 1.0000 Uiso R . . . . . H272 H 0.0226 0.0139 0.5945 0.0595 1.0000 Uiso R . . . . . H273 H 0.0510 -0.0633 0.5960 0.0601 1.0000 Uiso R . . . . . H281 H 0.1746 0.0084 0.5264 0.0545 1.0000 Uiso R . . . . . H282 H 0.2199 -0.0655 0.5465 0.0551 1.0000 Uiso R . . . . . H283 H 0.3019 -0.0038 0.5548 0.0541 1.0000 Uiso R . . . . . H301 H 0.4131 0.2681 0.4770 0.0304 1.0000 Uiso R . . . . . H321 H 0.6194 0.2944 0.3512 0.0422 1.0000 Uiso R . . . . . H341 H 0.7196 0.1882 0.5028 0.0394 1.0000 Uiso R . . . . . H351 H 0.4407 0.3537 0.3418 0.0683 1.0000 Uiso R . . . . . H352 H 0.3859 0.3621 0.3977 0.0686 1.0000 Uiso R . . . . . H353 H 0.3510 0.3043 0.3558 0.0694 1.0000 Uiso R . . . . . H361 H 0.8567 0.2354 0.4330 0.1149 1.0000 Uiso R . . . . . H362 H 0.8050 0.1796 0.3887 0.1154 1.0000 Uiso R . . . . . H363 H 0.8061 0.2539 0.3670 0.1146 1.0000 Uiso R . . . . . H371 H 0.7366 0.0954 0.5598 0.0274 1.0000 Uiso R . . . . . H381 H 0.5310 0.0317 0.5730 0.0433 1.0000 Uiso R . . . . . H382 H 0.5653 0.0619 0.5121 0.0428 1.0000 Uiso R . . . . . H383 H 0.6228 -0.0043 0.5398 0.0440 1.0000 Uiso R . . . . . H391 H 0.7749 -0.0006 0.6240 0.0520 1.0000 Uiso R . . . . . H392 H 0.6965 0.0296 0.6708 0.0513 1.0000 Uiso R . . . . . H393 H 0.8097 0.0677 0.6598 0.0519 1.0000 Uiso R . . . . . H401 H 0.8019 0.1946 0.6311 0.0295 1.0000 Uiso R . . . . . H411 H 0.7843 0.3098 0.6506 0.0542 1.0000 Uiso R . . . . . H412 H 0.7106 0.2930 0.5905 0.0530 1.0000 Uiso R . . . . . H413 H 0.6551 0.3022 0.6492 0.0534 1.0000 Uiso R . . . . . H421 H 0.6914 0.2161 0.7355 0.0601 1.0000 Uiso R . . . . . H422 H 0.8209 0.2227 0.7367 0.0606 1.0000 Uiso R . . . . . H423 H 0.7616 0.1519 0.7275 0.0608 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 0.01142(9) 0.01720(9) 0.01802(9) -0.00097(7) 0.00090(7) -0.00043(7) Br1 0.01175(10) 0.06252(18) 0.03877(14) -0.01133(12) -0.00168(9) -0.00411(10) Br2 0.02204(11) 0.03841(13) 0.02097(11) -0.00124(9) 0.00016(8) -0.00459(9) Co1 0.01234(13) 0.02453(15) 0.02292(14) -0.00325(11) -0.00073(10) -0.00091(11) P1 0.0143(3) 0.0199(3) 0.0356(3) -0.0037(2) 0.0006(2) 0.0020(2) P2 0.0160(3) 0.0203(3) 0.0233(3) -0.0023(2) 0.0050(2) -0.0026(2) P3 0.0133(2) 0.0217(3) 0.0188(2) 0.0007(2) 0.00134(19) 0.0004(2) N1 0.0140(8) 0.0201(9) 0.0290(9) -0.0050(7) 0.0018(7) -0.0009(7) N2 0.0153(8) 0.0199(9) 0.0248(9) 0.0014(7) 0.0015(7) -0.0022(7) N3 0.0144(8) 0.0225(9) 0.0196(8) 0.0023(7) 