# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2010
data_global
_journal_coden_Cambridge 182
loop_
_publ_author_name
'Thomas, Christine'
'Napoline, J.'
'Rowe, Gerard'
'Foxman, Bruce'
_publ_contact_author_name 'Thomas, Christine'
_publ_contact_author_email thomasc@brandeis.edu
_publ_section_title
;
Oxidative Addition Across Co/Zr Multiple Bonds in
Early/Late Heterobimetallic Complexes
;
# Attachment '- combined_rev.cif'
data_4
_database_code_depnum_ccdc_archive 'CCDC 776339'
#TrackingRef '- combined_rev.cif'
# start Validation Reply Form: Three Alert B issues
_vrf_PLAT222_4
;
PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 4.04 Ratio
RESPONSE:The 4.04 ratio is between a typical ring H atom and an H atom
attached to methyl group C29, which is slightly disordered. The disorder
was not resolved.
;
_vrf_PLAT232_4
;
PROBLEM: Hirshfeld Test Diff (M-X) I1 -- Co1 .. 19.09 su
Hirshfeld Test Diff (M-X) I2 -- Zr1 .. 10.16 su
RESPONSE:For the Hirshfeld test alerts, the differences are quite small.
Thus we have I-Co at 0.0010(1); I-Zr at 0.0019(1) and Zr-P averaging
0.0012(2). They may reflect a less than adequate absorption correction,
with some difficulty accurately measuring the fragment cut from a larger
crystal.
;
# end Validation Reply Form
_audit_creation_date 09-12-18
_audit_creation_method CRYSTALS_ver_14.01
_oxford_structure_analysis_title 'cmt32_0m in C2/c'
_chemical_name_systematic ?
_chemical_melting_point ?
_cell_length_a 27.2429(12)
_cell_length_b 31.7135(14)
_cell_length_c 16.8195(7)
_cell_angle_alpha 90
_cell_angle_beta 127.715(2)
_cell_angle_gamma 90
_cell_volume 11495.3(9)
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_H-M 'C 1 2/c 1 '
_symmetry_space_group_name_Hall ?
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/2,y+1/2,z
-x+1/2,-y+1/2,-z
-x,y,-z+1/2
x,-y,z+1/2
-x+1/2,y+1/2,-z+1/2
x+1/2,-y+1/2,z+1/2
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Co 0.3494 0.9721 12.2841 4.2791 7.3409 0.2784 4.0034 13.5359 2.3488 71.1692
1.0118 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Zr -2.9673 0.5597 17.8765 1.2762 10.9480 11.9160 5.4173 0.1176 3.6572 87.6627
2.0693 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
I -0.4742 1.8119 20.1472 4.3470 18.9949 0.3814 7.5138 27.7660 2.2735 66.8776
4.0712 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
_cell_formula_units_Z 8
# Given Formula = C45 H75 Co1 I2 N3 P3 Zr1
# Dc = 1.33 Fooo = 4672.00 Mu = 16.56 M = 1154.99
# Found Formula = C45 H75 Co1 I2 N3 P3 Zr1
# Dc = 1.33 FOOO = 4672.00 Mu = 16.56 M = 1154.99
_chemical_formula_sum 'C45 H75 Co1 I2 N3 P3 Zr1'
_chemical_formula_moiety 'C45 H75 Co1 I2 N3 P3 Zr1'
_chemical_compound_source ?
_chemical_formula_weight 1154.99
_cell_measurement_reflns_used 9918
_cell_measurement_theta_min 2
_cell_measurement_theta_max 30
_cell_measurement_temperature 120
_exptl_crystal_description 'acicular fragment'
_exptl_crystal_colour orange
_exptl_crystal_size_min 0.160
_exptl_crystal_size_mid 0.200
_exptl_crystal_size_max 0.473
_exptl_crystal_density_diffrn 1.335
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 4672
_exptl_absorpt_coefficient_mu 1.656
# Sheldrick geometric approximatio 0.72 0.77
_exptl_absorpt_correction_type numerical
_exptl_absorpt_process_details
;
Analytical Absorption (De Meulenaer & Tompa, 1965)
;
_exptl_absorpt_correction_T_min 0.72
_exptl_absorpt_correction_T_max 0.77
_diffrn_measurement_device-type 'Bruker Kappa Apex2'
_diffrn_measurement_device Area
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_measurement_method '\f & \w scans'
# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection 'Apex2 (Bruker AXS, 2006)'
_computing_cell_refinement 'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction 'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material 'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics 'CAMERON (Watkin et al., 1996)'
_diffrn_standards_interval_time .
_diffrn_standards_interval_count .
_diffrn_standards_number 0
_diffrn_standards_decay_% ?
_diffrn_ambient_temperature 120
_diffrn_reflns_number 16791
_reflns_number_total 16791
_diffrn_reflns_av_R_equivalents 0.038
# Number of reflections without Friedels Law is 0
# Number of reflections with Friedels Law is 16791
# Theoretical number of reflections is about 33641
_diffrn_reflns_theta_min 1.142
_diffrn_reflns_theta_max 30.036
_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full 30.036
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_limit_h_min -38
_diffrn_reflns_limit_h_max 30
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_k_max 44
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_limit_l_max 23
_reflns_limit_h_min -38
_reflns_limit_h_max 30
_reflns_limit_k_min 0
_reflns_limit_k_max 44
_reflns_limit_l_min 0
_reflns_limit_l_max 23
_oxford_diffrn_Wilson_B_factor 1.51
_oxford_diffrn_Wilson_scale 67.75
_atom_sites_solution_primary direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_diff_density_min -0.66
_refine_diff_density_max 0.92
# The current dictionary definitions do not cover the
# situation where the reflections used for refinement were
# selected by a user-defined sigma threshold
# The values actually used during refinement
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns 16791
_refine_ls_number_restraints 0
_refine_ls_number_parameters 496
_oxford_refine_ls_R_factor_ref 0.0315
_refine_ls_wR_factor_ref 0.0608
_refine_ls_goodness_of_fit_ref 1.0639
_refine_ls_shift/su_max 0.0050614
_refine_ls_shift/su_mean 0.0001011
# The values computed from all data
_oxford_reflns_number_all 16791
_refine_ls_R_factor_all 0.0315
_refine_ls_wR_factor_all 0.0608
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression I>2.0\s(I)
_reflns_number_gt 13736
_refine_ls_R_factor_gt 0.0228
_refine_ls_wR_factor_gt 0.0515
# choose from: rm (reference molecule of known chirality),
# ad (anomolous dispersion - Flack), rmad (rm and ad),
# syn (from synthesis), unk (unknown) or . (not applicable).
_chemical_absolute_configuration .
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_hydrogen_treatment none # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.02P)^2^ +18.68P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
# Insert your own references if required - in alphabetical order
_publ_section_references
;
Betteridge, P.W., Carruthers, J.R., Cooper, R.I.,
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487.
Bruker Analytical X-ray Systems, Inc., 2006. Apex2,
Version 2 User Manual, M86-E01078, Madison, WI.
De Meulenaer, J. & Tompa, H. (1965). Acta Cryst. 19, 1014.
Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst. 40, 786-790.
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical
Crystallography Laboratory, Oxford, UK.
;
# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3
# Replace last . with number of unfound hydrogen atomsattached to an atom.
# ..._refinement_flags_...
# . no refinement constraints S special position constraint on site
# G rigid group refinement of site R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond) P partial occupancy constraint
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_oxford_atom_site_special_shape
_atom_site_attached_hydrogens
I1 I 0.278017(7) 0.401098(4) 0.070007(10) 0.0246 1.0000 Uani . . . . . . .
I2 I 0.241408(6) 0.524009(4) -0.057307(9) 0.0172 1.0000 Uani . . . . . . .
Zr1 Zr 0.250124(7) 0.564666(5) 0.102945(12) 0.0118 1.0000 Uani . . . . . . .
Co1 Co 0.259465(11) 0.477739(8) 0.093936(18) 0.0146 1.0000 Uani . . . . . . .
P1 P 0.34471(2) 0.503583(15) 0.24185(3) 0.0139 1.0000 Uani . . . . . . .
P2 P 0.16783(2) 0.493313(15) 0.06581(3) 0.0151 1.0000 Uani . . . . . . .
P3 P 0.25249(2) 0.646898(15) 0.13584(4) 0.0158 1.0000 Uani . . . . . . .
N1 N 0.33947(7) 0.55695(5) 0.24339(11) 0.0143 1.0000 Uani . . . . . . .
N2 N 0.16555(7) 0.54655(5) 0.07533(11) 0.0163 1.0000 Uani . . . . . . .
N3 N 0.24337(7) 0.62430(5) 0.03714(11) 0.0151 1.0000 Uani . . . . . . .
C1 C 0.35471(9) 0.48333(6) 0.35422(14) 0.0193 1.0000 Uani . . . . . . .
C2 C 0.41685(10) 0.49318(7) 0.45606(15) 0.0260 1.0000 Uani . . . . . . .
C3 C 0.34065(10) 0.43609(7) 0.34802(16) 0.0263 1.0000 Uani . . . . . . .
C4 C 0.41789(8) 0.49067(6) 0.26122(14) 0.0171 1.0000 Uani . . . . . . .
C5 C 0.44008(9) 0.44506(7) 0.29491(16) 0.0243 1.0000 Uani . . . . . . .
C6 C 0.40985(9) 0.49887(7) 0.16419(14) 0.0203 1.0000 Uani . . . . . . .
C7 C 0.37925(8) 0.58196(6) 0.33351(13) 0.0169 1.0000 Uani . . . . . . .
C8 C 0.43779(9) 0.59642(6) 0.36630(14) 0.0201 1.0000 Uani . . . . . . .
C9 C 0.47460(10) 0.61922(7) 0.45629(16) 0.0273 1.0000 Uani . . . . . . .
C10 C 0.45598(11) 0.62869(7) 0.51415(15) 0.0303 1.0000 Uani . . . . . . .
C11 C 0.39767(11) 0.61494(7) 0.47960(16) 0.0285 1.0000 Uani . . . . . . .
C12 C 0.35876(9) 0.59229(6) 0.39045(14) 0.0217 1.0000 Uani . . . . . . .
C13 C 0.46353(9) 0.59034(7) 0.30924(16) 0.0245 1.0000 Uani . . . . . . .
C14 C 0.49654(13) 0.65447(9) 0.60936(18) 0.0463 1.0000 Uani . . . . . . .
C15 C 0.29626(10) 0.58034(7) 0.35962(16) 0.0271 1.0000 Uani . . . . . . .
C16 C 0.10090(9) 0.47655(6) -0.06346(15) 0.0215 1.0000 Uani . . . . . . .
C17 C 0.03556(9) 0.48576(7) -0.09581(16) 0.0262 1.0000 Uani . . . . . . .
C18 C 0.10413(11) 0.43048(8) -0.08547(19) 0.0365 1.0000 Uani . . . . . . .
C19 C 0.15968(9) 0.46733(6) 0.15594(14) 0.0185 1.0000 Uani . . . . . . .
C20 C 0.09804(9) 0.47342(7) 0.13944(17) 0.0251 1.0000 Uani . . . . . . .
C21 C 0.17493(11) 0.42024(7) 0.16824(18) 0.0289 1.0000 Uani . . . . . . .
C22 C 0.11447(8) 0.57288(6) 0.04867(15) 0.0191 1.0000 Uani . . . . . . .
C23 C 0.10531(9) 0.58423(7) 0.11957(17) 0.0244 1.0000 Uani . . . . . . .
C24 C 0.05726(10) 0.61250(7) 0.0907(2) 0.0332 1.0000 Uani . . . . . . .
C25 C 0.01963(10) 0.63031(7) -0.0039(2) 0.0372 1.0000 Uani . . . . . . .
C26 C 0.02928(10) 0.61887(7) -0.07245(19) 0.0344 1.0000 Uani . . . . . . .
C27 C 0.07497(9) 0.59023(7) -0.04951(16) 0.0255 1.0000 Uani . . . . . . .
C28 C 0.14400(10) 0.56840(7) 0.22574(17) 0.0285 1.0000 Uani . . . . . . .
C29 C -0.02986(12) 0.66223(10) -0.0305(3) 0.0574 1.0000 Uani . . . . . . .
C30 C 0.07986(10) 0.57829(7) -0.13104(16) 0.0311 1.0000 Uani . . . . . . .
C31 C 0.18615(9) 0.67998(6) 0.10104(17) 0.0243 1.0000 Uani . . . . . . .
C32 C 0.18239(12) 0.68300(8) 0.1884(2) 0.0359 1.0000 Uani . . . . . . .
C33 C 0.18211(10) 0.72399(7) 0.05978(19) 0.0335 1.0000 Uani . . . . . . .
C34 C 0.32357(9) 0.67983(6) 0.20721(15) 0.0205 1.0000 Uani . . . . . . .
C35 C 0.32873(9) 0.71374(6) 0.14752(17) 0.0245 1.0000 Uani . . . . . . .
C36 C 0.33520(11) 0.69924(7) 0.30084(16) 0.0294 1.0000 Uani . . . . . . .
C37 C 0.24623(9) 0.64237(6) -0.03885(13) 0.0169 1.0000 Uani . . . . . . .
C38 C 0.30209(10) 0.63966(6) -0.02648(15) 0.0214 1.0000 Uani . . . . . . .
C39 C 0.30510(11) 0.65589(6) -0.10065(18) 0.0278 1.0000 Uani . . . . . . .
C40 C 0.25447(12) 0.67440(7) -0.18759(17) 0.0307 1.0000 Uani . . . . . . .
C41 C 0.20069(11) 0.67730(6) -0.19744(15) 0.0276 1.0000 Uani . . . . . . .
C42 C 0.19497(9) 0.66176(6) -0.12564(14) 0.0216 1.0000 Uani . . . . . . .
C43 C 0.35898(9) 0.62009(7) 0.06467(17) 0.0247 1.0000 Uani . . . . . . .
C44 C 0.25854(16) 0.69002(8) -0.2684(2) 0.0468 1.0000 Uani . . . . . . .
C45 C 0.13295(10) 0.66703(8) -0.14746(17) 0.0331 1.0000 Uani . . . . . . .
H11 H 0.3232 0.4983 0.3538 0.0228 1.0000 Uiso R . . . . . .
H21 H 0.4257 0.5228 0.4606 0.0390 1.0000 Uiso R . . . . . .
H22 H 0.4490 0.4771 0.4627 0.0390 1.0000 Uiso R . . . . . .
H23 H 0.4148 0.4854 0.5092 0.0387 1.0000 Uiso R . . . . . .
H31 H 0.3308 0.4294 0.3920 0.0388 1.0000 Uiso R . . . . . .
H32 H 0.3059 0.4291 0.2802 0.0392 1.0000 Uiso R . . . . . .
H33 H 0.3759 0.4199 0.3667 0.0390 1.0000 Uiso R . . . . . .
H41 H 0.4500 0.5101 0.3137 0.0211 1.0000 Uiso R . . . . . .
H51 H 0.4540 0.4406 0.3629 0.0358 1.0000 Uiso R . . . . . .
H52 H 0.4746 0.4394 0.2949 0.0357 1.0000 Uiso R . . . . . .
H53 H 0.4074 0.4256 0.2501 0.0361 1.0000 Uiso R . . . . . .
H61 H 0.3882 0.5255 0.1347 0.0299 1.0000 Uiso R . . . . . .
H62 H 0.4498 0.5011 0.1786 0.0299 1.0000 Uiso R . . . . . .
H63 H 0.3864 0.4766 0.1167 0.0301 1.0000 Uiso R . . . . . .
H91 H 0.5140 0.6284 0.4799 0.0330 1.0000 Uiso R . . . . . .
H111 H 0.3837 0.6209 0.5166 0.0340 1.0000 Uiso R . . . . . .
H131 H 0.5009 0.5730 0.3468 0.0358 1.0000 Uiso R . . . . . .
H132 H 0.4733 0.6169 0.2954 0.0360 1.0000 Uiso R . . . . . .
H133 H 0.4329 0.5767 0.2455 0.0359 1.0000 Uiso R . . . . . .
H141 H 0.4923 0.6440 0.6587 0.0692 1.0000 Uiso R . . . . . .
H142 H 0.5395 0.6511 0.6359 0.0688 1.0000 Uiso R . . . . . .
H143 H 0.4857 0.6838 0.5955 0.0689 1.0000 Uiso R . . . . . .
H151 H 0.2748 0.6042 0.3591 0.0402 1.0000 Uiso R . . . . . .
H152 H 0.2708 0.5695 0.2932 0.0400 1.0000 Uiso R . . . . . .
H153 H 0.2980 0.5597 0.4030 0.0401 1.0000 Uiso R . . . . . .
H161 H 0.1055 0.4930 -0.1081 0.0259 1.0000 Uiso R . . . . . .
H171 H 0.0061 0.4854 -0.1682 0.0378 1.0000 Uiso R . . . . . .
H172 H 0.0238 0.4651 -0.0688 0.0378 1.0000 Uiso R . . . . . .
H173 H 0.0331 0.5128 -0.0735 0.0375 1.0000 Uiso R . . . . . .
H181 H 0.0984 0.4129 -0.0453 0.0550 1.0000 Uiso R . . . . . .
H182 H 0.0717 0.4239 -0.1553 0.0548 1.0000 Uiso R . . . . . .
H183 H 0.1440 0.4247 -0.0700 0.0550 1.0000 Uiso R . . . . . .
H191 H 0.1916 0.4807 0.2197 0.0218 1.0000 Uiso R . . . . . .
H201 H 0.0832 0.5014 0.1147 0.0366 1.0000 Uiso R . . . . . .
H202 H 0.1050 0.4702 0.2023 0.0367 1.0000 Uiso R . . . . . .
H203 H 0.0679 0.4531 0.0909 0.0371 1.0000 Uiso R . . . . . .
H211 H 0.1392 0.4052 0.1129 0.0427 1.0000 Uiso R . . . . . .
H212 H 0.1849 0.4104 0.2301 0.0431 1.0000 Uiso R . . . . . .
H213 H 0.2093 0.4154 0.1664 0.0430 1.0000 Uiso R . . . . . .
H241 H 0.0505 0.6192 0.1371 0.0398 1.0000 Uiso R . . . . . .
H261 H 0.0045 0.6306 -0.1356 0.0412 1.0000 Uiso R . . . . . .
H281 H 0.1180 0.5555 0.2394 0.0430 1.0000 Uiso R . . . . . .
H282 H 0.1667 0.5912 0.2727 0.0429 1.0000 Uiso R . . . . . .
H283 H 0.1735 0.5477 0.2375 0.0427 1.0000 Uiso R . . . . . .
H291 H -0.0485 0.6536 0.0002 0.0852 1.0000 Uiso R . . . . . .
H292 H -0.0124 0.6894 -0.0077 0.0852 1.0000 Uiso R . . . . . .
H293 H -0.0619 0.6625 -0.1021 0.0850 1.0000 Uiso R . . . . . .
H301 H 0.0588 0.5987 -0.1838 0.0459 1.0000 Uiso R . . . . . .
H302 H 0.1220 0.5774 -0.1059 0.0455 1.0000 Uiso R . . . . . .