0.0023(7) 0.0000(7) C1 0.0125(10) 0.0262(11) 0.0332(12) -0.0114(9) 0.0042(8) 0.0004(8) C2 0.0211(11) 0.0252(12) 0.0417(13) -0.0105(10) 0.0076(10) -0.0020(9) C3 0.0229(12) 0.0292(13) 0.0599(17) -0.0207(12) 0.0141(11) -0.0040(10) C4 0.0209(12) 0.0498(17) 0.0571(18) -0.0327(14) 0.0044(12) -0.0033(11) C5 0.0238(12) 0.0521(17) 0.0397(14) -0.0210(12) 0.0003(10) 0.0050(11) C6 0.0210(11) 0.0328(13) 0.0357(13) -0.0088(10) 0.0017(9) 0.0023(9) C7 0.0415(17) 0.0343(15) 0.090(2) -0.0190(15) 0.0214(16) -0.0155(13) C8 0.0489(19) 0.083(2) 0.0388(16) -0.0206(16) -0.0126(14) 0.0040(17) C9 0.0307(13) 0.0253(13) 0.0582(17) 0.0056(11) -0.0017(12) 0.0054(10) C10 0.0371(18) 0.052(2) 0.120(3) 0.032(2) -0.0100(19) 0.0147(15) C11 0.069(2) 0.0325(15) 0.0485(17) 0.0097(13) -0.0027(15) 0.0054(14) C12 0.0211(11) 0.0322(13) 0.0440(14) -0.0142(11) 0.0097(10) -0.0010(10) C13 0.0274(13) 0.0410(15) 0.0670(19) -0.0288(14) 0.0123(13) -0.0038(11) C14 0.0246(13) 0.0505(17) 0.0676(19) -0.0274(15) 0.0165(13) -0.0080(12) C15 0.0178(10) 0.0234(11) 0.0269(11) 0.0069(9) 0.0048(8) -0.0004(8) C16 0.0202(11) 0.0243(11) 0.0337(12) 0.0050(9) 0.0083(9) -0.0013(9) C17 0.0225(12) 0.0260(12) 0.0502(15) 0.0149(11) 0.0135(11) 0.0007(9) C18 0.0244(12) 0.0407(15) 0.0462(15) 0.0218(12) 0.0052(11) 0.0052(11) C19 0.0270(13) 0.0479(16) 0.0330(13) 0.0093(11) 0.0006(10) 0.0003(11) C20 0.0257(12) 0.0322(13) 0.0300(12) 0.0023(10) 0.0015(9) 0.0018(10) C21 0.0347(15) 0.0264(13) 0.072(2) 0.0124(13) 0.0170(14) 0.0080(11) C22 0.0505(19) 0.077(2) 0.0422(17) -0.0001(16) -0.0180(14) 0.0098(17) C23 0.0321(13) 0.0322(13) 0.0284(12) -0.0017(10) 0.0111(10) -0.0013(10) C24 0.0376(15) 0.0460(16) 0.0340(13) 0.0074(11) 0.0126(11) -0.0006(12) C25 0.0449(16) 0.0519(17) 0.0413(15) 0.0017(13) 0.0228(13) 0.0117(13) C26 0.0254(12) 0.0239(11) 0.0359(12) -0.0050(10) 0.0094(9) -0.0059(9) C27 0.0309(14) 0.0376(14) 0.0535(16) -0.0101(12) 0.0142(12) -0.0165(11) C28 0.0413(15) 0.0322(13) 0.0380(14) -0.0113(11) 0.0130(11) -0.0119(11) C29 0.0215(11) 0.0234(11) 0.0193(10) 0.0015(8) 0.0016(8) -0.0015(8) C30 0.0188(11) 0.0305(12) 0.0272(11) 0.0052(9) 0.0030(9) -0.0012(9) C31 0.0283(12) 0.0295(12) 0.0284(12) 0.0071(9) -0.0018(9) -0.0036(10) C32 0.0393(14) 0.0444(15) 0.0229(12) 0.0117(10) 0.0068(10) 0.0012(12) C33 0.0344(14) 0.0565(17) 0.0349(14) 0.0150(12) 0.0160(11) 0.0110(12) C34 0.0271(12) 0.0447(15) 0.0274(12) 0.0119(10) 0.0063(10) 0.0115(11) C35 0.0343(14) 0.0577(18) 0.0418(15) 0.0255(13) -0.0017(12) 0.0020(13) C36 0.054(2) 0.129(3) 0.056(2) 0.050(2) 0.0384(17) 0.041(2) C37 0.0194(10) 0.0219(11) 0.0303(11) 0.0013(9) 0.0092(9) 0.0019(8) C38 0.0301(12) 0.0277(12) 0.0326(12) -0.0066(10) 0.0113(10) -0.0022(10) C39 0.0226(12) 0.0320(13) 0.0494(15) 0.0111(11) 0.0027(10) 0.0052(10) C40 0.0138(10) 0.0313(12) 0.0287(11) -0.0064(9) 0.0029(8) -0.0028(9) C41 0.0243(12) 0.0300(13) 0.0530(16) -0.0111(11) 0.0020(11) -0.0067(10) C42 0.0273(13) 0.0654(19) 0.0279(13) -0.0084(12) -0.0015(10) -0.0093(12) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.072012(7) 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 . Br2 . 2.6374(3) yes Zr1 . Co1 . 2.7602(3) yes Zr1 . P1 . 2.9186(6) yes Zr1 . P2 . 2.9272(6) yes Zr1 . P3 . 2.6716(5) yes Zr1 . N1 . 2.0893(17) yes Zr1 . N2 . 2.1067(17) yes Zr1 . N3 . 2.1365(17) yes Br1 . Co1 . 2.3603(3) yes Br2 . Co1 . 2.5273(4) yes Co1 . P1 . 2.2807(6) yes Co1 . P2 . 2.2872(6) yes P1 . N1 . 1.6824(18) yes P1 . C9 . 1.850(3) yes P1 . C12 . 1.863(2) yes P2 . N2 . 1.6903(18) yes P2 . C23 . 1.866(2) yes P2 . C26 . 1.852(2) yes P3 . N3 . 1.6723(17) yes P3 . C37 . 1.843(2) yes P3 . C40 . 1.849(2) yes N1 . C1 . 1.427(3) yes N2 . C15 . 1.430(3) yes N3 . C29 . 1.416(3) yes C1 . C2 . 1.392(3) yes C1 . C6 . 1.390(3) yes C2 . C3 . 1.398(3) yes C2 . H21 . 0.953 no C3 . C4 . 1.386(4) yes C3 . C7 . 1.510(4) yes C4 . C5 . 1.383(4) yes C4 . H41 . 0.927 no C5 . C6 . 1.396(3) yes C5 . C8 . 1.507(4) yes C6 . H61 . 0.936 no C7 . H71 . 0.955 no C7 . H72 . 0.958 no C7 . H73 . 0.945 no C8 . H81 . 0.957 no C8 . H82 . 0.963 no C8 . H83 . 0.941 no C9 . C10 . 1.531(4) yes C9 . C11 . 1.510(4) yes C9 . H91 . 0.976 no C10 . H101 . 0.974 no C10 . H102 . 0.963 no C10 . H103 . 0.961 no C11 . H111 . 0.954 no C11 . H112 . 0.951 no C11 . H113 . 0.953 no C12 . C13 . 1.526(3) yes C12 . C14 . 1.538(3) yes C12 . H121 . 0.983 no C13 . H131 . 0.951 no C13 . H132 . 0.958 no C13 . H133 . 0.969 no C14 . H141 . 0.964 no C14 . H142 . 0.992 no C14 . H143 . 0.985 no C15 . C16 . 1.388(3) yes C15 . C20 . 1.396(3) yes C16 . C17 . 1.402(3) yes C16 . H161 . 0.947 no C17 . C18 . 1.381(4) yes C17 . C21 . 1.508(4) yes C18 . C19 . 1.394(4) yes C18 . H181 . 0.927 no C19 . C20 . 1.387(3) yes C19 . C22 . 1.514(4) yes C20 . H201 . 0.932 no C21 . H211 . 0.954 no C21 . H212 . 0.960 no C21 . H213 . 