H303 H 0.0610 0.5514 -0.1590 0.0456 1.0000 Uiso R . . . . . .
H311 H 0.1489 0.6643 0.0466 0.0301 1.0000 Uiso R . . . . . .
H321 H 0.2133 0.7026 0.2384 0.0528 1.0000 Uiso R . . . . . .
H322 H 0.1428 0.6933 0.1633 0.0531 1.0000 Uiso R . . . . . .
H323 H 0.1886 0.6557 0.2179 0.0528 1.0000 Uiso R . . . . . .
H331 H 0.1422 0.7360 0.0311 0.0492 1.0000 Uiso R . . . . . .
H332 H 0.2133 0.7420 0.1133 0.0489 1.0000 Uiso R . . . . . .
H333 H 0.1886 0.7225 0.0089 0.0489 1.0000 Uiso R . . . . . .
H341 H 0.3576 0.6595 0.2318 0.0253 1.0000 Uiso R . . . . . .
H351 H 0.3700 0.7260 0.1882 0.0369 1.0000 Uiso R . . . . . .
H352 H 0.2988 0.7362 0.1257 0.0373 1.0000 Uiso R . . . . . .
H353 H 0.3224 0.7023 0.0888 0.0372 1.0000 Uiso R . . . . . .
H361 H 0.3768 0.7100 0.3455 0.0438 1.0000 Uiso R . . . . . .
H362 H 0.3288 0.6776 0.3346 0.0439 1.0000 Uiso R . . . . . .
H363 H 0.3066 0.7220 0.2814 0.0439 1.0000 Uiso R . . . . . .
H391 H 0.3426 0.6544 -0.0912 0.0329 1.0000 Uiso R . . . . . .
H411 H 0.1663 0.6898 -0.2548 0.0332 1.0000 Uiso R . . . . . .
H431 H 0.3748 0.6361 0.1234 0.0371 1.0000 Uiso R . . . . . .
H432 H 0.3501 0.5922 0.0762 0.0371 1.0000 Uiso R . . . . . .
H433 H 0.3910 0.6172 0.0578 0.0371 1.0000 Uiso R . . . . . .
H441 H 0.2926 0.7099 -0.2377 0.0730 1.0000 Uiso R . . . . . .
H442 H 0.2207 0.7036 -0.3200 0.0730 1.0000 Uiso R . . . . . .
H443 H 0.2670 0.6666 -0.2947 0.0729 1.0000 Uiso R . . . . . .
H451 H 0.1010 0.6544 -0.2113 0.0489 1.0000 Uiso R . . . . . .
H452 H 0.1324 0.6533 -0.0967 0.0487 1.0000 Uiso R . . . . . .
H453 H 0.1236 0.6964 -0.1495 0.0491 1.0000 Uiso R . . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
I1 0.03442(7) 0.01687(6) 0.03224(7) -0.00006(5) 0.02543(6) 0.00102(5)
I2 0.02104(6) 0.01857(6) 0.01476(5) -0.00062(4) 0.01242(5) -0.00121(4)
Zr1 0.01184(7) 0.01216(8) 0.01219(7) 0.00070(6) 0.00776(6) 0.00015(6)
Co1 0.01581(11) 0.01432(12) 0.01584(11) 0.00008(9) 0.01075(10) -0.00047(9)
P1 0.01348(19) 0.0158(2) 0.0137(2) 0.00260(16) 0.00908(17) 0.00148(16)
P2 0.01363(19) 0.0171(2) 0.0153(2) 0.00119(17) 0.00924(18) -0.00173(16)
P3 0.0166(2) 0.0139(2) 0.0177(2) -0.00049(17) 0.01075(18) 0.00029(17)
N1 0.0137(7) 0.0158(7) 0.0138(7) 0.0005(5) 0.0086(6) 0.0005(5)
N2 0.0138(7) 0.0181(8) 0.0167(7) 0.0022(6) 0.0092(6) 0.0009(6)
N3 0.0166(7) 0.0141(7) 0.0156(7) 0.0017(6) 0.0104(6) 0.0005(6)
C1 0.0217(9) 0.0215(10) 0.0182(9) 0.0049(7) 0.0140(8) 0.0030(7)
C2 0.0312(11) 0.0273(11) 0.0156(9) 0.0054(8) 0.0123(8) 0.0030(9)
C3 0.0333(11) 0.0250(11) 0.0252(10) 0.0041(8) 0.0202(9) -0.0033(8)
C4 0.0143(8) 0.0200(9) 0.0176(8) 0.0048(7) 0.0101(7) 0.0038(7)
C5 0.0218(9) 0.0254(10) 0.0297(10) 0.0083(8) 0.0178(9) 0.0075(8)
C6 0.0164(8) 0.0268(10) 0.0221(9) 0.0042(8) 0.0140(8) 0.0033(7)
C7 0.0171(8) 0.0170(9) 0.0125(8) 0.0019(6) 0.0069(7) 0.0014(7)
C8 0.0172(8) 0.0174(9) 0.0173(9) 0.0034(7) 0.0062(7) 0.0008(7)
C9 0.0207(9) 0.0226(10) 0.0220(10) 0.0015(8) 0.0045(8) -0.0012(8)
C10 0.0350(12) 0.0216(10) 0.0168(9) -0.0001(8) 0.0069(9) 0.0030(9)
C11 0.0376(12) 0.0251(11) 0.0196(10) -0.0005(8) 0.0158(9) 0.0052(9)
C12 0.0256(9) 0.0214(10) 0.0166(9) 0.0024(7) 0.0122(8) 0.0046(8)
C13 0.0192(9) 0.0252(10) 0.0270(10) 0.0028(8) 0.0131(8) -0.0039(8)
C14 0.0496(16) 0.0359(14) 0.0241(12) -0.0100(10) 0.0076(11) -0.0005(12)
C15 0.0318(11) 0.0313(11) 0.0264(10) -0.0013(9) 0.0220(9) 0.0028(9)
C16 0.0171(8) 0.0257(10) 0.0179(9) -0.0027(7) 0.0087(7) -0.0042(7)
C17 0.0163(9) 0.0314(11) 0.0255(10) -0.0038(8) 0.0101(8) -0.0053(8)
C18 0.0298(11) 0.0353(13) 0.0325(12) -0.0139(10) 0.0131(10) -0.0022(10)
C19 0.0192(8) 0.0201(9) 0.0199(9) 0.0026(7) 0.0139(8) -0.0004(7)
C20 0.0236(9) 0.0279(11) 0.0315(11) 0.0043(8) 0.0209(9) -0.0005(8)
C21 0.0393(12) 0.0198(10) 0.0398(12) 0.0058(9) 0.0304(11) 0.0017(9)
C22 0.0127(8) 0.0159(9) 0.0266(10) 0.0015(7) 0.0109(7) -0.0008(6)
C23 0.0194(9) 0.0205(10) 0.0366(11) -0.0023(8) 0.0188(9) -0.0020(7)
C24 0.0244(10) 0.0280(12) 0.0516(15) -0.0088(10) 0.0255(11) -0.0025(9)
C25 0.0169(9) 0.0239(11) 0.0547(15) -0.0050(10) 0.0137(10) 0.0025(8)
C26 0.0160(9) 0.0256(11) 0.0375(13) 0.0018(9) 0.0041(9) 0.0016(8)
C27 0.0165(9) 0.0199(10) 0.0290(10) 0.0023(8) 0.0082(8) -0.0016(7)
C28 0.0330(11) 0.0298(11) 0.0355(12) -0.0020(9) 0.0276(10) 0.0005(9)
C29 0.0282(13) 0.0424(16) 0.077(2) -0.0080(15) 0.0199(14) 0.0140(12)
C30 0.0281(11) 0.0294(12) 0.0211(10) 0.0081(8) 0.0076(9) -0.0012(9)
C31 0.0210(9) 0.0163(9) 0.0375(11) -0.0037(8) 0.0188(9) 0.0000(7)
C32 0.0382(13) 0.0291(12) 0.0585(16) -0.0156(11) 0.0388(13) -0.0071(10)
C33 0.0246(10) 0.0192(10) 0.0474(14) 0.0027(9) 0.0172(10) 0.0053(8)
C34 0.0173(8) 0.0165(9) 0.0214(9) -0.0006(7) 0.0086(8) 0.0000(7)
C35 0.0235(9) 0.0187(9) 0.0336(11) -0.0030(8) 0.0186(9) -0.0042(7)
C36 0.0306(11) 0.0238(11) 0.0236(10) -0.0023(8) 0.0114(9) -0.0025(9)
C37 0.0240(9) 0.0116(8) 0.0159(8) 0.0002(6) 0.0126(7) -0.0014(7)
C38 0.0307(10) 0.0134(9) 0.0267(10) 0.0000(7) 0.0209(9) 0.0000(7)
C39 0.0476(13) 0.0150(9) 0.0405(12) -0.0017(8) 0.0370(11) -0.0014(9)
C40 0.0619(15) 0.0140(9) 0.0303(11) -0.0016(8) 0.0354(12) -0.0020(9)
C41 0.0440(13) 0.0155(9) 0.0163(9) -0.0015(7) 0.0149(9) -0.0031(8)
C42 0.0279(10) 0.0122(8) 0.0179(9) -0.0007(7) 0.0105(8) -0.0020(7)
C43 0.0249(10) 0.0207(10) 0.0354(11) 0.0015(8) 0.0220(9) 0.0011(8)
C44 0.099(2) 0.0242(12) 0.0489(16) 0.0038(11) 0.0618(18) 0.0041(13)
C45 0.0225(10) 0.0311(12) 0.0277(11) 0.0099(9) 0.0062(9) -0.0009(9)
_refine_ls_extinction_method None
_oxford_refine_ls_scale 0.0224655(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
I1 . Co1 . 2.5640(3) yes
I2 . Zr1 . 2.8637(2) yes
I2 . Co1 . 2.7084(3) yes
Zr1 . Co1 . 2.7811(3) yes
Zr1 . P1 . 2.9129(5) yes
Zr1 . P2 . 2.9705(5) yes
Zr1 . P3 . 2.6585(5) yes
Zr1 . N1 . 2.1283(14) yes
Zr1 . N2 . 2.1320(15) yes
Zr1 . N3 . 2.1415(15) yes
Co1 . P1 . 2.2772(5) yes
Co1 . P2 . 2.2923(5) yes
P1 . N1 . 1.7000(16) yes
P1 . C1 . 1.8518(19) yes
P1 . C4 . 1.8584(18) yes
P2 . N2 . 1.7008(17) yes
P2 . C16 . 1.8666(19) yes
P2 . C19 . 1.8541(19) yes
P3 . N3 . 1.6812(16) yes
P3 . C31 . 1.848(2) yes
P3 . C34 . 1.8540(19) yes
N1 . C7 . 1.446(2) yes
N2 . C22 . 1.439(2) yes
N3 . C37 . 1.446(2) yes
C1 . C2 . 1.533(3) yes
C1 . C3 . 1.534(3) yes
C1 . H11 . 0.976 no
C2 . H21 . 0.961 no
C2 . H22 . 0.959 no
C2 . H23 . 0.961 no
C3 . H31 . 0.953 no
C3 . H32 . 0.962 no
C3 . H33 . 0.957 no
C4 . C5 . 1.536(3) yes
C4 . C6 . 1.530(3) yes
C4 . H41 . 0.990 no
C5 . H51 . 0.970 no
C5 . H52 . 0.959 no
C5 . H53 . 0.959 no
C6 . H61 . 0.975 no
C6 . H62 . 0.961 no
C6 . H63 . 0.961 no
C7 . C8 . 1.408(3) yes
C7 . C12 . 1.411(3) yes
C8 . C9 . 1.401(3) yes
C8 . C13 . 1.508(3) yes
C9 . C10 . 1.378(3) yes
C9 . H91 . 0.933 no
C10 . C11 . 1.386(3) yes
C10 . C14 . 1.513(3) yes
C11 . C12 . 1.394(3) yes
C11 . H111 . 0.926 no
C12 . C15 . 1.494(3) yes
C13 . H131 . 0.976 no
C13 . H132 . 0.953 no
C13 . H133 . 0.970 no
C14 . H141 . 0.965 no
C14 . H142 . 0.970 no
C14 . H143 . 0.960 no
C15 . H151 . 0.954 no
C15 . H152 . 0.949 no
C15 . H153 . 0.958 no
C16 . C17 . 1.538(3) yes
C16 . C18 . 1.523(3) yes
C16 . H161 . 0.984 no
C17 . H171 . 0.965 no
C17 . H172 . 0.957 no
C17 . H173 . 0.955 no
C18 . H181 . 0.960 no
C18 . H182 . 0.966 no
C18 . H183 . 0.968 no
C19 . C20 . 1.538(3) yes
C19 . C21 . 1.530(3) yes
C19 . H191 . 0.972 no
C20 . H201 . 0.957 no
C20 . H202 . 0.959 no
C20 . H203 . 0.967 no
C21 . H211 . 0.965 no
C21 . H212 . 0.952 no
C21 . H213 . 0.967 no
C22 . C23 . 1.406(3) yes
C22 . C27 . 1.419(3) yes
C23 . C24 . 1.405(3) yes
C23 . C28 . 1.500(3) yes
C24 . C25 . 1.380(4) yes
C24 . H241 . 0.931 no
C25 . C26 . 1.379(4) yes
C25 . C29 . 1.518(3) yes
C26 . C27 . 1.391(3) yes
C26 . H261 . 0.919 no
C27 . C30 . 1.505(3) yes
C28 . H281 . 0.959 no
C28 . H282 . 0.966 no
C28 . H283 . 0.961 no
C29 . H291 . 0.959 no
C29 . H292 . 0.945 no
C29 . H293 . 0.962 no
C30 . H301 . 0.955 no
C30 . H302 . 0.950 no
C30 . H303 . 0.957 no
C31 . C32 . 1.537(3) yes
C31 . C33 . 1.533(3) yes
C31 . H311 . 0.989 no
C32 . H321 . 0.967 no
C32 . H322 . 0.943 no
C32 . H323 . 0.961 no
C33 . H331 . 0.958 no
C33 . H332 . 0.961 no
C33 . H333 . 0.974 no
C34 . C35 . 1.535(3) yes
C34 . C36 . 1.533(3) yes
C34 . H341 . 0.988 no
C35 . H351 . 0.970 no
C35 . H352 . 0.970 no
C35 . H353 . 0.964 no
C36 . H361 . 0.962 no
C36 . H362 . 0.971 no
C36 . H363 . 0.961 no
C37 . C38 . 1.407(3) yes
C37 . C42 . 1.402(3) yes
C38 . C39 . 1.397(3) yes
C38 . C43 . 1.493(3) yes
C39 . C40 . 1.385(3) yes
C39 . H391 . 0.935 no
C40 . C41 . 1.373(3) yes
C40 . C44 . 1.513(3) yes
C41 . C42 . 1.399(3) yes
C41 . H411 . 0.928 no
C42 . C45 . 1.503(3) yes
C43 . H431 . 0.946 no
C43 . H432 . 0.967 no
C43 . H433 . 0.950 no
C44 . H441 . 0.969 no
C44 . H442 . 0.953 no
C44 . H443 . 0.961 no
C45 . H451 . 0.964 no
C45 . H452 . 0.965 no
C45 . H453 . 0.960 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Zr1 . I2 . Co1 . 59.806(7) yes
I2 . Zr1 . Co1 . 57.322(7) yes
I2 . Zr1 . P1 . 88.786(11) yes
Co1 . Zr1 . P1 . 47.076(11) yes
I2 . Zr1 . P2 . 80.893(11) yes
Co1 . Zr1 . P2 . 46.833(11) yes
P1 . Zr1 . P2 . 81.118(14) yes
I2 . Zr1 . P3 . 127.955(12) yes
Co1 . Zr1 . P3 . 172.896(13) yes
P1 . Zr1 . P3 . 126.049(15) yes
P2 . Zr1 . P3 . 135.248(15) yes
I2 . Zr1 . N1 . 111.90(4) yes
Co1 . Zr1 . N1 . 82.29(4) yes
P1 . Zr1 . N1 . 35.26(4) yes
P2 . Zr1 . N1 . 110.45(4) yes
P3 . Zr1 . N1 . 90.92(4) yes
I2 . Zr1 . N2 . 102.55(4) yes
Co1 . Zr1 . N2 . 81.01(4) yes
P1 . Zr1 . N2 . 107.66(4) yes
P2 . Zr1 . N2 . 34.19(4) yes
P3 . Zr1 . N2 . 101.25(4) yes
I2 . Zr1 . N3 . 88.84(4) yes
Co1 . Zr1 . N3 . 146.00(4) yes
P1 . Zr1 . N3 . 139.11(4) yes
P2 . Zr1 . N3 . 138.49(4) yes
P3 . Zr1 . N3 . 39.17(4) yes
N1 . Zr1 . N2 . 124.10(6) yes
N1 . Zr1 . N3 . 110.70(6) yes
N2 . Zr1 . N3 . 112.68(6) yes
I2 . Co1 . Zr1 . 62.872(8) yes
I2 . Co1 . I1 . 107.827(10) yes
Zr1 . Co1 . I1 . 168.995(11) yes
I2 . Co1 . P1 . 107.999(15) yes
Zr1 . Co1 . P1 . 69.503(14) yes
I1 . Co1 . P1 . 110.212(15) yes
I2 . Co1 . P2 . 98.063(15) yes
Zr1 . Co1 . P2 . 70.930(14) yes
I1 . Co1 . P2 . 117.789(16) yes
P1 . Co1 . P2 . 113.70(2) yes
Zr1 . P1 . Co1 . 63.421(13) yes
Co1 . P1 . N1 . 109.63(5) yes
Zr1 . P1 . C1 . 123.71(6) yes
Co1 . P1 . C1 . 113.90(6) yes
N1 . P1 . C1 . 106.92(8) yes
Zr1 . P1 . C4 . 127.95(6) yes
Co1 . P1 . C4 . 112.33(6) yes
N1 . P1 . C4 . 107.93(8) yes
C1 . P1 . C4 . 105.80(8) yes
Zr1 . P2 . Co1 . 62.237(13) yes
Co1 . P2 . N2 . 107.00(5) yes
Zr1 . P2 . C16 . 122.39(7) yes
Co1 . P2 . C16 . 110.09(7) yes
N2 . P2 . C16 . 109.06(8) yes
Zr1 . P2 . C19 . 128.24(6) yes
Co1 . P2 . C19 . 113.29(6) yes
N2 . P2 . C19 . 109.55(8) yes
C16 . P2 . C19 . 107.79(9) yes
Zr1 . P3 . N3 . 53.57(5) yes
Zr1 . P3 . C31 . 126.61(7) yes
N3 . P3 . C31 . 113.83(9) yes
Zr1 . P3 . C34 . 124.76(6) yes
N3 . P3 . C34 . 110.15(8) yes
C31 . P3 . C34 . 108.48(9) yes
P1 . N1 . Zr1 . 98.47(7) yes
P1 . N1 . C7 . 123.09(12) yes
Zr1 . N1 . C7 . 135.66(12) yes
P2 . N2 . Zr1 . 101.02(7) yes
P2 . N2 . C22 . 129.10(13) yes
Zr1 . N2 . C22 . 128.45(12) yes
P3 . N3 . Zr1 . 87.25(6) yes
P3 . N3 . C37 . 130.44(13) yes
Zr1 . N3 . C37 . 140.62(12) yes
P1 . C1 . C2 . 116.24(14) yes
P1 . C1 . C3 . 113.24(14) yes
C2 . C1 . C3 . 109.53(16) yes
P1 . C1 . H11 . 104.2 no
C2 . C1 . H11 . 105.9 no
C3 . C1 . H11 . 107.0 no
C1 . C2 . H21 . 109.9 no
C1 . C2 . H22 . 109.2 no
H21 . C2 . H22 . 110.1 no
C1 . C2 . H23 . 109.5 no
H21 . C2 . H23 . 109.4 no
H22 . C2 . H23 . 108.8 no
C1 . C3 . H31 . 109.9 no
C1 . C3 . H32 . 109.2 no
H31 . C3 . H32 . 109.3 no
C1 . C3 . H33 . 110.0 no
H31 . C3 . H33 . 109.3 no
H32 . C3 . H33 . 109.2 no
P1 . C4 . C5 . 114.21(13) yes
P1 . C4 . C6 . 109.71(12) yes
C5 . C4 . C6 . 108.70(16) yes
P1 . C4 . H41 . 106.7 no
C5 . C4 . H41 . 108.9 no
C6 . C4 . H41 . 108.4 no
C4 . C5 . H51 . 110.7 no
C4 . C5 . H52 . 110.0 no
H51 . C5 . H52 . 107.3 no
C4 . C5 . H53 . 110.5 no
H51 . C5 . H53 . 109.8 no
H52 . C5 . H53 . 108.5 no
C4 . C6 . H61 . 109.8 no
C4 . C6 . H62 . 110.0 no
H61 . C6 . H62 . 107.6 no
C4 . C6 . H63 . 110.5 no
H61 . C6 . H63 . 109.2 no
H62 . C6 . H63 . 109.8 no
N1 . C7 . C8 . 122.16(16) yes
N1 . C7 . C12 . 119.00(16) yes
C8 . C7 . C12 . 118.84(17) yes
C7 . C8 . C9 . 118.82(19) yes
C7 . C8 . C13 . 124.44(17) yes
C9 . C8 . C13 . 116.72(18) yes
C8 . C9 . C10 . 123.1(2) yes
C8 . C9 . H91 . 119.8 no
C10 . C9 . H91 . 117.0 no
C9 . C10 . C11 . 117.25(19) yes
C9 . C10 . C14 . 121.3(2) yes
C11 . C10 . C14 . 121.4(2) yes
C10 . C11 . C12 . 122.4(2) yes
C10 . C11 . H111 . 119.4 no
C12 . C11 . H111 . 118.2 no
C7 . C12 . C11 . 119.57(19) yes
C7 . C12 . C15 . 123.08(18) yes
C11 . C12 . C15 . 117.35(19) yes
C8 . C13 . H131 . 111.5 no
C8 . C13 . H132 . 110.5 no
H131 . C13 . H132 . 108.7 no
C8 . C13 . H133 . 109.9 no
H131 . C13 . H133 . 108.4 no
H132 . C13 . H133 . 107.8 no
C10 . C14 . H141 . 109.2 no
C10 . C14 . H142 . 108.8 no
H141 . C14 . H142 . 108.2 no
C10 . C14 . H143 . 110.5 no
H141 . C14 . H143 . 111.2 no
H142 . C14 . H143 . 108.9 no
C12 . C15 . H151 . 111.4 no
C12 . C15 . H152 . 110.9 no
H151 . C15 . H152 . 106.0 no
C12 . C15 . H153 . 113.2 no
H151 . C15 . H153 . 107.0 no
H152 . C15 . H153 . 108.0 no
P2 . C16 . C17 . 116.90(14) yes
P2 . C16 . C18 . 113.31(15) yes
C17 . C16 . C18 . 108.83(17) yes
P2 . C16 . H161 . 104.3 no
C17 . C16 . H161 . 106.8 no
C18 . C16 . H161 . 105.7 no
C16 . C17 . H171 . 109.4 no
C16 . C17 . H172 . 110.6 no
H171 . C17 . H172 . 109.2 no
C16 . C17 . H173 . 112.2 no
H171 . C17 . H173 . 107.7 no
H172 . C17 . H173 . 107.8 no
C16 . C18 . H181 . 109.2 no
C16 . C18 . H182 . 110.8 no
H181 . C18 . H182 . 108.0 no
C16 . C18 . H183 . 109.8 no
H181 . C18 . H183 . 109.9 no
H182 . C18 . H183 . 109.2 no
P2 . C19 . C20 . 117.42(14) yes
P2 . C19 . C21 . 112.70(14) yes
C20 . C19 . C21 . 108.85(16) yes
P2 . C19 . H191 . 103.6 no
C20 . C19 . H191 . 106.7 no
C21 . C19 . H191 . 106.8 no
C19 . C20 . H201 . 108.5 no
C19 . C20 . H202 . 109.3 no
H201 . C20 . H202 . 109.0 no
C19 . C20 . H203 . 109.8 no
H201 . C20 . H203 . 109.5 no
H202 . C20 . H203 . 110.7 no
C19 . C21 . H211 . 108.8 no
C19 . C21 . H212 . 109.8 no
H211 . C21 . H212 . 109.6 no
C19 . C21 . H213 . 109.8 no
H211 . C21 . H213 . 108.3 no
H212 . C21 . H213 . 110.4 no
N2 . C22 . C23 . 121.58(17) yes
N2 . C22 . C27 . 119.20(18) yes
C23 . C22 . C27 . 119.07(18) yes
C22 . C23 . C24 . 118.7(2) yes
C22 . C23 . C28 . 124.33(18) yes
C24 . C23 . C28 . 116.9(2) yes
C23 . C24 . C25 . 122.5(2) yes
C23 . C24 . H241 . 118.5 no
C25 . C24 . H241 . 119.0 no
C24 . C25 . C26 . 118.0(2) yes
C24 . C25 . C29 . 120.8(3) yes
C26 . C25 . C29 . 121.2(3) yes
C25 . C26 . C27 . 122.4(2) yes
C25 . C26 . H261 . 118.6 no
C27 . C26 . H261 . 119.0 no
C22 . C27 . C26 . 119.3(2) yes
C22 . C27 . C30 . 122.41(19) yes
C26 . C27 . C30 . 118.3(2) yes
C23 . C28 . H281 . 110.1 no
C23 . C28 . H282 . 110.8 no
H281 . C28 . H282 . 108.7 no
C23 . C28 . H283 . 111.4 no
H281 . C28 . H283 . 107.8 no
H282 . C28 . H283 . 107.9 no
C25 . C29 . H291 . 108.5 no
C25 . C29 . H292 . 110.7 no
H291 . C29 . H292 . 110.0 no
C25 . C29 . H293 . 109.6 no
H291 . C29 . H293 . 107.6 no
H292 . C29 . H293 . 110.2 no
C27 . C30 . H301 . 109.8 no
C27 . C30 . H302 . 111.0 no
H301 . C30 . H302 . 108.0 no
C27 . C30 . H303 . 110.5 no
H301 . C30 . H303 . 108.1 no
H302 . C30 . H303 . 109.4 no
P3 . C31 . C32 . 110.91(16) yes
P3 . C31 . C33 . 116.48(15) yes
C32 . C31 . C33 . 110.35(18) yes
P3 . C31 . H311 . 104.9 no
C32 . C31 . H311 . 106.6 no
C33 . C31 . H311 . 106.9 no
C31 . C32 . H321 . 109.9 no
C31 . C32 . H322 . 108.7 no
H321 . C32 . H322 . 108.4 no
C31 . C32 . H323 . 110.2 no
H321 . C32 . H323 . 110.2 no
H322 . C32 . H323 . 109.4 no
C31 . C33 . H331 . 109.6 no
C31 . C33 . H332 . 109.9 no
H331 . C33 . H332 . 108.4 no
C31 . C33 . H333 . 110.6 no
H331 . C33 . H333 . 109.6 no
H332 . C33 . H333 . 108.6 no
P3 . C34 . C35 . 116.64(14) yes
P3 . C34 . C36 . 111.65(14) yes
C35 . C34 . C36 . 110.28(17) yes
P3 . C34 . H341 . 104.2 no
C35 . C34 . H341 . 107.0 no
C36 . C34 . H341 . 106.2 no
C34 . C35 . H351 . 110.4 no
C34 . C35 . H352 . 111.8 no
H351 . C35 . H352 . 108.3 no
C34 . C35 . H353 . 112.1 no
H351 . C35 . H353 . 106.1 no
H352 . C35 . H353 . 107.9 no
C34 . C36 . H361 . 110.4 no
C34 . C36 . H362 . 108.6 no
H361 . C36 . H362 . 110.0 no
C34 . C36 . H363 . 109.7 no
H361 . C36 . H363 . 108.8 no
H362 . C36 . H363 . 109.3 no
N3 . C37 . C38 . 118.92(16) yes
N3 . C37 . C42 . 122.44(17) yes
C38 . C37 . C42 . 118.63(17) yes
C37 . C38 . C39 . 119.62(19) yes
C37 . C38 . C43 . 121.77(17) yes
C39 . C38 . C43 . 118.61(19) yes
C38 . C39 . C40 . 122.3(2) yes
C38 . C39 . H391 . 118.9 no
C40 . C39 . H391 . 118.8 no
C39 . C40 . C41 . 117.12(19) yes
C39 . C40 . C44 . 121.0(2) yes
C41 . C40 . C44 . 121.9(2) yes
C40 . C41 . C42 . 123.1(2) yes
C40 . C41 . H411 . 118.6 no
C42 . C41 . H411 . 118.2 no
C37 . C42 . C41 . 119.2(2) yes
C37 . C42 . C45 . 123.92(18) yes
C41 . C42 . C45 . 116.90(19) yes
C38 . C43 . H431 . 111.9 no
C38 . C43 . H432 . 110.8 no
H431 . C43 . H432 . 106.8 no
C38 . C43 . H433 . 111.6 no
H431 . C43 . H433 . 108.1 no
H432 . C43 . H433 . 107.4 no
C40 . C44 . H441 . 107.8 no
C40 . C44 . H442 . 109.5 no
H441 . C44 . H442 . 109.8 no
C40 . C44 . H443 . 109.3 no
H441 . C44 . H443 . 109.1 no
H442 . C44 . H443 . 111.2 no
C42 . C45 . H451 . 109.8 no
C42 . C45 . H452 . 110.9 no
H451 . C45 . H452 . 107.9 no
C42 . C45 . H453 . 110.6 no
H451 . C45 . H453 . 109.0 no
H452 . C45 . H453 . 108.7 no
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.025 0.250 0.165 1279 268 ' '
2 -0.010 0.750 0.232 1279 268 ' '
_platon_squeeze_details
;During the structure solution, electron density difference
maps revealed that there were considerable disordered
solvent molecules (from history, likely pentane) in a
volume of 2562.8 \%A3 per unit cell (22.3%); the peaks
could not be modeled successfully. Areas of continuous
electron density appeared in the ac plane (in the
n-glide planes), creating bilayer arrangements at
b = 1/4 and 3/4.Attempts at modeling the disordered
pentane using restraints was unsuccessful, as was
step by step acquisition of peaks using successive
electron density difference maps. Thus, the structure
factors were modified using the PLATON SQUEEZE technique,
in order to produce a ?solvate-free? structure factor set.
PLATON reported a total electron density of 536 e- per
unit cell, likely representing twelve pentane molecules.
Use of the SQUEEZE technique resulted in a decrease of
ca. 1.6 % in R.
;
#===END
data_5
_database_code_depnum_ccdc_archive 'CCDC 776340'
#TrackingRef '- combined_rev.cif'
_audit_creation_date 09-12-18
_audit_creation_method CRYSTALS_ver_14.01
_oxford_structure_analysis_title 'cmt31_0m in P-1'
_chemical_name_systematic ?
_chemical_melting_point ?
_cell_length_a 10.0365(4)
_cell_length_b 15.6058(7)
_cell_length_c 18.1449(8)
_cell_angle_alpha 83.098(2)
_cell_angle_beta 74.691(2)
_cell_angle_gamma 85.221(2)
_cell_volume 2717.3(2)
_symmetry_cell_setting Triclinic
_symmetry_space_group_name_H-M 'P -1 '
_symmetry_space_group_name_Hall ?
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Co 0.3494 0.9721 12.2841 4.2791 7.3409 0.2784 4.0034 13.5359 2.3488 71.1692
1.0118 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Zr -2.9673 0.5597 17.8765 1.2762 10.9480 11.9160 5.4173 0.1176 3.6572 87.6627
2.0693 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
I -0.4742 1.8119 20.1472 4.3470 18.9949 0.3814 7.5138 27.7660 2.2735 66.8776
4.0712 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
_cell_formula_units_Z 2
# Given Formula = C51.97 H83.95 Co1 I1.03 N3 P3 Zr1
# Dc = 1.37 Fooo = 1166.70 Mu = 12.06 M = 1124.68
# Found Formula = C51.97 H83.91 Co1 I1.03 N3 P3 Zr1
# Dc = 1.37 FOOO = 1166.70 Mu = 12.06 M = 1124.67
_chemical_formula_sum 'C51.97 H83.91 Co1 I1.03 N3 P3 Zr1'
_chemical_formula_moiety 'C51.97 H83.91 Co1 I1.03 N3 P3 Zr1'
_chemical_compound_source ?
_chemical_formula_weight 1124.67
_cell_measurement_reflns_used 9314
_cell_measurement_theta_min 3
_cell_measurement_theta_max 30
_cell_measurement_temperature 120
_exptl_crystal_description 'prism fragment'
_exptl_crystal_colour green
_exptl_crystal_size_min 0.348
_exptl_crystal_size_mid 0.391
_exptl_crystal_size_max 0.610
_exptl_crystal_density_diffrn 1.374
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 1166.702
_exptl_absorpt_coefficient_mu 1.206
# Sheldrick geometric approximatio 0.62 0.66
_exptl_absorpt_correction_type numerical
_exptl_absorpt_process_details
;
Analytical Absorption (De Meulenaer & Tompa, 1965)
;
_exptl_absorpt_correction_T_min 0.62
_exptl_absorpt_correction_T_max 0.66
_diffrn_measurement_device-type 'Bruker Kappa Apex2'
_diffrn_measurement_device Area
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_measurement_method '\f & \w scans'
# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection 'Apex2 (Bruker AXS, 2006)'
_computing_cell_refinement 'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction 'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material 'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics 'CAMERON (Watkin et al., 1996)'
_diffrn_standards_interval_time .
_diffrn_standards_interval_count .
_diffrn_standards_number 0
_diffrn_standards_decay_% ?
_diffrn_ambient_temperature 120
_diffrn_reflns_number 82444
_reflns_number_total 15766
_diffrn_reflns_av_R_equivalents 0.019
# Number of reflections without Friedels Law is 0
# Number of reflections with Friedels Law is 15766
# Theoretical number of reflections is about 31688
_diffrn_reflns_theta_min 2.107
_diffrn_reflns_theta_max 29.994
_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full 29.994
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_k_min -21
_diffrn_reflns_limit_k_max 21
_diffrn_reflns_limit_l_min -25
_diffrn_reflns_limit_l_max 25
_reflns_limit_h_min -13
_reflns_limit_h_max 14
_reflns_limit_k_min -21
_reflns_limit_k_max 21
_reflns_limit_l_min 0
_reflns_limit_l_max 25
_oxford_diffrn_Wilson_B_factor 1.35
_oxford_diffrn_Wilson_scale 62.19
_atom_sites_solution_primary direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_diff_density_min -0.71
_refine_diff_density_max 0.77
# The current dictionary definitions do not cover the
# situation where the reflections used for refinement were
# selected by a user-defined sigma threshold
# The values actually used during refinement
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns 15766
_refine_ls_number_restraints 0
_refine_ls_number_parameters 567
_oxford_refine_ls_R_factor_ref 0.0196
_refine_ls_wR_factor_ref 0.0480
_refine_ls_goodness_of_fit_ref 1.0161
_refine_ls_shift/su_max 0.0032166
_refine_ls_shift/su_mean 0.0000755
# The values computed from all data
_oxford_reflns_number_all 15766
_refine_ls_R_factor_all 0.0196
_refine_ls_wR_factor_all 0.0480
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression I>2.0\s(I)
_reflns_number_gt 15133
_refine_ls_R_factor_gt 0.0185
_refine_ls_wR_factor_gt 0.0454
# choose from: rm (reference molecule of known chirality),
# ad (anomolous dispersion - Flack), rmad (rm and ad),
# syn (from synthesis), unk (unknown) or . (not applicable).
_chemical_absolute_configuration .
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_hydrogen_treatment none # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.02P)^2^ + 1.44P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
# Insert your own references if required - in alphabetical order
_publ_section_references
;
Betteridge, P.W., Carruthers, J.R., Cooper, R.I.,
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487.
Bruker Analytical X-ray Systems, Inc., 2006. Apex2,
Version 2 User Manual, M86-E01078, Madison, WI.
De Meulenaer, J. & Tompa, H. (1965). Acta Cryst. 19, 1014.
Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst. 40, 786-790.
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical
Crystallography Laboratory, Oxford, UK.
;
# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3
# Replace last . with number of unfound hydrogen atomsattached to an atom.
# ..._refinement_flags_...
# . no refinement constraints S special position constraint on site
# G rigid group refinement of site R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond) P partial occupancy constraint
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_oxford_atom_site_special_shape
_atom_site_attached_hydrogens
I1 I 0.549215(8) 0.241985(6) 0.479152(4) 0.0239 1.0000 Uani . . . . . . .
I2 I 0.5713(4) 0.2053(2) 0.2548(2) 0.0210(11) 0.0307(7) Uiso . . P 1 2 . .
Zr1 Zr 0.302620(9) 0.258160(6) 0.261524(5) 0.0103 1.0000 Uani . . . . . . .
Co1 Co 0.399145(14) 0.253878(9) 0.382409(8) 0.0132 1.0000 Uani . . . . . . .
P1 P 0.32770(3) 0.392461(17) 0.353598(15) 0.0123 1.0000 Uani . . . . . . .
P2 P 0.21955(3) 0.162899(18) 0.408227(15) 0.0140 1.0000 Uani . . . . . . .
P3 P 0.22117(3) 0.273139(19) 0.129921(16) 0.0156 1.0000 Uani . . . . . . .
N1 N 0.24888(9) 0.39174(6) 0.28188(5) 0.0123 1.0000 Uani . . . . . . .
N2 N 0.18330(9) 0.15381(6) 0.32316(5) 0.0143 1.0000 Uani . . . . . . .
N3 N 0.37793(9) 0.23831(6) 0.14238(5) 0.0148 1.0000 Uani . . . . . . .
C1 C 0.46938(11) 0.46885(7) 0.32093(6) 0.0174 1.0000 Uani . . . . . . .
C2 C 0.52125(13) 0.49775(9) 0.38598(7) 0.0237 1.0000 Uani . . . . . . .
C3 C 0.59258(12) 0.42730(9) 0.26478(7) 0.0229 1.0000 Uani . . . . . . .