0.936 no C22 . H221 . 0.944 no C22 . H222 . 0.939 no C22 . H223 . 0.950 no C23 . C24 . 1.520(3) yes C23 . C25 . 1.531(4) yes C23 . H231 . 0.983 no C24 . H241 . 0.974 no C24 . H242 . 0.967 no C24 . H243 . 0.967 no C25 . H251 . 0.979 no C25 . H252 . 0.968 no C25 . H253 . 0.979 no C26 . C27 . 1.535(3) yes C26 . C28 . 1.514(3) yes C26 . H261 . 0.978 no C27 . H271 . 0.988 no C27 . H272 . 0.980 no C27 . H273 . 0.956 no C28 . H281 . 0.986 no C28 . H282 . 0.965 no C28 . H283 . 0.954 no C29 . C30 . 1.401(3) yes C29 . C34 . 1.391(3) yes C30 . C31 . 1.385(3) yes C30 . H301 . 0.927 no C31 . C32 . 1.380(3) yes C31 . C35 . 1.503(3) yes C32 . C33 . 1.396(3) yes C32 . H321 . 0.935 no C33 . C34 . 1.395(3) yes C33 . C36 . 1.511(4) yes C34 . H341 . 0.896 no C35 . H351 . 0.911 no C35 . H352 . 0.925 no C35 . H353 . 0.942 no C36 . H361 . 0.933 no C36 . H362 . 0.954 no C36 . H363 . 0.944 no C37 . C38 . 1.521(3) yes C37 . C39 . 1.528(3) yes C37 . H371 . 0.979 no C38 . H381 . 0.971 no C38 . H382 . 0.965 no C38 . H383 . 0.961 no C39 . H391 . 0.983 no C39 . H392 . 0.983 no C39 . H393 . 0.963 no C40 . C41 . 1.516(3) yes C40 . C42 . 1.532(3) yes C40 . H401 . 0.984 no C41 . H411 . 0.964 no C41 . H412 . 0.935 no C41 . H413 . 0.957 no C42 . H421 . 0.943 no C42 . H422 . 0.971 no C42 . H423 . 0.956 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 Br2 . Zr1 . Co1 . 55.783(9) yes Br2 . Zr1 . P1 . 88.140(14) yes Co1 . Zr1 . P1 . 47.257(13) yes Br2 . Zr1 . P2 . 83.492(13) yes Co1 . Zr1 . P2 . 47.314(13) yes P1 . Zr1 . P2 . 78.433(16) yes Br2 . Zr1 . P3 . 121.014(14) yes Co1 . Zr1 . P3 . 172.023(15) yes P1 . Zr1 . P3 . 140.453(17) yes P2 . Zr1 . P3 . 127.043(17) yes Br2 . Zr1 . N1 . 116.54(5) yes Co1 . Zr1 . N1 . 81.41(5) yes P1 . Zr1 . N1 . 34.48(5) yes P2 . Zr1 . N1 . 100.78(5) yes P3 . Zr1 . N1 . 106.11(5) yes Br2 . Zr1 . N2 . 106.06(5) yes Co1 . Zr1 . N2 . 81.93(5) yes P1 . Zr1 . N2 . 105.01(5) yes P2 . Zr1 . N2 . 34.62(5) yes P3 . Zr1 . N2 . 92.60(5) yes Br2 . Zr1 . N3 . 90.60(5) yes Co1 . Zr1 . N3 . 142.96(5) yes P1 . Zr1 . N3 . 126.41(5) yes P2 . Zr1 . N3 . 154.39(5) yes P3 . Zr1 . N3 . 38.73(5) yes N1 . Zr1 . N2 . 111.95(7) yes N1 . Zr1 . N3 . 104.13(7) yes N2 . Zr1 . N3 . 126.53(7) yes Zr1 . Br2 . Co1 . 64.569(9) yes Br2 . Co1 . Br1 . 107.484(13) yes Br2 . Co1 . Zr1 . 59.648(9) yes Br1 . Co1 . Zr1 . 167.092(15) yes Br2 . Co1 . P1 . 107.078(19) yes Br1 . Co1 . P1 . 116.058(19) yes Zr1 . Co1 . P1 . 70.019(16) yes Br2 . Co1 . P2 . 100.745(18) yes Br1 . Co1 . P2 . 115.998(19) yes Zr1 . Co1 . P2 . 70.177(15) yes P1 . Co1 . P2 . 108.02(2) yes Zr1 . P1 . Co1 . 62.724(15) yes Co1 . P1 . N1 . 106.89(6) yes Zr1 . P1 . C9 . 122.04(9) yes Co1 . P1 . C9 . 117.78(9) yes N1 . P1 . C9 . 107.25(11) yes Zr1 . P1 . C12 . 129.03(8) yes Co1 . P1 . C12 . 112.41(8) yes N1 . P1 . C12 . 106.68(10) yes C9 . P1 . C12 . 105.25(12) yes Zr1 . P2 . Co1 . 62.509(15) yes Zr1 . P2 . N2 . 45.08(6) yes Co1 . P2 . N2 . 107.59(6) yes Zr1 . P2 . C23 . 124.25(8) yes Co1 . P2 . C23 . 114.30(8) yes N2 . P2 . C23 . 106.46(10) yes Zr1 . P2 . C26 . 127.36(7) yes Co1 . P2 . C26 . 115.61(8) yes N2 . P2 . C26 . 107.47(10) yes C23 . P2 . C26 . 104.89(11) yes Zr1 . P3 . N3 . 53.06(6) yes Zr1 . P3 . C37 . 121.84(7) yes N3 . P3 . C37 . 110.28(9) yes Zr1 . P3 . C40 . 134.44(7) yes N3 . P3 . C40 . 113.44(10) yes C37 . P3 . C40 . 103.72(10) yes P1 . N1 . Zr1 . 100.85(8) yes P1 . N1 . C1 . 127.21(14) yes Zr1 . N1 . C1 . 131.85(13) yes P2 . N2 . Zr1 . 100.30(8) yes P2 . N2 . C15 . 124.84(14) yes Zr1 . N2 . C15 . 134.71(13) yes P3 . N3 . Zr1 . 88.21(7) yes P3 . N3 . C29 . 130.13(14) yes Zr1 . N3 . C29 . 141.29(14) yes N1 . C1 . C2 . 121.7(2) yes N1 . C1 . C6 . 118.7(2) yes C2 . C1 . C6 . 119.5(2) yes C1 . C2 . C3 . 120.2(2) yes C1 . C2 . H21 . 119.2 no C3 . C2 . H21 . 120.6 no C2 . C3 . C4 . 119.1(2) yes C2 . C3 . C7 . 119.4(3) yes C4 . C3 . C7 . 121.5(2) yes C3 . C4 . C5 . 121.8(2) yes C3 . C4 . H41 . 118.7 no C5 . C4 . H41 . 119.5 no C4 . C5 . C6 . 118.4(3) yes C4 . C5 . C8 . 121.1(3) yes C6 . C5 . C8 . 120.5(3) yes C5 . C6 . C1 . 121.0(2) yes C5 . C6 . H61 . 118.8 no C1 . C6 . H61 . 120.2 no C3 . C7 . H71 . 110.8 no C3 . C7 . H72 . 110.6 no H71 . C7 . H72 . 107.5 no C3 . C7 . H73 . 110.3 no H71 . C7 . H73 . 109.3 no H72 . C7 . H73 . 108.2 no C5 . C8 . H81 . 111.7 no C5 . C8 . H82 . 112.2 no H81 . C8 . H82 . 105.2 no C5 . C8 . H83 . 110.8 no H81 . C8 . H83 . 107.2 no H82 . C8 . H83 . 109.4 no P1 . C9 . C10 . 112.1(2) yes P1 . C9 . C11 . 110.36(18) yes C10 . C9 . C11 . 111.3(3) yes P1 . C9 . H91 . 108.7 no C10 . C9 . H91 . 105.5 no C11 . C9 . H91 . 108.7 no C9 . C10 . H101 . 110.2 no C9 . C10 . H102 . 107.5 no H101 . C10 . H102 . 110.7 no C9 . C10 . H103 . 109.6 no H101 . C10 . H103 . 109.3 no H102 . C10 . H103 . 109.5 no C9 . C11 . H111 . 