C4 C 0.20318(11) 0.44048(7) 0.43556(6) 0.0153 1.0000 Uani . . . . . . .
C5 C 0.24781(12) 0.42518(8) 0.51122(6) 0.0197 1.0000 Uani . . . . . . .
C6 C 0.16182(12) 0.53652(7) 0.41916(7) 0.0194 1.0000 Uani . . . . . . .
C7 C 0.16731(11) 0.46256(7) 0.25444(6) 0.0136 1.0000 Uani . . . . . . .
C8 C 0.02303(11) 0.47091(7) 0.28671(6) 0.0152 1.0000 Uani . . . . . . .
C9 C -0.05518(12) 0.53974(7) 0.25955(7) 0.0201 1.0000 Uani . . . . . . .
C10 C 0.00339(13) 0.60107(8) 0.20043(8) 0.0230 1.0000 Uani . . . . . . .
C11 C 0.14447(13) 0.59138(7) 0.16838(7) 0.0211 1.0000 Uani . . . . . . .
C12 C 0.22752(11) 0.52439(7) 0.19413(6) 0.0162 1.0000 Uani . . . . . . .
C13 C 0.37944(12) 0.52280(8) 0.15438(7) 0.0203 1.0000 Uani . . . . . . .
C14 C -0.08313(16) 0.67537(10) 0.17273(10) 0.0384 1.0000 Uani . . . . . . .
C15 C -0.05248(11) 0.41122(7) 0.35293(7) 0.0180 1.0000 Uani . . . . . . .
C16 C 0.05397(12) 0.19681(7) 0.47467(6) 0.0185 1.0000 Uani . . . . . . .
C17 C 0.06940(15) 0.23194(9) 0.54733(7) 0.0273 1.0000 Uani . . . . . . .
C18 C -0.05657(12) 0.12981(8) 0.49435(7) 0.0231 1.0000 Uani . . . . . . .
C19 C 0.27362(12) 0.05544(7) 0.44977(7) 0.0190 1.0000 Uani . . . . . . .
C20 C 0.25126(13) 0.04842(9) 0.53714(7) 0.0256 1.0000 Uani . . . . . . .
C21 C 0.42687(12) 0.03199(8) 0.41356(7) 0.0229 1.0000 Uani . . . . . . .
C22 C 0.09188(11) 0.09674(7) 0.30591(6) 0.0157 1.0000 Uani . . . . . . .
C23 C 0.13078(12) 0.00960(7) 0.29340(6) 0.0186 1.0000 Uani . . . . . . .
C24 C 0.03930(14) -0.04042(8) 0.27288(7) 0.0241 1.0000 Uani . . . . . . .
C25 C -0.08819(14) -0.00854(9) 0.26340(8) 0.0265 1.0000 Uani . . . . . . .
C26 C -0.12448(12) 0.07765(9) 0.27460(7) 0.0243 1.0000 Uani . . . . . . .
C27 C -0.03811(11) 0.13038(7) 0.29544(7) 0.0183 1.0000 Uani . . . . . . .
C28 C 0.26721(13) -0.03478(8) 0.29875(7) 0.0229 1.0000 Uani . . . . . . .
C29 C -0.18526(17) -0.06388(11) 0.24184(11) 0.0430 1.0000 Uani . . . . . . .
C30 C -0.08795(12) 0.22231(8) 0.30722(7) 0.0208 1.0000 Uani . . . . . . .
C31 C 0.14089(13) 0.18916(8) 0.09452(7) 0.0231 1.0000 Uani . . . . . . .
C32 C -0.01168(15) 0.21360(11) 0.09865(9) 0.0340 1.0000 Uani . . . . . . .
C33 C 0.21493(17) 0.16121(10) 0.01477(8) 0.0324 1.0000 Uani . . . . . . .
C34 C 0.23540(13) 0.37206(8) 0.06148(7) 0.0204 1.0000 Uani . . . . . . .
C35 C 0.09501(15) 0.42122(9) 0.06685(9) 0.0309 1.0000 Uani . . . . . . .
C36 C 0.31355(16) 0.36399(9) -0.02251(7) 0.0290 1.0000 Uani . . . . . . .
C37 C 0.49836(11) 0.20362(7) 0.09041(6) 0.0156 1.0000 Uani . . . . . . .
C38 C 0.60664(11) 0.25669(7) 0.05040(6) 0.0165 1.0000 Uani . . . . . . .
C39 C 0.72445(12) 0.22052(8) 0.00211(6) 0.0185 1.0000 Uani . . . . . . .
C40 C 0.74110(12) 0.13315(8) -0.00778(7) 0.0212 1.0000 Uani . . . . . . .
C41 C 0.63583(13) 0.08132(8) 0.03412(7) 0.0232 1.0000 Uani . . . . . . .
C42 C 0.51579(13) 0.11432(7) 0.08326(6) 0.0201 1.0000 Uani . . . . . . .
C43 C 0.60235(13) 0.35104(8) 0.06068(7) 0.0220 1.0000 Uani . . . . . . .
C44 C 0.86979(14) 0.09611(9) -0.06068(8) 0.0308 1.0000 Uani . . . . . . .
C45 C 0.41224(15) 0.05154(8) 0.12911(8) 0.0305 1.0000 Uani . . . . . . .
C46 C 0.5258(2) 0.20883(9) 0.26948(9) 0.0183 0.9693(7) Uani . . P 1 1 . .
C47 C 0.33261(17) 0.76110(9) 0.19261(8) 0.0309 1.0000 Uani . . . . . . .
C48 C 0.30333(18) 0.72829(9) 0.26944(8) 0.0340 1.0000 Uani . . . . . . .
C49 C 0.39894(19) 0.73243(10) 0.31110(9) 0.0380 1.0000 Uani . . . . . . .
C50 C 0.52385(19) 0.76908(11) 0.27603(11) 0.0430 1.0000 Uani . . . . . . .
C51 C 0.55329(17) 0.80125(11) 0.19930(10) 0.0404 1.0000 Uani . . . . . . .
C52 C 0.45710(16) 0.79725(9) 0.15758(8) 0.0321 1.0000 Uani . . . . . . .
H11 H 0.4327 0.5189 0.2952 0.0210 1.0000 Uiso R . . . . . .
H21 H 0.4531 0.5336 0.4183 0.0349 1.0000 Uiso R . . . . . .
H22 H 0.5464 0.4490 0.4170 0.0352 1.0000 Uiso R . . . . . .
H23 H 0.6036 0.5309 0.3635 0.0367 1.0000 Uiso R . . . . . .
H31 H 0.6567 0.4703 0.2389 0.0356 1.0000 Uiso R . . . . . .
H32 H 0.6402 0.3824 0.2920 0.0339 1.0000 Uiso R . . . . . .
H33 H 0.5638 0.4023 0.2263 0.0333 1.0000 Uiso R . . . . . .
H41 H 0.1221 0.4072 0.4425 0.0187 1.0000 Uiso R . . . . . .
H51 H 0.1658 0.4246 0.5547 0.0300 1.0000 Uiso R . . . . . .
H52 H 0.3031 0.4712 0.5158 0.0302 1.0000 Uiso R . . . . . .
H53 H 0.2991 0.3719 0.5163 0.0306 1.0000 Uiso R . . . . . .
H61 H 0.1296 0.5480 0.3731 0.0296 1.0000 Uiso R . . . . . .
H62 H 0.0886 0.5542 0.4612 0.0304 1.0000 Uiso R . . . . . .
H63 H 0.2380 0.5715 0.4140 0.0298 1.0000 Uiso R . . . . . .
H91 H -0.1509 0.5438 0.2833 0.0253 1.0000 Uiso R . . . . . .
H111 H 0.1859 0.6303 0.1269 0.0260 1.0000 Uiso R . . . . . .
H131 H 0.4227 0.4676 0.1639 0.0301 1.0000 Uiso R . . . . . .
H132 H 0.3942 0.5343 0.0995 0.0307 1.0000 Uiso R . . . . . .
H133 H 0.4279 0.5646 0.1708 0.0313 1.0000 Uiso R . . . . . .
H141 H -0.0578 0.6879 0.1184 0.0594 1.0000 Uiso R . . . . . .
H142 H -0.0718 0.7263 0.1925 0.0599 1.0000 Uiso R . . . . . .
H143 H -0.1783 0.6653 0.1879 0.0585 1.0000 Uiso R . . . . . .
H151 H -0.0796 0.4387 0.3995 0.0278 1.0000 Uiso R . . . . . .
H152 H -0.1364 0.3937 0.3445 0.0273 1.0000 Uiso R . . . . . .
H153 H 0.0041 0.3606 0.3619 0.0251 1.0000 Uiso R . . . . . .
H161 H 0.0209 0.2454 0.4431 0.0229 1.0000 Uiso R . . . . . .
H171 H 0.0699 0.1869 0.5873 0.0411 1.0000 Uiso R . . . . . .
H172 H 0.1507 0.2636 0.5383 0.0428 1.0000 Uiso R . . . . . .
H173 H -0.0066 0.2711 0.5651 0.0425 1.0000 Uiso R . . . . . .
H181 H -0.1452 0.1542 0.5197 0.0355 1.0000 Uiso R . . . . . .
H182 H -0.0334 0.0823 0.5293 0.0343 1.0000 Uiso R . . . . . .
H183 H -0.0671 0.1065 0.4489 0.0340 1.0000 Uiso R . . . . . .
H191 H 0.2161 0.0149 0.4379 0.0223 1.0000 Uiso R . . . . . .
H201 H 0.2883 -0.0072 0.5540 0.0388 1.0000 Uiso R . . . . . .
H202 H 0.2999 0.0921 0.5518 0.0382 1.0000 Uiso R . . . . . .
H203 H 0.1553 0.0537 0.5655 0.0374 1.0000 Uiso R . . . . . .
H211 H 0.4537 0.0461 0.3591 0.0330 1.0000 Uiso R . . . . . .
H212 H 0.4469 -0.0296 0.4251 0.0354 1.0000 Uiso R . . . . . .
H213 H 0.4836 0.0624 0.4356 0.0340 1.0000 Uiso R . . . . . .
H241 H 0.0671 -0.0979 0.2640 0.0299 1.0000 Uiso R . . . . . .
H261 H -0.2109 0.1019 0.2684 0.0305 1.0000 Uiso R . . . . . .
H281 H 0.3352 0.0058 0.2933 0.0330 1.0000 Uiso R . . . . . .
H282 H 0.2997 -0.0723 0.2593 0.0336 1.0000 Uiso R . . . . . .
H283 H 0.2583 -0.0699 0.3474 0.0345 1.0000 Uiso R . . . . . .
H291 H -0.2022 -0.0418 0.1951 0.0677 1.0000 Uiso R . . . . . .
H292 H -0.1477 -0.1207 0.2348 0.0676 1.0000 Uiso R . . . . . .
H293 H -0.2700 -0.0676 0.2779 0.0667 1.0000 Uiso R . . . . . .
H301 H -0.1105 0.2328 0.3600 0.0309 1.0000 Uiso R . . . . . .
H302 H -0.1692 0.2375 0.2902 0.0332 1.0000 Uiso R . . . . . .
H303 H -0.0215 0.2628 0.2792 0.0301 1.0000 Uiso R . . . . . .
H311 H 0.1434 0.1406 0.1327 0.0279 1.0000 Uiso R . . . . . .
H321 H -0.0587 0.1644 0.0933 0.0516 1.0000 Uiso R . . . . . .
H322 H -0.0189 0.2571 0.0562 0.0515 1.0000 Uiso R . . . . . .
H323 H -0.0595 0.2377 0.1450 0.0503 1.0000 Uiso R . . . . . .
H331 H 0.3155 0.1526 0.0083 0.0487 1.0000 Uiso R . . . . . .
H332 H 0.1983 0.2034 -0.0256 0.0481 1.0000 Uiso R . . . . . .
H333 H 0.1792 0.1088 0.0079 0.0481 1.0000 Uiso R . . . . . .
H341 H 0.2878 0.4076 0.0825 0.0232 1.0000 Uiso R . . . . . .
H351 H 0.1107 0.4788 0.0417 0.0459 1.0000 Uiso R . . . . . .
H352 H 0.0456 0.4269 0.1187 0.0455 1.0000 Uiso R . . . . . .
H353 H 0.0378 0.3942 0.0418 0.0457 1.0000 Uiso R . . . . . .
H361 H 0.2560 0.3394 -0.0493 0.0430 1.0000 Uiso R . . . . . .
H362 H 0.3362 0.4201 -0.0488 0.0434 1.0000 Uiso R . . . . . .
H363 H 0.3978 0.3277 -0.0267 0.0435 1.0000 Uiso R . . . . . .
H391 H 0.7971 0.2565 -0.0235 0.0220 1.0000 Uiso R . . . . . .
H411 H 0.6445 0.0213 0.0302 0.0280 1.0000 Uiso R . . . . . .
H431 H 0.5302 0.3829 0.0440 0.0367 1.0000 Uiso R . . . . . .
H432 H 0.6858 0.3770 0.0312 0.0373 1.0000 Uiso R . . . . . .
H433 H 0.5897 0.3598 0.1116 0.0377 1.0000 Uiso R . . . . . .
H441 H 0.9128 0.0496 -0.0349 0.0497 1.0000 Uiso R . . . . . .
H442 H 0.9352 0.1391 -0.0817 0.0488 1.0000 Uiso R . . . . . .
H443 H 0.8485 0.0729 -0.1005 0.0494 1.0000 Uiso R . . . . . .
H451 H 0.3568 0.0330 0.0992 0.0468 1.0000 Uiso R . . . . . .
H452 H 0.4575 0.0015 0.1485 0.0467 1.0000 Uiso R . . . . . .
H453 H 0.3514 0.0767 0.1711 0.0441 1.0000 Uiso R . . . . . .
H461 H 0.5219(18) 0.1542(12) 0.2493(10) 0.029(4) 0.9693(7) Uiso . . P 1 1 . .
H462 H 0.5749(19) 0.1987(12) 0.3096(11) 0.035(5) 0.9693(7) Uiso . . P 1 1 . .
H463 H 0.5855(17) 0.2447(13) 0.2289(11) 0.022(4) 0.9693(7) Uiso . . P 1 1 . .
H471 H 0.2647 0.7601 0.1650 0.0377 1.0000 Uiso R . . . . . .
H481 H 0.2179 0.7027 0.2929 0.0418 1.0000 Uiso R . . . . . .
H491 H 0.3801 0.7112 0.3622 0.0472 1.0000 Uiso R . . . . . .
H501 H 0.5883 0.7726 0.3045 0.0524 1.0000 Uiso R . . . . . .
H511 H 0.6384 0.8243 0.1744 0.0490 1.0000 Uiso R . . . . . .
H521 H 0.4766 0.8190 0.1061 0.0390 1.0000 Uiso R . . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
I1 0.02301(4) 0.03227(4) 0.02066(4) -0.00465(3) -0.01391(3) 0.00508(3)
Zr1 0.00974(4) 0.01129(4) 0.00981(4) -0.00128(3) -0.00273(3) -0.00001(3)
Co1 0.01176(6) 0.01623(7) 0.01223(6) -0.00082(5) -0.00465(5) 0.00080(5)
P1 0.01176(11) 0.01424(11) 0.01172(11) -0.00268(9) -0.00372(9) -0.00078(9)
P2 0.01331(11) 0.01449(12) 0.01286(11) 0.00138(9) -0.00264(9) -0.00007(9)
P3 0.01638(12) 0.01892(13) 0.01288(11) -0.00254(9) -0.00601(9) -0.00057(10)
N1 0.0133(4) 0.0121(4) 0.0124(4) -0.0019(3) -0.0050(3) 0.0006(3)
N2 0.0133(4) 0.0143(4) 0.0149(4) 0.0000(3) -0.0034(3) -0.0016(3)
N3 0.0154(4) 0.0167(4) 0.0124(4) -0.0032(3) -0.0035(3) 0.0012(3)
C1 0.0165(5) 0.0199(5) 0.0172(5) -0.0032(4) -0.0050(4) -0.0046(4)
C2 0.0210(5) 0.0310(6) 0.0225(5) -0.0074(5) -0.0071(4) -0.0086(5)
C3 0.0163(5) 0.0316(6) 0.0209(5) -0.0064(5) -0.0016(4) -0.0061(4)
C4 0.0153(4) 0.0169(5) 0.0143(4) -0.0044(4) -0.0035(4) -0.0006(4)
C5 0.0217(5) 0.0241(5) 0.0143(5) -0.0054(4) -0.0053(4) 0.0011(4)
C6 0.0217(5) 0.0176(5) 0.0196(5) -0.0061(4) -0.0055(4) 0.0014(4)
C7 0.0152(4) 0.0124(4) 0.0146(4) -0.0025(3) -0.0061(4) 0.0005(3)
C8 0.0151(4) 0.0146(4) 0.0176(5) -0.0032(4) -0.0064(4) 0.0002(4)
C9 0.0170(5) 0.0185(5) 0.0266(6) -0.0036(4) -0.0093(4) 0.0029(4)
C10 0.0253(6) 0.0167(5) 0.0298(6) 0.0006(4) -0.0147(5) 0.0029(4)
C11 0.0261(6) 0.0162(5) 0.0222(5) 0.0029(4) -0.0103(4) -0.0016(4)
C12 0.0188(5) 0.0153(5) 0.0156(5) -0.0013(4) -0.0061(4) -0.0015(4)
C13 0.0205(5) 0.0216(5) 0.0169(5) 0.0014(4) -0.0025(4) -0.0028(4)
C14 0.0350(7) 0.0277(7) 0.0534(9) 0.0083(6) -0.0211(7) 0.0078(6)
C15 0.0145(4) 0.0182(5) 0.0208(5) -0.0024(4) -0.0036(4) -0.0013(4)
C16 0.0172(5) 0.0183(5) 0.0165(5) 0.0014(4) -0.0001(4) 0.0011(4)
C17 0.0341(7) 0.0250(6) 0.0186(5) -0.0036(4) 0.0014(5) -0.0024(5)
C18 0.0162(5) 0.0259(6) 0.0230(5) 0.0038(4) -0.0001(4) -0.0021(4)
C19 0.0187(5) 0.0173(5) 0.0194(5) 0.0039(4) -0.0050(4) 0.0006(4)
C20 0.0250(6) 0.0295(6) 0.0195(5) 0.0073(5) -0.0059(4) 0.0014(5)
C21 0.0199(5) 0.0214(5) 0.0259(6) 0.0016(4) -0.0065(4) 0.0039(4)
C22 0.0155(4) 0.0156(5) 0.0148(4) -0.0021(4) -0.0010(4) -0.0032(4)
C23 0.0209(5) 0.0158(5) 0.0160(5) -0.0018(4) 0.0008(4) -0.0016(4)
C24 0.0296(6) 0.0173(5) 0.0228(5) -0.0066(4) 0.0009(5) -0.0053(4)
C25 0.0254(6) 0.0275(6) 0.0268(6) -0.0107(5) -0.0008(5) -0.0109(5)
C26 0.0167(5) 0.0295(6) 0.0280(6) -0.0094(5) -0.0043(4) -0.0050(4)
C27 0.0152(5) 0.0192(5) 0.0203(5) -0.0052(4) -0.0026(4) -0.0023(4)
C28 0.0267(6) 0.0178(5) 0.0209(5) -0.0022(4) -0.0020(4) 0.0043(4)
C29 0.0365(8) 0.0416(9) 0.0559(10) -0.0236(8) -0.0081(7) -0.0163(7)
C30 0.0157(5) 0.0213(5) 0.0266(6) -0.0067(4) -0.0065(4) 0.0019(4)
C31 0.0272(6) 0.0262(6) 0.0196(5) -0.0018(4) -0.0106(4) -0.0080(5)
C32 0.0300(7) 0.0424(8) 0.0367(7) -0.0003(6) -0.0203(6) -0.0099(6)
C33 0.0464(8) 0.0335(7) 0.0216(6) -0.0075(5) -0.0110(6) -0.0123(6)
C34 0.0247(5) 0.0202(5) 0.0184(5) -0.0007(4) -0.0104(4) -0.0001(4)
C35 0.0310(7) 0.0280(6) 0.0377(7) -0.0026(5) -0.0188(6) 0.0066(5)
C36 0.0390(7) 0.0296(6) 0.0178(5) 0.0024(5) -0.0074(5) -0.0051(5)
C37 0.0177(5) 0.0179(5) 0.0110(4) -0.0027(4) -0.0036(4) 0.0017(4)
C38 0.0185(5) 0.0179(5) 0.0139(4) -0.0023(4) -0.0057(4) 0.0007(4)
C39 0.0172(5) 0.0230(5) 0.0149(5) -0.0010(4) -0.0042(4) -0.0002(4)
C40 0.0207(5) 0.0247(6) 0.0164(5) -0.0046(4) -0.0025(4) 0.0044(4)
C41 0.0276(6) 0.0186(5) 0.0203(5) -0.0047(4) -0.0008(4) 0.0033(4)
C42 0.0243(5) 0.0181(5) 0.0152(5) -0.0024(4) -0.0003(4) 0.0004(4)
C43 0.0226(5) 0.0194(5) 0.0235(5) -0.0045(4) -0.0035(4) -0.0020(4)
C44 0.0245(6) 0.0321(7) 0.0303(7) -0.0084(5) 0.0029(5) 0.0049(5)
C45 0.0358(7) 0.0180(5) 0.0283(6) -0.0014(5) 0.0081(5) -0.0022(5)
C46 0.0156(6) 0.0239(7) 0.0155(6) -0.0022(5) -0.0047(5) 0.0002(5)
C47 0.0447(8) 0.0242(6) 0.0283(6) -0.0053(5) -0.0147(6) -0.0058(5)
C48 0.0486(9) 0.0260(6) 0.0294(7) -0.0008(5) -0.0118(6) -0.0115(6)
C49 0.0624(10) 0.0274(7) 0.0290(7) 0.0009(5) -0.0208(7) -0.0056(7)
C50 0.0469(9) 0.0412(9) 0.0495(10) -0.0047(7) -0.0287(8) 0.0011(7)
C51 0.0313(7) 0.0426(9) 0.0460(9) -0.0063(7) -0.0070(6) -0.0010(6)
C52 0.0432(8) 0.0278(6) 0.0236(6) -0.0064(5) -0.0048(6) 0.0009(6)
_refine_ls_extinction_method None
_oxford_refine_ls_scale 0.127061(13)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
I1 . Co1 . 2.57987(18) yes
I2 . Zr1 . 2.729(4) yes
I2 . Co1 . 2.647(4) yes
Zr1 . Co1 . 2.61347(19) yes
Zr1 . P1 . 2.8981(3) yes
Zr1 . P2 . 2.8415(3) yes
Zr1 . P3 . 2.7000(3) yes
Zr1 . N1 . 2.1600(9) yes
Zr1 . N2 . 2.1253(9) yes
Zr1 . N3 . 2.1448(9) yes
Zr1 . C46 . 2.3430(18) yes
Zr1 . Co1 . 2.61347(19) yes
Zr1 . P1 . 2.8981(3) yes
Zr1 . P2 . 2.8415(3) yes
Zr1 . P3 . 2.7000(3) yes
Zr1 . N1 . 2.1600(9) yes
Zr1 . N2 . 2.1253(9) yes
Zr1 . N3 . 2.1448(9) yes
Co1 . P1 . 2.2655(3) yes
Co1 . P2 . 2.3032(3) yes
Co1 . C46 . 2.2653(19) yes
Co1 . H462 . 2.095(19) no
Co1 . P1 . 2.2655(3) yes
Co1 . P2 . 2.3032(3) yes
P1 . N1 . 1.6936(9) yes
P1 . C1 . 1.8606(11) yes
P1 . C4 . 1.8616(11) yes
P2 . N2 . 1.7008(10) yes
P2 . C16 . 1.8558(11) yes
P2 . C19 . 1.8535(11) yes
P3 . N3 . 1.6845(10) yes
P3 . C31 . 1.8523(12) yes
P3 . C34 . 1.8515(12) yes
N1 . C7 . 1.4394(13) yes
N2 . C22 . 1.4450(13) yes
N3 . C37 . 1.4335(13) yes
C1 . C2 . 1.5359(15) yes
C1 . C3 . 1.5321(16) yes
C1 . H11 . 0.958 no
C2 . H21 . 0.963 no
C2 . H22 . 0.948 no
C2 . H23 . 0.979 no
C3 . H31 . 0.959 no
C3 . H32 . 0.975 no
C3 . H33 . 0.957 no
C4 . C5 . 1.5396(15) yes
C4 . C6 . 1.5367(15) yes
C4 . H41 . 0.973 no
C5 . H51 . 0.978 no
C5 . H52 . 0.967 no
C5 . H53 . 0.949 no
C6 . H61 . 0.966 no
C6 . H62 . 0.958 no
C6 . H63 . 0.955 no
C7 . C8 . 1.4127(14) yes
C7 . C12 . 1.4099(14) yes
C8 . C9 . 1.3962(15) yes
C8 . C15 . 1.5012(15) yes
C9 . C10 . 1.3879(17) yes
C9 . H91 . 0.944 no
C10 . C11 . 1.3844(18) yes
C10 . C14 . 1.5080(17) yes
C11 . C12 . 1.3961(15) yes
C11 . H111 . 0.936 no
C12 . C13 . 1.5043(16) yes
C13 . H131 . 0.950 no
C13 . H132 . 0.965 no
C13 . H133 . 0.963 no
C14 . H141 . 0.952 no
C14 . H142 . 0.937 no
C14 . H143 . 0.943 no
C15 . H151 . 0.959 no
C15 . H152 . 0.961 no
C15 . H153 . 0.958 no
C16 . C17 . 1.5359(17) yes
C16 . C18 . 1.5316(16) yes
C16 . H161 . 0.984 no
C17 . H171 . 0.949 no
C17 . H172 . 0.956 no
C17 . H173 . 0.948 no
C18 . H181 . 0.958 no
C18 . H182 . 0.970 no
C18 . H183 . 0.973 no
C19 . C20 . 1.5331(17) yes
C19 . C21 . 1.5368(16) yes
C19 . H191 . 0.969 no
C20 . H201 . 0.963 no
C20 . H202 . 0.970 no
C20 . H203 . 0.967 no
C21 . H211 . 0.956 no
C21 . H212 . 0.974 no
C21 . H213 . 0.960 no
C22 . C23 . 1.4114(15) yes
C22 . C27 . 1.4166(15) yes
C23 . C24 . 1.4003(17) yes
C23 . C28 . 1.5034(17) yes
C24 . C25 . 1.380(2) yes
C24 . H241 . 0.937 no
C25 . C26 . 1.3885(18) yes
C25 . C29 . 1.5069(18) yes
C26 . C27 . 1.3922(16) yes
C26 . H261 . 0.946 no
C27 . C30 . 1.5006(16) yes
C28 . H281 . 0.948 no
C28 . H282 . 0.952 no
C28 . H283 . 0.969 no
C29 . H291 . 0.929 no
C29 . H292 . 0.944 no
C29 . H293 . 0.927 no
C30 . H301 . 0.956 no
C30 . H302 . 0.948 no
C30 . H303 . 0.957 no
C31 . C32 . 1.5313(19) yes
C31 . C33 . 1.5382(18) yes
C31 . H311 . 0.966 no
C32 . H321 . 0.962 no
C32 . H322 . 0.977 no
C32 . H323 . 0.956 no
C33 . H331 . 0.984 no
C33 . H332 . 0.964 no
C33 . H333 . 0.954 no
C34 . C35 . 1.5326(17) yes
C34 . C36 . 1.5336(17) yes
C34 . H341 . 0.966 no
C35 . H351 . 0.963 no
C35 . H352 . 0.951 no
C35 . H353 . 0.969 no
C36 . H361 . 0.973 no
C36 . H362 . 0.960 no
C36 . H363 . 0.969 no
C37 . C38 . 1.4082(15) yes
C37 . C42 . 1.4073(15) yes
C38 . C39 . 1.3947(15) yes
C38 . C43 . 1.5020(16) yes
C39 . C40 . 1.3871(17) yes
C39 . H391 . 0.943 no
C40 . C41 . 1.3852(17) yes
C40 . C44 . 1.5092(17) yes
C41 . C42 . 1.3970(16) yes
C41 . H411 . 0.943 no
C42 . C45 . 1.4998(17) yes
C43 . H431 . 0.940 no
C43 . H432 . 0.959 no
C43 . H433 . 0.923 no
C44 . H441 . 0.951 no
C44 . H442 . 0.952 no
C44 . H443 . 0.925 no
C45 . H451 . 0.955 no
C45 . H452 . 0.949 no
C45 . H453 . 0.946 no
C46 . H461 . 0.974(19) no
C46 . H462 . 0.97(2) no
C46 . H463 . 0.97(2) no
C47 . C48 . 1.389(2) yes
C47 . C52 . 1.377(2) yes
C47 . H471 . 0.948 no
C48 . C49 . 1.379(2) yes
C48 . H481 . 0.948 no
C49 . C50 . 1.384(3) yes
C49 . H491 . 0.921 no
C50 . C51 . 1.385(3) yes
C50 . H501 . 0.937 no
C51 . C52 . 1.384(2) yes
C51 . H511 . 0.934 no
C52 . H521 . 0.929 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Zr1 . I2 . Co1 . 58.15(8) yes
Co1 . Zr1 . P1 . 48.201(6) yes
Co1 . Zr1 . P2 . 49.734(7) yes
P1 . Zr1 . P2 . 82.142(9) yes
Co1 . Zr1 . P3 . 174.628(8) yes
P1 . Zr1 . P3 . 128.931(9) yes
P2 . Zr1 . P3 . 135.637(9) yes
Co1 . Zr1 . N1 . 83.41(2) yes
P1 . Zr1 . N1 . 35.47(2) yes
P2 . Zr1 . N1 . 105.15(2) yes
P3 . Zr1 . N1 . 94.26(2) yes
Co1 . Zr1 . N2 . 85.55(3) yes
P1 . Zr1 . N2 . 114.85(3) yes
P2 . Zr1 . N2 . 36.58(3) yes
P3 . Zr1 . N2 . 99.76(3) yes
N1 . Zr1 . N2 . 123.58(3) yes
Co1 . Zr1 . N3 . 138.50(2) yes
P1 . Zr1 . N3 . 134.57(3) yes
P2 . Zr1 . N3 . 140.49(3) yes
P3 . Zr1 . N3 . 38.59(3) yes
N1 . Zr1 . N3 . 113.95(3) yes
Co1 . Zr1 . C46 . 54.06(4) yes
P1 . Zr1 . C46 . 86.23(3) yes
P2 . Zr1 . C46 . 83.90(4) yes
P3 . Zr1 . C46 . 123.36(4) yes
N1 . Zr1 . C46 . 114.97(4) yes
N2 . Zr1 . N3 . 110.58(4) yes
N2 . Zr1 . C46 . 101.71(4) yes
N3 . Zr1 . C46 . 84.77(5) yes
I2 . Zr1 . Co1 . 59.36(8) yes
I2 . Zr1 . P1 . 88.65(7) yes
Co1 . Zr1 . P1 . 48.201(6) yes
I2 . Zr1 . P2 . 89.57(8) yes
Co1 . Zr1 . P2 . 49.734(7) yes
P1 . Zr1 . P2 . 82.142(9) yes
I2 . Zr1 . P3 . 117.83(8) yes
Co1 . Zr1 . P3 . 174.628(8) yes
P1 . Zr1 . P3 . 128.931(9) yes
P2 . Zr1 . P3 . 135.637(9) yes
I2 . Zr1 . N1 . 115.09(8) yes
Co1 . Zr1 . N1 . 83.41(2) yes
P1 . Zr1 . N1 . 35.47(2) yes
P2 . Zr1 . N1 . 105.15(2) yes
P3 . Zr1 . N1 . 94.26(2) yes
I2 . Zr1 . N2 . 105.58(8) yes
Co1 . Zr1 . N2 . 85.55(3) yes
P1 . Zr1 . N2 . 114.85(3) yes
P2 . Zr1 . N2 . 36.58(3) yes
P3 . Zr1 . N2 . 99.76(3) yes
I2 . Zr1 . N3 . 79.27(8) yes
Co1 . Zr1 . N3 . 138.50(2) yes
P1 . Zr1 . N3 . 134.57(3) yes
P2 . Zr1 . N3 . 140.49(3) yes
P3 . Zr1 . N3 . 38.59(3) yes
N1 . Zr1 . N2 . 123.58(3) yes
N1 . Zr1 . N3 . 113.95(3) yes
N2 . Zr1 . N3 . 110.58(4) yes
I1 . Co1 . Zr1 . 166.525(7) yes
I1 . Co1 . P1 . 111.994(9) yes
Zr1 . Co1 . P1 . 72.484(8) yes
I1 . Co1 . P2 . 117.441(9) yes
Zr1 . Co1 . P2 . 70.287(9) yes
P1 . Co1 . P2 . 111.260(11) yes
I1 . Co1 . C46 . 109.88(4) yes
Zr1 . Co1 . C46 . 56.86(4) yes
P1 . Co1 . C46 . 105.44(4) yes
P2 . Co1 . C46 . 99.44(4) yes
I1 . Co1 . H462 . 84.7(5) no
Zr1 . Co1 . H462 . 82.2(5) no
P1 . Co1 . H462 . 119.7(5) no
P2 . Co1 . H462 . 109.8(5) no
C46 . Co1 . H462 . 25.4(5) no
I2 . Co1 . I1 . 104.15(8) yes
I2 . Co1 . Zr1 . 62.49(8) yes
I1 . Co1 . Zr1 . 166.525(7) yes
I2 . Co1 . P1 . 106.12(8) yes
I1 . Co1 . P1 . 111.994(9) yes
Zr1 . Co1 . P1 . 72.484(8) yes
I2 . Co1 . P2 . 104.69(8) yes
I1 . Co1 . P2 . 117.441(9) yes
Zr1 . Co1 . P2 . 70.287(9) yes
P1 . Co1 . P2 . 111.260(11) yes
Zr1 . P1 . Co1 . 59.315(8) yes
Zr1 . P1 . N1 . 47.74(3) yes
Co1 . P1 . N1 . 106.65(3) yes
Zr1 . P1 . C1 . 121.50(4) yes
Co1 . P1 . C1 . 114.39(4) yes
N1 . P1 . C1 . 108.45(5) yes
Zr1 . P1 . C4 . 132.01(3) yes
Co1 . P1 . C4 . 113.77(4) yes
N1 . P1 . C4 . 108.56(5) yes
C1 . P1 . C4 . 104.84(5) yes
Zr1 . P2 . Co1 . 59.978(8) yes
Zr1 . P2 . N2 . 48.14(3) yes
Co1 . P2 . N2 . 106.97(3) yes
Zr1 . P2 . C16 . 118.27(4) yes
Co1 . P2 . C16 . 117.46(4) yes
N2 . P2 . C16 . 106.28(5) yes
Zr1 . P2 . C19 . 133.73(4) yes
Co1 . P2 . C19 . 109.56(4) yes
N2 . P2 . C19 . 109.92(5) yes
C16 . P2 . C19 . 106.51(5) yes
Zr1 . P3 . N3 . 52.58(3) yes
Zr1 . P3 . C31 . 126.35(4) yes
N3 . P3 . C31 . 111.51(5) yes
Zr1 . P3 . C34 . 124.17(4) yes
N3 . P3 . C34 . 110.33(5) yes
C31 . P3 . C34 . 109.47(5) yes
P1 . N1 . Zr1 . 96.79(4) yes
P1 . N1 . C7 . 125.75(7) yes
Zr1 . N1 . C7 . 137.31(7) yes
P2 . N2 . Zr1 . 95.27(4) yes
P2 . N2 . C22 . 129.28(7) yes
Zr1 . N2 . C22 . 135.28(7) yes
P3 . N3 . Zr1 . 88.83(4) yes
P3 . N3 . C37 . 131.01(7) yes
Zr1 . N3 . C37 . 139.91(7) yes
P1 . C1 . C2 . 114.43(8) yes
P1 . C1 . C3 . 109.67(8) yes
C2 . C1 . C3 . 108.19(9) yes
P1 . C1 . H11 . 106.3 no
C2 . C1 . H11 . 108.4 no
C3 . C1 . H11 . 109.8 no
C1 . C2 . H21 . 112.5 no
C1 . C2 . H22 . 110.5 no
H21 . C2 . H22 . 108.5 no
C1 . C2 . H23 . 109.0 no
H21 . C2 . H23 . 108.3 no
H22 . C2 . H23 . 108.0 no
C1 . C3 . H31 . 110.0 no
C1 . C3 . H32 . 110.6 no
H31 . C3 . H32 . 108.8 no
C1 . C3 . H33 . 111.4 no
H31 . C3 . H33 . 107.4 no
H32 . C3 . H33 . 108.6 no
P1 . C4 . C5 . 113.86(7) yes
P1 . C4 . C6 . 114.66(8) yes
C5 . C4 . C6 . 110.22(9) yes
P1 . C4 . H41 . 102.0 no
C5 . C4 . H41 . 107.0 no
C6 . C4 . H41 . 108.3 no
C4 . C5 . H51 . 109.6 no
C4 . C5 . H52 . 111.1 no
H51 . C5 . H52 . 107.3 no
C4 . C5 . H53 . 113.0 no
H51 . C5 . H53 . 107.5 no
H52 . C5 . H53 . 108.2 no
C4 . C6 . H61 . 112.4 no
C4 . C6 . H62 . 109.5 no
H61 . C6 . H62 . 107.8 no
C4 . C6 . H63 . 110.7 no
H61 . C6 . H63 . 108.5 no
H62 . C6 . H63 . 107.8 no
N1 . C7 . C8 . 120.42(9) yes
N1 . C7 . C12 . 121.50(9) yes
C8 . C7 . C12 . 118.08(9) yes
C7 . C8 . C9 . 119.95(10) yes
C7 . C8 . C15 . 123.18(9) yes
C9 . C8 . C15 . 116.80(10) yes
C8 . C9 . C10 . 122.32(11) yes
C8 . C9 . H91 . 117.4 no
C10 . C9 . H91 . 120.3 no
C9 . C10 . C11 . 117.20(10) yes
C9 . C10 . C14 . 121.28(12) yes
C11 . C10 . C14 . 121.52(12) yes
C10 . C11 . C12 . 122.69(11) yes
C10 . C11 . H111 . 119.0 no
C12 . C11 . H111 . 118.3 no
C7 . C12 . C11 . 119.74(10) yes
C7 . C12 . C13 . 123.55(10) yes
C11 . C12 . C13 . 116.71(10) yes
C12 . C13 . H131 . 110.9 no
C12 . C13 . H132 . 111.0 no
H131 . C13 . H132 . 106.9 no
C12 . C13 . H133 . 112.8 no
H131 . C13 . H133 . 107.4 no
H132 . C13 . H133 . 107.5 no
C10 . C14 . H141 . 112.8 no
C10 . C14 . H142 . 110.8 no
H141 . C14 . H142 . 105.7 no