109.0 no C9 . C11 . H112 . 109.7 no H111 . C11 . H112 . 108.5 no C9 . C11 . H113 . 112.6 no H111 . C11 . H113 . 108.8 no H112 . C11 . H113 . 108.2 no P1 . C12 . C13 . 115.54(19) yes P1 . C12 . C14 . 113.10(18) yes C13 . C12 . C14 . 109.2(2) yes P1 . C12 . H121 . 103.6 no C13 . C12 . H121 . 106.8 no C14 . C12 . H121 . 108.0 no C12 . C13 . H131 . 110.3 no C12 . C13 . H132 . 109.8 no H131 . C13 . H132 . 109.6 no C12 . C13 . H133 . 109.9 no H131 . C13 . H133 . 107.3 no H132 . C13 . H133 . 109.9 no C12 . C14 . H141 . 110.1 no C12 . C14 . H142 . 108.7 no H141 . C14 . H142 . 109.9 no C12 . C14 . H143 . 107.5 no H141 . C14 . H143 . 110.0 no H142 . C14 . H143 . 110.6 no N2 . C15 . C16 . 121.52(19) yes N2 . C15 . C20 . 119.8(2) yes C16 . C15 . C20 . 118.6(2) yes C15 . C16 . C17 . 121.1(2) yes C15 . C16 . H161 . 119.5 no C17 . C16 . H161 . 119.3 no C16 . C17 . C18 . 118.7(2) yes C16 . C17 . C21 . 119.1(2) yes C18 . C17 . C21 . 122.1(2) yes C17 . C18 . C19 . 121.6(2) yes C17 . C18 . H181 . 120.8 no C19 . C18 . H181 . 117.5 no C18 . C19 . C20 . 118.5(2) yes C18 . C19 . C22 . 121.5(2) yes C20 . C19 . C22 . 120.0(3) yes C15 . C20 . C19 . 121.4(2) yes C15 . C20 . H201 . 118.8 no C19 . C20 . H201 . 119.8 no C17 . C21 . H211 . 109.6 no C17 . C21 . H212 . 110.5 no H211 . C21 . H212 . 108.5 no C17 . C21 . H213 . 112.4 no H211 . C21 . H213 . 107.8 no H212 . C21 . H213 . 108.0 no C19 . C22 . H221 . 107.9 no C19 . C22 . H222 . 113.2 no H221 . C22 . H222 . 106.3 no C19 . C22 . H223 . 112.8 no H221 . C22 . H223 . 106.7 no H222 . C22 . H223 . 109.6 no P2 . C23 . C24 . 115.36(17) yes P2 . C23 . C25 . 111.64(17) yes C24 . C23 . C25 . 110.4(2) yes P2 . C23 . H231 . 104.7 no C24 . C23 . H231 . 106.1 no C25 . C23 . H231 . 108.1 no C23 . C24 . H241 . 110.1 no C23 . C24 . H242 . 111.9 no H241 . C24 . H242 . 107.1 no C23 . C24 . H243 . 110.1 no H241 . C24 . H243 . 109.8 no H242 . C24 . H243 . 107.7 no C23 . C25 . H251 . 106.7 no C23 . C25 . H252 . 109.2 no H251 . C25 . H252 . 110.9 no C23 . C25 . H253 . 110.0 no H251 . C25 . H253 . 110.6 no H252 . C25 . H253 . 109.4 no P2 . C26 . C27 . 112.82(17) yes P2 . C26 . C28 . 110.12(16) yes C27 . C26 . C28 . 109.6(2) yes P2 . C26 . H261 . 108.6 no C27 . C26 . H261 . 107.1 no C28 . C26 . H261 . 108.4 no C26 . C27 . H271 . 112.3 no C26 . C27 . H272 . 110.2 no H271 . C27 . H272 . 110.4 no C26 . C27 . H273 . 107.7 no H271 . C27 . H273 . 