C10 . C14 . H143 . 112.3 no
H141 . C14 . H143 . 107.7 no
H142 . C14 . H143 . 107.3 no
C8 . C15 . H151 . 111.5 no
C8 . C15 . H152 . 111.7 no
H151 . C15 . H152 . 106.0 no
C8 . C15 . H153 . 111.4 no
H151 . C15 . H153 . 107.4 no
H152 . C15 . H153 . 108.7 no
P2 . C16 . C17 . 114.62(9) yes
P2 . C16 . C18 . 114.49(8) yes
C17 . C16 . C18 . 111.24(10) yes
P2 . C16 . H161 . 101.5 no
C17 . C16 . H161 . 107.4 no
C18 . C16 . H161 . 106.6 no
C16 . C17 . H171 . 111.4 no
C16 . C17 . H172 . 112.8 no
H171 . C17 . H172 . 109.1 no
C16 . C17 . H173 . 109.3 no
H171 . C17 . H173 . 107.7 no
H172 . C17 . H173 . 106.3 no
C16 . C18 . H181 . 111.4 no
C16 . C18 . H182 . 110.3 no
H181 . C18 . H182 . 106.7 no
C16 . C18 . H183 . 112.3 no
H181 . C18 . H183 . 107.3 no
H182 . C18 . H183 . 108.6 no
P2 . C19 . C20 . 113.57(9) yes
P2 . C19 . C21 . 111.26(8) yes
C20 . C19 . C21 . 108.11(10) yes
P2 . C19 . H191 . 105.4 no
C20 . C19 . H191 . 108.5 no
C21 . C19 . H191 . 109.8 no
C19 . C20 . H201 . 108.9 no
C19 . C20 . H202 . 111.0 no
H201 . C20 . H202 . 107.5 no
C19 . C20 . H203 . 114.1 no
H201 . C20 . H203 . 107.3 no
H202 . C20 . H203 . 107.7 no
C19 . C21 . H211 . 113.3 no
C19 . C21 . H212 . 109.9 no
H211 . C21 . H212 . 108.8 no
C19 . C21 . H213 . 109.4 no
H211 . C21 . H213 . 107.9 no
H212 . C21 . H213 . 107.3 no
N2 . C22 . C23 . 122.54(10) yes
N2 . C22 . C27 . 119.25(9) yes
C23 . C22 . C27 . 118.05(10) yes
C22 . C23 . C24 . 119.23(11) yes
C22 . C23 . C28 . 124.69(10) yes
C24 . C23 . C28 . 116.07(10) yes
C23 . C24 . C25 . 123.16(11) yes
C23 . C24 . H241 . 118.3 no
C25 . C24 . H241 . 118.5 no
C24 . C25 . C26 . 117.15(11) yes
C24 . C25 . C29 . 122.15(13) yes
C26 . C25 . C29 . 120.70(13) yes
C25 . C26 . C27 . 122.25(12) yes
C25 . C26 . H261 . 119.6 no
C27 . C26 . H261 . 118.1 no
C22 . C27 . C26 . 120.16(11) yes
C22 . C27 . C30 . 121.78(10) yes
C26 . C27 . C30 . 118.05(10) yes
C23 . C28 . H281 . 111.3 no
C23 . C28 . H282 . 110.4 no
H281 . C28 . H282 . 108.0 no
C23 . C28 . H283 . 111.0 no
H281 . C28 . H283 . 108.8 no
H282 . C28 . H283 . 107.2 no
C25 . C29 . H291 . 110.6 no
C25 . C29 . H292 . 112.4 no
H291 . C29 . H292 . 105.3 no
C25 . C29 . H293 . 112.8 no
H291 . C29 . H293 . 107.5 no
H292 . C29 . H293 . 107.8 no
C27 . C30 . H301 . 112.6 no
C27 . C30 . H302 . 111.5 no
H301 . C30 . H302 . 106.3 no
C27 . C30 . H303 . 112.5 no
H301 . C30 . H303 . 107.6 no
H302 . C30 . H303 . 106.0 no
P3 . C31 . C32 . 111.29(10) yes
P3 . C31 . C33 . 117.01(9) yes
C32 . C31 . C33 . 109.96(11) yes
P3 . C31 . H311 . 102.0 no
C32 . C31 . H311 . 107.0 no
C33 . C31 . H311 . 108.8 no
C31 . C32 . H321 . 110.8 no
C31 . C32 . H322 . 109.7 no
H321 . C32 . H322 . 106.9 no
C31 . C32 . H323 . 112.9 no
H321 . C32 . H323 . 109.3 no
H322 . C32 . H323 . 106.9 no
C31 . C33 . H331 . 111.5 no
C31 . C33 . H332 . 111.3 no
H331 . C33 . H332 . 108.5 no
C31 . C33 . H333 . 109.7 no
H331 . C33 . H333 . 109.3 no
H332 . C33 . H333 . 106.4 no
P3 . C34 . C35 . 111.92(9) yes
P3 . C34 . C36 . 117.95(9) yes
C35 . C34 . C36 . 110.95(11) yes
P3 . C34 . H341 . 101.7 no
C35 . C34 . H341 . 105.5 no
C36 . C34 . H341 . 107.6 no
C34 . C35 . H351 . 108.6 no
C34 . C35 . H352 . 111.8 no
H351 . C35 . H352 . 106.9 no
C34 . C35 . H353 . 112.2 no
H351 . C35 . H353 . 107.9 no
H352 . C35 . H353 . 109.2 no
C34 . C36 . H361 . 110.7 no
C34 . C36 . H362 . 110.1 no
H361 . C36 . H362 . 106.8 no
C34 . C36 . H363 . 111.9 no
H361 . C36 . H363 . 108.2 no
H362 . C36 . H363 . 109.0 no
N3 . C37 . C38 . 120.85(10) yes
N3 . C37 . C42 . 120.42(10) yes
C38 . C37 . C42 . 118.52(10) yes
C37 . C38 . C39 . 119.53(10) yes
C37 . C38 . C43 . 121.96(10) yes
C39 . C38 . C43 . 118.45(10) yes
C38 . C39 . C40 . 122.64(11) yes
C38 . C39 . H391 . 118.7 no
C40 . C39 . H391 . 118.6 no
C39 . C40 . C41 . 117.09(10) yes
C39 . C40 . C44 . 121.30(11) yes
C41 . C40 . C44 . 121.60(11) yes
C40 . C41 . C42 . 122.51(11) yes
C40 . C41 . H411 . 119.7 no
C42 . C41 . H411 . 117.8 no
C37 . C42 . C41 . 119.62(11) yes
C37 . C42 . C45 . 122.43(10) yes
C41 . C42 . C45 . 117.90(11) yes
C38 . C43 . H431 . 112.6 no
C38 . C43 . H432 . 111.3 no
H431 . C43 . H432 . 105.7 no
C38 . C43 . H433 . 111.6 no
H431 . C43 . H433 . 106.7 no
H432 . C43 . H433 . 108.6 no
C40 . C44 . H441 . 111.7 no
C40 . C44 . H442 . 111.2 no
H441 . C44 . H442 . 108.6 no
C40 . C44 . H443 . 110.9 no
H441 . C44 . H443 . 105.3 no
H442 . C44 . H443 . 108.9 no
C42 . C45 . H451 . 112.2 no
C42 . C45 . H452 . 110.6 no
H451 . C45 . H452 . 107.4 no
C42 . C45 . H453 . 110.9 no
H451 . C45 . H453 . 107.2 no
H452 . C45 . H453 . 108.3 no
Co1 . C46 . Zr1 . 69.08(6) yes
Co1 . C46 . H461 . 127.7(11) no
Zr1 . C46 . H461 . 94.0(10) no
Co1 . C46 . H462 . 67.5(11) no
Zr1 . C46 . H462 . 136.3(11) no
H461 . C46 . H462 . 109.0(15) no
Co1 . C46 . H463 . 124.9(10) no
Zr1 . C46 . H463 . 103.7(11) no
H461 . C46 . H463 . 106.9(15) no
H462 . C46 . H463 . 104.3(15) no
C48 . C47 . C52 . 120.36(14) yes
C48 . C47 . H471 . 119.3 no
C52 . C47 . H471 . 120.3 no
C47 . C48 . C49 . 119.91(15) yes
C47 . C48 . H481 . 119.8 no
C49 . C48 . H481 . 120.3 no
C48 . C49 . C50 . 119.77(15) yes
C48 . C49 . H491 . 120.5 no
C50 . C49 . H491 . 119.7 no
C49 . C50 . C51 . 120.26(15) yes
C49 . C50 . H501 . 119.8 no
C51 . C50 . H501 . 119.9 no
C50 . C51 . C52 . 119.92(15) yes
C50 . C51 . H511 . 121.3 no
C52 . C51 . H511 . 118.8 no
C51 . C52 . C47 . 119.78(14) yes
C51 . C52 . H521 . 120.0 no
C47 . C52 . H521 . 120.2 no
C46 . H462 . Co1 . 87.1(12) no
#===END
data_6
_database_code_depnum_ccdc_archive 'CCDC 776341'
#TrackingRef '- combined_rev.cif'
_audit_creation_date 10-01-26
_audit_creation_method CRYSTALS_ver_14.01
_oxford_structure_analysis_title 'cmt34_0m in P2(1)/n'
_chemical_name_systematic ?
_chemical_melting_point ?
_cell_length_a 12.6346(10)
_cell_length_b 29.449(2)
_cell_length_c 13.3675(10)
_cell_angle_alpha 90
_cell_angle_beta 106.141(4)
_cell_angle_gamma 90
_cell_volume 4777.7(6)
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_H-M 'P 1 21/n 1 '
_symmetry_space_group_name_Hall '-P 2yn'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x+1/2,y+1/2,-z+1/2
x+1/2,-y+1/2,z+1/2
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Co 0.3494 0.9721 12.2841 4.2791 7.3409 0.2784 4.0034 13.5359 2.3488 71.1692
1.0118 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Zr -2.9673 0.5597 17.8765 1.2762 10.9480 11.9160 5.4173 0.1176 3.6572 87.6627
2.0693 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
I -0.4742 1.8119 20.1472 4.3470 18.9949 0.3814 7.5138 27.7660 2.2735 66.8776
4.0712 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
_cell_formula_units_Z 4
# Given Formula = C45 H74 Co1 I1 N3 P3 Zr1
# Dc = 1.43 Fooo = 2120.00 Mu = 13.45 M = 1027.08
# Found Formula = C45 H74 Co1 I1 N3 P3 Zr1
# Dc = 1.43 FOOO = 2120.00 Mu = 13.45 M = 1027.08
_chemical_formula_sum 'C45 H74 Co1 I1 N3 P3 Zr1'
_chemical_formula_moiety 'C45 H74 Co1 I1 N3 P3 Zr1'
_chemical_compound_source ?
_chemical_formula_weight 1027.08
_cell_measurement_reflns_used 9455
_cell_measurement_theta_min 3
_cell_measurement_theta_max 30
_cell_measurement_temperature 120
_exptl_crystal_description 'acicular fragment'
_exptl_crystal_colour yellow-green
_exptl_crystal_size_min 0.064
_exptl_crystal_size_mid 0.156
_exptl_crystal_size_max 0.631
_exptl_crystal_density_diffrn 1.428
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 2120
_exptl_absorpt_coefficient_mu 1.345
# Sheldrick geometric approximatio 0.81 0.92
_exptl_absorpt_correction_type numerical
_exptl_absorpt_process_details
;
Analytical Absorption (De Meulenaer & Tompa, 1965)
;
_exptl_absorpt_correction_T_min 0.81
_exptl_absorpt_correction_T_max 0.92
_diffrn_measurement_device-type 'Bruker Kappa Apex2'
_diffrn_measurement_device Area
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_measurement_method '\f & \w scans'
# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection 'Apex2 (Bruker AXS, 2006)'
_computing_cell_refinement 'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction 'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution 'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material 'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics 'CAMERON (Watkin et al., 1996)'
_diffrn_standards_interval_time .
_diffrn_standards_interval_count .
_diffrn_standards_number 0
_diffrn_standards_decay_% ?
_diffrn_ambient_temperature 120
_diffrn_reflns_number 81515
_reflns_number_total 13879
_diffrn_reflns_av_R_equivalents 0.035
# Number of reflections without Friedels Law is 0
# Number of reflections with Friedels Law is 13879
# Theoretical number of reflections is about 27889
_diffrn_reflns_theta_min 2.669
_diffrn_reflns_theta_max 30.007
_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full 30.007
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_limit_h_min -17
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_k_min -41
_diffrn_reflns_limit_k_max 40
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_limit_l_max 18
_reflns_limit_h_min -17
_reflns_limit_h_max 17
_reflns_limit_k_min 0
_reflns_limit_k_max 41
_reflns_limit_l_min 0
_reflns_limit_l_max 18
_oxford_diffrn_Wilson_B_factor 1.36
_oxford_diffrn_Wilson_scale 134.48
_atom_sites_solution_primary direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_diff_density_min -0.66
_refine_diff_density_max 1.40
# The current dictionary definitions do not cover the
# situation where the reflections used for refinement were
# selected by a user-defined sigma threshold
# The values actually used during refinement
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns 13879
_refine_ls_number_restraints 4
_refine_ls_number_parameters 495
_oxford_refine_ls_R_factor_ref 0.0417
_refine_ls_wR_factor_ref 0.0859
_refine_ls_goodness_of_fit_ref 1.0000
_refine_ls_shift/su_max 0.0020412
_refine_ls_shift/su_mean 4.0074372
# The values computed from all data
_oxford_reflns_number_all 13879
_refine_ls_R_factor_all 0.0417
_refine_ls_wR_factor_all 0.0859
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression I>2.0\s(I)
_reflns_number_gt 11309
_refine_ls_R_factor_gt 0.0322
_refine_ls_wR_factor_gt 0.0819
# choose from: rm (reference molecule of known chirality),
# ad (anomolous dispersion - Flack), rmad (rm and ad),
# syn (from synthesis), unk (unknown) or . (not applicable).
_chemical_absolute_configuration .
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_hydrogen_treatment none # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.01P)^2^ +16.15P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
# Insert your own references if required - in alphabetical order
_publ_section_references
;
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C.,
Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435.
Betteridge, P.W., Carruthers, J.R., Cooper, R.I.,
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487.
Bruker Analytical X-ray Systems, Inc., 2006. Apex2,
Version 2 User Manual, M86-E01078, Madison, WI.
De Meulenaer, J. & Tompa, H. (1965). Acta Cryst. 19, 1014.
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical
Crystallography Laboratory, Oxford, UK.
;
# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3
# Replace last . with number of unfound hydrogen atomsattached to an atom.
# ..._refinement_flags_...
# . no refinement constraints S special position constraint on site
# G rigid group refinement of site R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond) P partial occupancy constraint
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_oxford_atom_site_special_shape
_atom_site_attached_hydrogens
I1 I 0.467845(16) 0.683020(8) 0.332795(16) 0.0282 1.0000 Uani . . . . . . .
Zr1 Zr 0.795053(19) 0.648584(8) 0.195326(18) 0.0132 1.0000 Uani . . . . . . .
Co1 Co 0.63220(3) 0.654455(12) 0.27311(3) 0.0162 1.0000 Uani . . . . . . .
P1 P 0.60552(5) 0.59374(2) 0.15725(5) 0.0151 1.0000 Uani . . . . . . .
P2 P 0.78969(6) 0.64356(2) 0.40694(5) 0.0168 1.0000 Uani . . . . . . .
P3 P 0.93836(6) 0.67091(2) 0.08759(5) 0.0170 1.0000 Uani . . . . . . .
N1 N 0.70512(17) 0.59683(8) 0.09532(17) 0.0156 1.0000 Uani . . . . . . .
N2 N 0.89008(17) 0.63291(8) 0.35027(17) 0.0165 1.0000 Uani . . . . . . .
N3 N 0.87344(18) 0.70480(8) 0.15074(17) 0.0169 1.0000 Uani . . . . . . .
C1 C 0.6184(2) 0.53679(9) 0.2187(2) 0.0199 1.0000 Uani . . . . . . .
C2 C 0.5551(3) 0.53144(11) 0.3016(2) 0.0288 1.0000 Uani . . . . . . .
C3 C 0.5976(3) 0.49658(10) 0.1429(3) 0.0253 1.0000 Uani . . . . . . .
C4 C 0.4677(2) 0.59609(10) 0.0604(2) 0.0194 1.0000 Uani . . . . . . .
C5 C 0.4318(2) 0.64468(10) 0.0295(2) 0.0232 1.0000 Uani . . . . . . .
C6 C 0.3776(2) 0.57356(11) 0.0991(3) 0.0293 1.0000 Uani . . . . . . .
C7 C 0.7216(2) 0.57179(9) 0.0093(2) 0.0164 1.0000 Uani . . . . . . .
C8 C 0.8049(2) 0.53832(9) 0.0270(2) 0.0182 1.0000 Uani . . . . . . .
C9 C 0.8237(2) 0.51445(10) -0.0562(2) 0.0212 1.0000 Uani . . . . . . .
C10 C 0.7632(2) 0.52242(10) -0.1589(2) 0.0213 1.0000 Uani . . . . . . .
C11 C 0.6853(2) 0.55646(10) -0.1756(2) 0.0203 1.0000 Uani . . . . . . .
C12 C 0.6645(2) 0.58208(9) -0.0947(2) 0.0180 1.0000 Uani . . . . . . .
C13 C 0.8752(2) 0.52774(10) 0.1341(2) 0.0233 1.0000 Uani . . . . . . .
C14 C 0.7819(3) 0.49476(11) -0.2471(2) 0.0284 1.0000 Uani . . . . . . .
C15 C 0.5847(2) 0.62095(10) -0.1247(2) 0.0238 1.0000 Uani . . . . . . .
C16 C 0.8337(3) 0.69211(11) 0.4964(2) 0.0268 1.0000 Uani . . . . . . .
C17 C 0.8158(3) 0.73660(11) 0.4337(3) 0.0312 1.0000 Uani . . . . . . .
C18 C 0.7779(3) 0.69567(13) 0.5830(3) 0.0366 1.0000 Uani . . . . . . .
C19 C 0.7791(2) 0.59496(10) 0.4928(2) 0.0219 1.0000 Uani . . . . . . .
C20 C 0.6752(3) 0.59505(13) 0.5306(2) 0.0309 1.0000 Uani . . . . . . .