108.8 no H272 . C27 . H273 . 107.2 no C26 . C28 . H281 . 108.2 no C26 . C28 . H282 . 108.2 no H281 . C28 . H282 . 109.8 no C26 . C28 . H283 . 111.3 no H281 . C28 . H283 . 110.4 no H282 . C28 . H283 . 108.8 no N3 . C29 . C30 . 118.06(19) yes N3 . C29 . C34 . 124.16(19) yes C30 . C29 . C34 . 117.8(2) yes C29 . C30 . C31 . 121.9(2) yes C29 . C30 . H301 . 120.2 no C31 . C30 . H301 . 117.9 no C30 . C31 . C32 . 118.9(2) yes C30 . C31 . C35 . 119.3(2) yes C32 . C31 . C35 . 121.8(2) yes C31 . C32 . C33 . 121.3(2) yes C31 . C32 . H321 . 119.8 no C33 . C32 . H321 . 118.8 no C32 . C33 . C34 . 118.5(2) yes C32 . C33 . C36 . 120.8(2) yes C34 . C33 . C36 . 120.6(2) yes C33 . C34 . C29 . 121.6(2) yes C33 . C34 . H341 . 119.0 no C29 . C34 . H341 . 119.4 no C31 . C35 . H351 . 111.6 no C31 . C35 . H352 . 110.0 no H351 . C35 . H352 . 107.1 no C31 . C35 . H353 . 112.4 no H351 . C35 . H353 . 109.8 no H352 . C35 . H353 . 105.7 no C33 . C36 . H361 . 109.1 no C33 . C36 . H362 . 109.8 no H361 . C36 . H362 . 109.6 no C33 . C36 . H363 . 109.7 no H361 . C36 . H363 . 110.1 no H362 . C36 . H363 . 108.5 no P3 . C37 . C38 . 108.00(15) yes P3 . C37 . C39 . 111.47(16) yes C38 . C37 . C39 . 112.43(19) yes P3 . C37 . H371 . 108.9 no C38 . C37 . H371 . 107.4 no C39 . C37 . H371 . 108.6 no C37 . C38 . H381 . 110.1 no C37 . C38 . H382 . 110.5 no H381 . C38 . H382 . 108.2 no C37 . C38 . H383 . 110.7 no H381 . C38 . H383 . 108.9 no H382 . C38 . H383 . 108.4 no C37 . C39 . H391 . 107.9 no C37 . C39 . H392 . 110.0 no H391 . C39 . H392 . 109.0 no C37 . C39 . H393 . 109.7 no H391 . C39 . H393 . 109.3 no H392 . C39 . H393 . 110.9 no P3 . C40 . C41 . 112.80(15) yes P3 . C40 . C42 . 108.71(16) yes C41 . C40 . C42 . 111.2(2) yes P3 . C40 . H401 . 107.3 no C41 . C40 . H401 . 107.4 no C42 . C40 . H401 . 109.3 no C40 . C41 . H411 . 109.5 no C40 . C41 . H412 . 112.9 no H411 . C41 . H412 . 106.7 no C40 . C41 . H413 . 110.5 no H411 . C41 . H413 . 108.5 no H412 . C41 . H413 . 108.7 no C40 . C42 . H421 . 109.3 no C40 . C42 . H422 . 110.3 no H421 . C42 . H422 . 109.4 no C40 . C42 . H423 . 110.0 no H421 . C42 . H423 . 108.8 no H422 . C42 . H423 . 