C21 C 0.8823(3) 0.58777(11) 0.5846(2) 0.0259 1.0000 Uani . . . . . . .
C22 C 1.0037(2) 0.62049(10) 0.3944(2) 0.0179 1.0000 Uani . . . . . . .
C23 C 1.0335(2) 0.57429(10) 0.4080(2) 0.0187 1.0000 Uani . . . . . . .
C24 C 1.1448(2) 0.56251(10) 0.4419(2) 0.0220 1.0000 Uani . . . . . . .
C25 C 1.2282(2) 0.59480(11) 0.4612(2) 0.0251 1.0000 Uani . . . . . . .
C26 C 1.1975(2) 0.63987(11) 0.4475(2) 0.0243 1.0000 Uani . . . . . . .
C27 C 1.0875(2) 0.65367(10) 0.4154(2) 0.0200 1.0000 Uani . . . . . . .
C28 C 0.9501(2) 0.53645(10) 0.3870(2) 0.0214 1.0000 Uani . . . . . . .
C29 C 1.3482(3) 0.58092(13) 0.4943(3) 0.0358 1.0000 Uani . . . . . . .
C30 C 1.0644(2) 0.70381(10) 0.4034(2) 0.0239 1.0000 Uani . . . . . . .
C31 C 1.0910(2) 0.67002(10) 0.1449(2) 0.0220 1.0000 Uani . . . . . . .
C32 C 1.1283(3) 0.62136(11) 0.1719(3) 0.0282 1.0000 Uani . . . . . . .
C33 C 1.1611(2) 0.69208(12) 0.0817(3) 0.0311 1.0000 Uani . . . . . . .
C34 C 0.9153(2) 0.68866(11) -0.0496(2) 0.0231 1.0000 Uani . . . . . . .
C35 C 0.9320(3) 0.64749(14) -0.1132(3) 0.0373 1.0000 Uani . . . . . . .
C36 C 0.8018(3) 0.70962(13) -0.0924(3) 0.0322 1.0000 Uani . . . . . . .
C37 C 0.8372(2) 0.74955(9) 0.1613(2) 0.0169 1.0000 Uani . . . . . . .
C38 C 0.7297(2) 0.75119(9) 0.1740(2) 0.0185 1.0000 Uani D . . . . . .
C39 C 0.6886(2) 0.79269(10) 0.1973(2) 0.0216 1.0000 Uani . . . . . . .
C40 C 0.7505(2) 0.83242(10) 0.2058(2) 0.0231 1.0000 Uani . . . . . . .
C41 C 0.8543(2) 0.82961(10) 0.1889(2) 0.0221 1.0000 Uani . . . . . . .
C42 C 0.8989(2) 0.78926(10) 0.1657(2) 0.0194 1.0000 Uani . . . . . . .
C43 C 0.6646(2) 0.70919(10) 0.1598(2) 0.0199 1.0000 Uani D . . . . . .
C44 C 0.7044(3) 0.87723(11) 0.2291(3) 0.0316 1.0000 Uani . . . . . . .
C45 C 1.0112(2) 0.78811(10) 0.1483(2) 0.0247 1.0000 Uani . . . . . . .
H11 H 0.6958 0.5352 0.2584 0.0245 1.0000 Uiso . . . . . . .
H21 H 0.5555 0.5605 0.3362 0.0425 1.0000 Uiso . . . . . . .
H22 H 0.5904 0.5095 0.3527 0.0429 1.0000 Uiso . . . . . . .
H23 H 0.4798 0.5230 0.2702 0.0429 1.0000 Uiso . . . . . . .
H31 H 0.6213 0.4685 0.1802 0.0384 1.0000 Uiso . . . . . . .
H32 H 0.5217 0.4943 0.1066 0.0373 1.0000 Uiso . . . . . . .
H33 H 0.6377 0.5003 0.0924 0.0383 1.0000 Uiso . . . . . . .
H41 H 0.4731 0.5793 -0.0011 0.0228 1.0000 Uiso . . . . . . .
H51 H 0.3685 0.6453 -0.0273 0.0344 1.0000 Uiso . . . . . . .
H52 H 0.4132 0.6596 0.0869 0.0342 1.0000 Uiso . . . . . . .
H53 H 0.4866 0.6620 0.0104 0.0341 1.0000 Uiso . . . . . . .
H61 H 0.3857 0.5406 0.1052 0.0426 1.0000 Uiso . . . . . . .
H62 H 0.3069 0.5791 0.0513 0.0431 1.0000 Uiso . . . . . . .
H63 H 0.3750 0.5856 0.1626 0.0443 1.0000 Uiso . . . . . . .
H91 H 0.8788 0.4922 -0.0418 0.0253 1.0000 Uiso . . . . . . .
H111 H 0.6436 0.5626 -0.2440 0.0242 1.0000 Uiso . . . . . . .
H131 H 0.9096 0.5545 0.1679 0.0343 1.0000 Uiso . . . . . . .
H132 H 0.8308 0.5148 0.1744 0.0350 1.0000 Uiso . . . . . . .
H133 H 0.9290 0.5063 0.1310 0.0354 1.0000 Uiso . . . . . . .
H141 H 0.7561 0.4646 -0.2451 0.0427 1.0000 Uiso . . . . . . .
H142 H 0.7427 0.5076 -0.3113 0.0420 1.0000 Uiso . . . . . . .
H143 H 0.8580 0.4943 -0.2436 0.0421 1.0000 Uiso . . . . . . .
H151 H 0.5983 0.6432 -0.0712 0.0342 1.0000 Uiso . . . . . . .
H152 H 0.5936 0.6353 -0.1853 0.0351 1.0000 Uiso . . . . . . .
H153 H 0.5097 0.6105 -0.1384 0.0350 1.0000 Uiso . . . . . . .
H161 H 0.9144 0.6893 0.5339 0.0325 1.0000 Uiso . . . . . . .
H171 H 0.7402 0.7434 0.4082 0.0458 1.0000 Uiso . . . . . . .
H172 H 0.8448 0.7350 0.3753 0.0460 1.0000 Uiso . . . . . . .
H173 H 0.8503 0.7608 0.4770 0.0467 1.0000 Uiso . . . . . . .
H181 H 0.7995 0.6704 0.6330 0.0528 1.0000 Uiso . . . . . . .
H182 H 0.6971 0.6969 0.5536 0.0526 1.0000 Uiso . . . . . . .
H183 H 0.8021 0.7246 0.6203 0.0529 1.0000 Uiso . . . . . . .
H191 H 0.7715 0.5686 0.4467 0.0257 1.0000 Uiso . . . . . . .
H201 H 0.6154 0.6089 0.4804 0.0452 1.0000 Uiso . . . . . . .
H202 H 0.6544 0.5644 0.5441 0.0460 1.0000 Uiso . . . . . . .
H203 H 0.6880 0.6137 0.5911 0.0464 1.0000 Uiso . . . . . . .
H211 H 0.8846 0.6097 0.6368 0.0392 1.0000 Uiso . . . . . . .
H212 H 0.8781 0.5583 0.6149 0.0388 1.0000 Uiso . . . . . . .
H213 H 0.9500 0.5893 0.5644 0.0387 1.0000 Uiso . . . . . . .
H241 H 1.1617 0.5315 0.4500 0.0272 1.0000 Uiso . . . . . . .
H261 H 1.2523 0.6620 0.4608 0.0288 1.0000 Uiso . . . . . . .
H281 H 0.9345 0.5270 0.4510 0.0318 1.0000 Uiso . . . . . . .
H282 H 0.9763 0.5110 0.3556 0.0323 1.0000 Uiso . . . . . . .
H283 H 0.8822 0.5452 0.3392 0.0314 1.0000 Uiso . . . . . . .
H291 H 1.3918 0.6044 0.4787 0.0543 1.0000 Uiso . . . . . . .
H292 H 1.3597 0.5543 0.4613 0.0549 1.0000 Uiso . . . . . . .
H293 H 1.3696 0.5760 0.5653 0.0548 1.0000 Uiso . . . . . . .
H301 H 1.0477 0.7156 0.4642 0.0354 1.0000 Uiso . . . . . . .
H302 H 1.0033 0.7100 0.3438 0.0359 1.0000 Uiso . . . . . . .
H303 H 1.1275 0.7188 0.3944 0.0359 1.0000 Uiso . . . . . . .
H311 H 1.1034 0.6863 0.2117 0.0277 1.0000 Uiso . . . . . . .
H321 H 1.0926 0.6083 0.2195 0.0421 1.0000 Uiso . . . . . . .
H322 H 1.2054 0.6204 0.2064 0.0415 1.0000 Uiso . . . . . . .
H323 H 1.1127 0.6031 0.1086 0.0419 1.0000 Uiso . . . . . . .
H331 H 1.2361 0.6931 0.1242 0.0450 1.0000 Uiso . . . . . . .
H332 H 1.1358 0.7221 0.0621 0.0458 1.0000 Uiso . . . . . . .
H333 H 1.1549 0.6743 0.0200 0.0462 1.0000 Uiso . . . . . . .
H341 H 0.9713 0.7106 -0.0519 0.0268 1.0000 Uiso . . . . . . .
H351 H 0.8755 0.6263 -0.1169 0.0547 1.0000 Uiso . . . . . . .
H352 H 0.9999 0.6334 -0.0830 0.0542 1.0000 Uiso . . . . . . .
H353 H 0.9313 0.6577 -0.1799 0.0551 1.0000 Uiso . . . . . . .
H361 H 0.7980 0.7363 -0.0522 0.0476 1.0000 Uiso . . . . . . .
H362 H 0.7902 0.7188 -0.1645 0.0480 1.0000 Uiso . . . . . . .
H363 H 0.7444 0.6884 -0.0886 0.0468 1.0000 Uiso . . . . . . .
H391 H 0.6163 0.7937 0.2058 0.0262 1.0000 Uiso . . . . . . .
H411 H 0.8962 0.8563 0.1925 0.0262 1.0000 Uiso . . . . . . .
H431 H 0.600(2) 0.7152(5) 0.168(3) 0.024(9) 1.0000 Uiso D . . . . . .
H432 H 0.657(3) 0.6984(9) 0.093(3) 0.037(11) 1.0000 Uiso D . . . . . .
H441 H 0.7595 0.8949 0.2751 0.0476 1.0000 Uiso . . . . . . .
H442 H 0.6444 0.8731 0.2578 0.0479 1.0000 Uiso . . . . . . .
H443 H 0.6793 0.8936 0.1666 0.0477 1.0000 Uiso . . . . . . .
H451 H 1.0395 0.8185 0.1515 0.0376 1.0000 Uiso . . . . . . .
H452 H 1.0064 0.7750 0.0820 0.0366 1.0000 Uiso . . . . . . .
H453 H 1.0591 0.7701 0.2024 0.0364 1.0000 Uiso . . . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
I1 0.02264(9) 0.03612(11) 0.03039(10) -0.00433(8) 0.01485(7) 0.00543(8)
Zr1 0.01196(10) 0.01420(11) 0.01374(11) -0.00035(9) 0.00426(8) -0.00053(8)
Co1 0.01466(15) 0.01663(17) 0.01886(17) -0.00229(13) 0.00747(13) -0.00012(13)
P1 0.0133(3) 0.0154(3) 0.0172(3) -0.0013(2) 0.0050(2) -0.0011(2)
P2 0.0187(3) 0.0184(3) 0.0146(3) -0.0017(2) 0.0066(2) -0.0018(2)
P3 0.0155(3) 0.0185(3) 0.0189(3) 0.0012(2) 0.0078(2) 0.0000(2)
N1 0.0137(9) 0.0182(10) 0.0155(10) -0.0026(8) 0.0050(8) -0.0008(8)
N2 0.013(1) 0.0215(11) 0.0143(10) 0.0005(8) 0.0032(8) -0.0015(8)
N3 0.0151(10) 0.0174(11) 0.0186(10) 0.0008(8) 0.0053(8) -0.0005(8)
C1 0.0198(12) 0.0178(12) 0.0221(13) 0.0005(10) 0.0057(10) -0.0021(10)
C2 0.0332(16) 0.0281(16) 0.0268(15) 0.0026(12) 0.0114(12) -0.0067(12)
C3 0.0265(14) 0.0172(13) 0.0327(16) -0.0019(11) 0.0089(12) -0.0018(11)
C4 0.0134(11) 0.0211(13) 0.0235(13) -0.0020(10) 0.0049(10) -0.0010(9)
C5 0.0174(12) 0.0241(14) 0.0264(14) -0.0026(11) 0.0033(10) 0.0030(10)
C6 0.0170(13) 0.0314(16) 0.0399(18) 0.0003(13) 0.0087(12) -0.0035(11)
C7 0.0157(11) 0.0176(12) 0.0168(11) -0.0019(9) 0.0063(9) -0.0026(9)
C8 0.0159(11) 0.0206(13) 0.0186(12) -0.0005(10) 0.0056(9) -0.0001(10)
C9 0.0206(12) 0.0213(13) 0.0236(13) -0.0024(11) 0.0095(10) 0.0012(10)
C10 0.0251(13) 0.0215(13) 0.0205(13) -0.0037(10) 0.0115(11) -0.0053(11)
C11 0.0220(13) 0.0231(13) 0.0158(12) 0.0003(10) 0.0054(10) -0.0045(10)
C12 0.0158(11) 0.0193(12) 0.0189(12) 0.0017(10) 0.0049(9) -0.0021(9)
C13 0.0195(12) 0.0275(15) 0.0217(13) -0.0012(11) 0.0037(10) 0.0069(11)
C14 0.0387(17) 0.0272(15) 0.0239(14) -0.0050(12) 0.0163(13) 0.0012(13)
C15 0.0245(14) 0.0252(14) 0.0216(13) 0.0052(11) 0.0062(11) 0.0052(11)
C16 0.0380(17) 0.0234(14) 0.0194(13) -0.0034(11) 0.0086(12) -0.0050(12)
C17 0.048(2) 0.0224(15) 0.0261(15) -0.0059(12) 0.0148(14) -0.0055(13)
C18 0.049(2) 0.0335(18) 0.0301(17) -0.0036(14) 0.0165(15) 0.0056(15)
C19 0.0241(13) 0.0256(14) 0.0181(12) 0.0019(10) 0.0095(10) -0.0024(11)
C20 0.0281(15) 0.0444(19) 0.0241(15) 0.0025(13) 0.0136(12) -0.0060(14)
C21 0.0314(15) 0.0288(15) 0.0178(13) 0.0039(11) 0.0075(11) 0.0026(12)
C22 0.0151(11) 0.0259(14) 0.0125(11) 0.0010(10) 0.0036(9) -0.0004(10)
C23 0.0178(12) 0.0252(13) 0.0137(11) -0.0001(10) 0.0053(9) -0.0016(10)
C24 0.0201(13) 0.0277(15) 0.0181(12) 0.0026(11) 0.0050(10) 0.0031(11)
C25 0.0175(12) 0.0368(17) 0.0202(13) 0.0010(12) 0.0042(10) 0.0004(11)
C26 0.0166(12) 0.0352(16) 0.0202(13) -0.0010(11) 0.0035(10) -0.0048(11)
C27 0.0177(12) 0.0264(14) 0.0151(11) -0.0004(10) 0.0034(9) -0.0033(10)
C28 0.0222(13) 0.0203(13) 0.0207(13) 0.0019(10) 0.0041(10) -0.0008(10)
C29 0.0192(14) 0.045(2) 0.0413(19) 0.0007(16) 0.0056(13) 0.0043(13)
C30 0.0214(13) 0.0267(14) 0.0221(13) -0.0020(11) 0.0037(10) -0.0071(11)
C31 0.0154(12) 0.0260(14) 0.0262(14) 0.0013(11) 0.0086(10) 0.0001(10)
C32 0.0244(14) 0.0296(16) 0.0337(16) 0.0053(13) 0.0131(12) 0.0076(12)
C33 0.0183(13) 0.0353(17) 0.0429(18) 0.0082(14) 0.0138(13) 0.0005(12)
C34 0.0229(13) 0.0288(15) 0.0193(13) 0.0014(11) 0.0086(10) -0.0026(11)
C35 0.045(2) 0.044(2) 0.0263(16) -0.0090(15) 0.0157(14) 0.0000(16)
C36 0.0254(15) 0.046(2) 0.0237(15) 0.0089(14) 0.0049(12) 0.0018(14)
C37 0.0180(12) 0.0167(12) 0.0164(11) 0.0014(9) 0.0057(9) 0.0003(9)
C38 0.0184(12) 0.0178(12) 0.0189(12) 0.0018(10) 0.0047(10) 0.0011(10)
C39 0.0213(13) 0.0200(13) 0.0239(13) -0.0002(11) 0.0069(10) 0.0026(10)
C40 0.0274(14) 0.0180(13) 0.0217(13) -0.0007(10) 0.0033(11) 0.0020(11)
C41 0.0247(13) 0.0185(13) 0.0215(13) -0.0001(10) 0.0041(10) -0.0034(10)
C42 0.0192(12) 0.0215(13) 0.0169(12) 0.0020(10) 0.0040(9) -0.0025(10)
C43 0.0109(11) 0.0319(15) 0.0178(12) 0.0018(11) 0.0054(9) 0.0005(10)
C44 0.0360(17) 0.0194(14) 0.0403(18) -0.0032(13) 0.0119(14) 0.0038(12)
C45 0.0228(13) 0.0228(14) 0.0294(15) -0.0010(11) 0.0087(11) -0.0062(11)
_refine_ls_extinction_method None
_oxford_refine_ls_scale 0.067419(6)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
I1 . Co1 . 2.5647(4) yes
Zr1 . Co1 . 2.5562(4) yes
Zr1 . P1 . 2.8151(7) yes
Zr1 . P2 . 2.8522(7) yes
Zr1 . P3 . 2.6897(7) yes
Zr1 . N1 . 2.135(2) yes
Zr1 . N2 . 2.136(2) yes
Zr1 . N3 . 2.099(2) yes
Zr1 . C43 . 2.386(3) yes
Co1 . P1 . 2.3279(8) yes
Co1 . P2 . 2.2986(8) yes
Co1 . C43 . 2.325(3) yes
P1 . N1 . 1.690(2) yes
P1 . C1 . 1.855(3) yes
P1 . C4 . 1.860(3) yes
P2 . N2 . 1.678(2) yes
P2 . C16 . 1.848(3) yes
P2 . C19 . 1.862(3) yes
P3 . N3 . 1.663(2) yes
P3 . C31 . 1.867(3) yes
P3 . C34 . 1.850(3) yes
N1 . C7 . 1.430(3) yes
N2 . C22 . 1.439(3) yes
N3 . C37 . 1.415(3) yes
C1 . C2 . 1.545(4) yes
C1 . C3 . 1.533(4) yes
C1 . H11 . 0.975 no
C2 . H21 . 0.973 no
C2 . H22 . 0.956 no
C2 . H23 . 0.960 no
C3 . H31 . 0.970 no
C3 . H32 . 0.949 no
C3 . H33 . 0.956 no
C4 . C5 . 1.523(4) yes
C4 . C6 . 1.526(4) yes
C4 . H41 . 0.978 no
C5 . H51 . 0.938 no
C5 . H52 . 0.968 no
C5 . H53 . 0.951 no