109.0 no _iucr_refine_instructions_details_constraints ; # # Punched on 15/04/13 at 10:50:50 # #LIST 12 BLOCK SCALE X'S, U'S RIDE C ( 2,X'S) H ( 21,X'S) RIDE C ( 4,X'S) H ( 41,X'S) RIDE C ( 6,X'S) H ( 61,X'S) RIDE C ( 7,X'S) H ( 73,X'S) H ( 72,X'S) H ( 71,X'S) RIDE C ( 8,X'S) H ( 81,X'S) H ( 82,X'S) H ( 83,X'S) RIDE C ( 9,X'S) H ( 91,X'S) RIDE C ( 10,X'S) H ( 102,X'S) H ( 101,X'S) H ( 103,X'S) RIDE C ( 11,X'S) H ( 112,X'S) H ( 113,X'S) H ( 111,X'S) RIDE C ( 12,X'S) H ( 121,X'S) RIDE C ( 13,X'S) H ( 132,X'S) H ( 131,X'S) H ( 133,X'S) RIDE C ( 14,X'S) H ( 142,X'S) H ( 143,X'S) H ( 141,X'S) RIDE C ( 16,X'S) H ( 161,X'S) RIDE C ( 18,X'S) H ( 181,X'S) RIDE C ( 20,X'S) H ( 201,X'S) RIDE C ( 21,X'S) H ( 213,X'S) H ( 211,X'S) H ( 212,X'S) RIDE C ( 22,X'S) H ( 221,X'S) H ( 223,X'S) H ( 222,X'S) RIDE C ( 23,X'S) H ( 231,X'S) RIDE C ( 24,X'S) H ( 241,X'S) H ( 242,X'S) H ( 243,X'S) RIDE C ( 25,X'S) H ( 252,X'S) H ( 253,X'S) H ( 251,X'S) RIDE C ( 26,X'S) H ( 261,X'S) RIDE C ( 27,X'S) H ( 273,X'S) H ( 271,X'S) H ( 272,X'S) RIDE C ( 28,X'S) H ( 282,X'S) H ( 283,X'S) H ( 281,X'S) RIDE C ( 30,X'S) H ( 301,X'S) RIDE C ( 32,X'S) H ( 321,X'S) RIDE C ( 34,X'S) H ( 341,X'S) RIDE C ( 35,X'S) H ( 352,X'S) H ( 351,X'S) H ( 353,X'S) RIDE C ( 36,X'S) H ( 363,X'S) H ( 361,X'S) H ( 362,X'S) RIDE C ( 37,X'S) H ( 371,X'S) RIDE C ( 38,X'S) H ( 383,X'S) H ( 381,X'S) H ( 382,X'S) RIDE C ( 39,X'S) H ( 391,X'S) H ( 393,X'S) H ( 392,X'S) RIDE C ( 40,X'S) H ( 401,X'S) RIDE C ( 41,X'S) H ( 411,X'S) H ( 413,X'S) H ( 412,X'S) RIDE C ( 42,X'S) H ( 422,X'S) H ( 421,X'S) H ( 423,X'S) END ; _iucr_refine_instructions_details_restraints ; # # Punched on 15/04/13 at 10:50:50 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; # 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 -0.012 0.000 0.000 350 79 ' ' 2 -0.110 0.500 0.500 350 79 ' ' _platon_squeeze_details ; During the structure solution, electron density difference maps revealed that there were disordered solvent molecule(s) which could not be successfully modeled. The pentane solvate was highly disordered in a volume PLATON SQUEEZE reported to be 704.8 \%A3 per unit cell (13.6%). It appeared that the cavity area contained ca. tfour pentane molecules, located near a center of symmetry at (0, 0, 0) and (0, 1/2, 1/2). 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. PLATON reported a total electron density of 158 e- per unit cell, likely representing four pentane molecules, consistent with our earlier observations. Use of the SQUEEZE technique resulted in a decrease of ca. 1.3 % in R. ; #===END _database_code_depnum_ccdc_archive 'CCDC 953852'