C6 . H61 . 0.976 no
C6 . H62 . 0.957 no
C6 . H63 . 0.930 no
C7 . C8 . 1.413(4) yes
C7 . C12 . 1.410(4) yes
C8 . C9 . 1.391(4) yes
C8 . C13 . 1.493(4) yes
C9 . C10 . 1.394(4) yes
C9 . H91 . 0.935 no
C10 . C11 . 1.379(4) yes
C10 . C14 . 1.504(4) yes
C11 . C12 . 1.402(4) yes
C11 . H111 . 0.937 no
C12 . C15 . 1.505(4) yes
C13 . H131 . 0.951 no
C13 . H132 . 0.958 no
C13 . H133 . 0.938 no
C14 . H141 . 0.950 no
C14 . H142 . 0.943 no
C14 . H143 . 0.949 no
C15 . H151 . 0.949 no
C15 . H152 . 0.949 no
C15 . H153 . 0.964 no
C16 . C17 . 1.538(5) yes
C16 . C18 . 1.517(5) yes
C16 . H161 . 1.006 no
C17 . H171 . 0.942 no
C17 . H172 . 0.952 no
C17 . H173 . 0.946 no
C18 . H181 . 0.987 no
C18 . H182 . 0.987 no
C18 . H183 . 0.991 no
C19 . C20 . 1.533(4) yes
C19 . C21 . 1.537(4) yes
C19 . H191 . 0.979 no
C20 . H201 . 0.952 no
C20 . H202 . 0.971 no
C20 . H203 . 0.953 no
C21 . H211 . 0.945 no
C21 . H212 . 0.964 no
C21 . H213 . 0.966 no
C22 . C23 . 1.410(4) yes
C22 . C27 . 1.411(4) yes
C23 . C24 . 1.396(4) yes
C23 . C28 . 1.505(4) yes
C24 . C25 . 1.390(4) yes
C24 . H241 . 0.936 no
C25 . C26 . 1.380(5) yes
C25 . C29 . 1.513(4) yes
C26 . C27 . 1.396(4) yes
C26 . H261 . 0.931 no
C27 . C30 . 1.505(4) yes
C28 . H281 . 0.972 no
C28 . H282 . 0.962 no
C28 . H283 . 0.951 no
C29 . H291 . 0.943 no
C29 . H292 . 0.930 no
C29 . H293 . 0.924 no
C30 . H301 . 0.960 no
C30 . H302 . 0.960 no
C30 . H303 . 0.947 no
C31 . C32 . 1.520(4) yes
C31 . C33 . 1.528(4) yes
C31 . H311 . 0.987 no
C32 . H321 . 0.957 no
C32 . H322 . 0.956 no
C32 . H323 . 0.974 no
C33 . H331 . 0.960 no
C33 . H332 . 0.952 no
C33 . H333 . 0.962 no
C34 . C35 . 1.529(5) yes
C34 . C36 . 1.519(4) yes
C34 . H341 . 0.964 no
C35 . H351 . 0.939 no
C35 . H352 . 0.938 no
C35 . H353 . 0.938 no
C36 . H361 . 0.961 no
C36 . H362 . 0.972 no
C36 . H363 . 0.970 no
C37 . C38 . 1.415(4) yes
C37 . C42 . 1.398(4) yes
C38 . C39 . 1.397(4) yes
C38 . C43 . 1.468(4) yes
C39 . C40 . 1.395(4) yes
C39 . H391 . 0.951 no
C40 . C41 . 1.394(4) yes
C40 . C44 . 1.510(4) yes
C41 . C42 . 1.387(4) yes
C41 . H411 . 0.941 no
C42 . C45 . 1.500(4) yes
C43 . H431 . 0.87(2) no
C43 . H432 . 0.92(3) no
C44 . H441 . 0.946 no
C44 . H442 . 0.948 no
C44 . H443 . 0.941 no
C45 . H451 . 0.960 no
C45 . H452 . 0.954 no
C45 . H453 . 0.963 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Co1 . Zr1 . P1 . 51.089(17) yes
Co1 . Zr1 . P2 . 49.934(17) yes
P1 . Zr1 . P2 . 84.03(2) yes
Co1 . Zr1 . P3 . 159.89(2) yes
P1 . Zr1 . P3 . 135.14(2) yes
P2 . Zr1 . P3 . 138.49(2) yes
Co1 . Zr1 . N1 . 87.39(6) yes
P1 . Zr1 . N1 . 36.79(6) yes
P2 . Zr1 . N1 . 115.39(6) yes
P3 . Zr1 . N1 . 99.18(6) yes
Co1 . Zr1 . N2 . 85.37(6) yes
P1 . Zr1 . N2 . 105.78(6) yes
P2 . Zr1 . N2 . 35.80(6) yes
P3 . Zr1 . N2 . 106.94(6) yes
N1 . Zr1 . N2 . 120.72(9) yes
Co1 . Zr1 . N3 . 123.98(6) yes
P1 . Zr1 . N3 . 147.79(6) yes
P2 . Zr1 . N3 . 117.76(6) yes
P3 . Zr1 . N3 . 38.20(6) yes
N1 . Zr1 . N3 . 126.61(9) yes
Co1 . Zr1 . C43 . 56.01(6) yes
P1 . Zr1 . C43 . 83.53(7) yes
P2 . Zr1 . C43 . 91.77(7) yes
P3 . Zr1 . C43 . 103.95(7) yes
N1 . Zr1 . C43 . 101.03(9) yes
N2 . Zr1 . N3 . 105.27(9) yes
N2 . Zr1 . C43 . 121.73(9) yes
N3 . Zr1 . C43 . 73.00(9) yes
I1 . Co1 . Zr1 . 164.080(18) yes
I1 . Co1 . P1 . 118.61(2) yes
Zr1 . Co1 . P1 . 70.21(2) yes
I1 . Co1 . P2 . 113.84(2) yes
Zr1 . Co1 . P2 . 71.74(2) yes
P1 . Co1 . P2 . 110.15(3) yes
I1 . Co1 . C43 . 106.24(7) yes
Zr1 . Co1 . C43 . 58.29(7) yes
P1 . Co1 . C43 . 96.78(8) yes
P2 . Co1 . C43 . 109.44(7) yes
Zr1 . P1 . Co1 . 58.696(18) yes
Zr1 . P1 . N1 . 49.14(8) yes
Co1 . P1 . N1 . 107.14(8) yes
Zr1 . P1 . C1 . 118.24(9) yes
Co1 . P1 . C1 . 114.92(9) yes
N1 . P1 . C1 . 106.26(12) yes
Zr1 . P1 . C4 . 133.56(9) yes
Co1 . P1 . C4 . 111.65(9) yes
N1 . P1 . C4 . 109.72(12) yes
C1 . P1 . C4 . 106.98(13) yes
Zr1 . P2 . Co1 . 58.328(18) yes
Zr1 . P2 . N2 . 48.13(8) yes
Co1 . P2 . N2 . 105.91(8) yes
Zr1 . P2 . C16 . 121.06(10) yes
Co1 . P2 . C16 . 115.82(11) yes
N2 . P2 . C16 . 107.91(13) yes
Zr1 . P2 . C19 . 132.56(9) yes
Co1 . P2 . C19 . 113.09(10) yes
N2 . P2 . C19 . 109.09(12) yes
C16 . P2 . C19 . 104.84(13) yes
Zr1 . P3 . N3 . 51.29(8) yes
Zr1 . P3 . C31 . 123.32(9) yes
N3 . P3 . C31 . 113.53(12) yes
Zr1 . P3 . C34 . 130.98(9) yes
N3 . P3 . C34 . 111.68(13) yes
C31 . P3 . C34 . 105.69(13) yes
P1 . N1 . Zr1 . 94.07(10) yes
P1 . N1 . C7 . 131.39(18) yes
Zr1 . N1 . C7 . 134.51(17) yes
P2 . N2 . Zr1 . 96.07(10) yes
P2 . N2 . C22 . 130.96(18) yes
Zr1 . N2 . C22 . 132.84(17) yes
P3 . N3 . Zr1 . 90.52(10) yes
P3 . N3 . C37 . 145.95(19) yes
Zr1 . N3 . C37 . 120.98(16) yes
P1 . C1 . C2 . 114.2(2) yes
P1 . C1 . C3 . 115.3(2) yes
C2 . C1 . C3 . 111.6(2) yes
P1 . C1 . H11 . 103.7 no
C2 . C1 . H11 . 104.2 no
C3 . C1 . H11 . 106.5 no
C1 . C2 . H21 . 108.4 no
C1 . C2 . H22 . 110.5 no
H21 . C2 . H22 . 108.4 no
C1 . C2 . H23 . 111.2 no
H21 . C2 . H23 . 108.1 no
H22 . C2 . H23 . 110.2 no
C1 . C3 . H31 . 110.3 no
C1 . C3 . H32 . 110.8 no
H31 . C3 . H32 . 109.0 no
C1 . C3 . H33 . 110.5 no
H31 . C3 . H33 . 108.3 no
H32 . C3 . H33 . 107.9 no
P1 . C4 . C5 . 111.98(19) yes
P1 . C4 . C6 . 112.9(2) yes
C5 . C4 . C6 . 107.9(2) yes
P1 . C4 . H41 . 107.2 no
C5 . C4 . H41 . 109.4 no
C6 . C4 . H41 . 107.3 no
C4 . C5 . H51 . 111.2 no
C4 . C5 . H52 . 109.3 no
H51 . C5 . H52 . 106.9 no
C4 . C5 . H53 . 113.2 no
H51 . C5 . H53 . 107.1 no
H52 . C5 . H53 . 109.0 no
C4 . C6 . H61 . 112.9 no
C4 . C6 . H62 . 110.2 no
H61 . C6 . H62 . 106.4 no
C4 . C6 . H63 . 111.3 no
H61 . C6 . H63 . 109.5 no
H62 . C6 . H63 . 106.2 no
N1 . C7 . C8 . 119.6(2) yes
N1 . C7 . C12 . 122.3(2) yes
C8 . C7 . C12 . 117.9(2) yes
C7 . C8 . C9 . 120.2(2) yes
C7 . C8 . C13 . 121.5(2) yes
C9 . C8 . C13 . 118.3(2) yes
C8 . C9 . C10 . 122.3(3) yes
C8 . C9 . H91 . 118.2 no
C10 . C9 . H91 . 119.6 no
C9 . C10 . C11 . 117.0(3) yes
C9 . C10 . C14 . 121.2(3) yes
C11 . C10 . C14 . 121.8(3) yes
C10 . C11 . C12 . 123.0(3) yes
C10 . C11 . H111 . 118.8 no
C12 . C11 . H111 . 118.2 no
C7 . C12 . C11 . 119.4(2) yes
C7 . C12 . C15 . 123.2(2) yes
C11 . C12 . C15 . 117.4(2) yes
C8 . C13 . H131 . 110.7 no
C8 . C13 . H132 . 109.8 no
H131 . C13 . H132 . 109.0 no
C8 . C13 . H133 . 110.0 no
H131 . C13 . H133 . 109.7 no
H132 . C13 . H133 . 107.6 no
C10 . C14 . H141 . 110.8 no
C10 . C14 . H142 . 109.9 no
H141 . C14 . H142 . 107.6 no
C10 . C14 . H143 . 110.3 no
H141 . C14 . H143 . 109.6 no
H142 . C14 . H143 . 108.6 no
C12 . C15 . H151 . 110.9 no
C12 . C15 . H152 . 109.7 no
H151 . C15 . H152 . 107.2 no
C12 . C15 . H153 . 111.0 no
H151 . C15 . H153 . 109.1 no
H152 . C15 . H153 . 108.9 no
P2 . C16 . C17 . 109.5(2) yes
P2 . C16 . C18 . 115.3(2) yes
C17 . C16 . C18 . 109.1(3) yes
P2 . C16 . H161 . 109.8 no
C17 . C16 . H161 . 108.5 no
C18 . C16 . H161 . 104.3 no
C16 . C17 . H171 . 111.1 no
C16 . C17 . H172 . 112.0 no
H171 . C17 . H172 . 107.2 no
C16 . C17 . H173 . 109.7 no
H171 . C17 . H173 . 108.0 no
H172 . C17 . H173 . 108.7 no
C16 . C18 . H181 . 111.4 no
C16 . C18 . H182 . 110.3 no
H181 . C18 . H182 . 110.9 no
C16 . C18 . H183 . 107.4 no
H181 . C18 . H183 . 108.7 no
H182 . C18 . H183 . 108.1 no
P2 . C19 . C20 . 114.6(2) yes
P2 . C19 . C21 . 114.1(2) yes
C20 . C19 . C21 . 110.5(2) yes
P2 . C19 . H191 . 103.5 no
C20 . C19 . H191 . 105.3 no
C21 . C19 . H191 . 107.9 no
C19 . C20 . H201 . 110.7 no
C19 . C20 . H202 . 111.2 no
H201 . C20 . H202 . 109.0 no
C19 . C20 . H203 . 108.8 no
H201 . C20 . H203 . 105.5 no
H202 . C20 . H203 . 111.6 no
C19 . C21 . H211 . 109.9 no
C19 . C21 . H212 . 109.0 no
H211 . C21 . H212 . 107.4 no
C19 . C21 . H213 . 112.9 no
H211 . C21 . H213 . 109.1 no
H212 . C21 . H213 . 108.4 no
N2 . C22 . C23 . 119.9(2) yes
N2 . C22 . C27 . 120.9(2) yes
C23 . C22 . C27 . 118.9(2) yes
C22 . C23 . C24 . 119.4(3) yes
C22 . C23 . C28 . 122.8(2) yes
C24 . C23 . C28 . 117.8(3) yes
C23 . C24 . C25 . 122.3(3) yes
C23 . C24 . H241 . 117.2 no
C25 . C24 . H241 . 120.5 no
C24 . C25 . C26 . 117.6(3) yes
C24 . C25 . C29 . 121.1(3) yes
C26 . C25 . C29 . 121.3(3) yes
C25 . C26 . C27 . 122.6(3) yes
C25 . C26 . H261 . 118.8 no
C27 . C26 . H261 . 118.6 no
C22 . C27 . C26 . 119.2(3) yes
C22 . C27 . C30 . 123.1(2) yes
C26 . C27 . C30 . 117.7(3) yes
C23 . C28 . H281 . 110.5 no
C23 . C28 . H282 . 110.6 no
H281 . C28 . H282 . 109.8 no
C23 . C28 . H283 . 112.3 no
H281 . C28 . H283 . 107.6 no
H282 . C28 . H283 . 105.9 no
C25 . C29 . H291 . 109.7 no
C25 . C29 . H292 . 111.4 no
H291 . C29 . H292 . 109.6 no
C25 . C29 . H293 . 109.0 no
H291 . C29 . H293 . 108.7 no
H292 . C29 . H293 . 108.4 no
C27 . C30 . H301 . 110.3 no
C27 . C30 . H302 . 111.2 no
H301 . C30 . H302 . 108.6 no
C27 . C30 . H303 . 109.0 no
H301 . C30 . H303 . 109.2 no
H302 . C30 . H303 . 108.5 no
P3 . C31 . C32 . 109.1(2) yes
P3 . C31 . C33 . 117.3(2) yes
C32 . C31 . C33 . 110.1(2) yes
P3 . C31 . H311 . 104.5 no
C32 . C31 . H311 . 106.4 no
C33 . C31 . H311 . 108.8 no
C31 . C32 . H321 . 111.3 no
C31 . C32 . H322 . 110.5 no
H321 . C32 . H322 . 105.8 no
C31 . C32 . H323 . 109.8 no
H321 . C32 . H323 . 109.8 no
H322 . C32 . H323 . 109.6 no
C31 . C33 . H331 . 108.3 no
C31 . C33 . H332 . 110.2 no
H331 . C33 . H332 . 109.5 no
C31 . C33 . H333 . 108.7 no
H331 . C33 . H333 . 110.8 no
H332 . C33 . H333 . 109.3 no
P3 . C34 . C35 . 108.6(2) yes
P3 . C34 . C36 . 111.1(2) yes
C35 . C34 . C36 . 112.0(3) yes
P3 . C34 . H341 . 107.9 no
C35 . C34 . H341 . 107.2 no
C36 . C34 . H341 . 109.9 no
C34 . C35 . H351 . 109.6 no
C34 . C35 . H352 . 111.2 no
H351 . C35 . H352 . 108.6 no
C34 . C35 . H353 . 108.0 no
H351 . C35 . H353 . 110.9 no
H352 . C35 . H353 . 108.5 no
C34 . C36 . H361 . 108.1 no
C34 . C36 . H362 . 110.7 no
H361 . C36 . H362 . 108.0 no
C34 . C36 . H363 . 111.2 no
H361 . C36 . H363 . 110.0 no
H362 . C36 . H363 . 108.7 no
N3 . C37 . C38 . 113.1(2) yes
N3 . C37 . C42 . 126.2(2) yes
C38 . C37 . C42 . 120.6(2) yes
C37 . C38 . C39 . 119.1(2) yes
C37 . C38 . C43 . 118.5(2) yes
C39 . C38 . C43 . 122.4(2) yes
C38 . C39 . C40 . 121.1(3) yes
C38 . C39 . H391 . 118.9 no
C40 . C39 . H391 . 119.9 no
C39 . C40 . C41 . 118.0(3) yes
C39 . C40 . C44 . 120.7(3) yes
C41 . C40 . C44 . 121.3(3) yes
C40 . C41 . C42 . 123.1(3) yes
C40 . C41 . H411 . 118.9 no
C42 . C41 . H411 . 118.0 no
C37 . C42 . C41 . 118.0(2) yes
C37 . C42 . C45 . 121.0(3) yes
C41 . C42 . C45 . 121.0(3) yes
Zr1 . C43 . C38 . 105.84(17) yes
Zr1 . C43 . Co1 . 65.70(8) yes
C38 . C43 . Co1 . 133.89(19) yes
Zr1 . C43 . H431 . 138.4(15) no
C38 . C43 . H431 . 108.9(9) no
Co1 . C43 . H431 . 73.8(18) no
Zr1 . C43 . H432 . 80(2) no
C38 . C43 . H432 . 108.8(9) no
Co1 . C43 . H432 . 113.4(12) no
H431 . C43 . H432 . 109(3) no
C40 . C44 . H441 . 110.9 no
C40 . C44 . H442 . 111.6 no
H441 . C44 . H442 . 109.6 no
C40 . C44 . H443 . 108.7 no
H441 . C44 . H443 . 107.5 no
H442 . C44 . H443 . 108.4 no
C42 . C45 . H451 . 109.2 no
C42 . C45 . H452 . 109.5 no
H451 . C45 . H452 . 110.2 no
C42 . C45 . H453 . 108.7 no
H451 . C45 . H453 . 109.4 no
H452 . C45 . H453 . 109.8 no
#===END
data_7
_database_code_depnum_ccdc_archive 'CCDC 776342'
#TrackingRef '- combined_rev.cif'
_audit_creation_date 10-02-15
_audit_creation_method CRYSTALS_ver_14.01
# start Validation Reply Form: One Alert B issue
_vrf_PLAT222_7
;
PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 4.70 Ratio
RESPONSE: The molecule is 7:1 disordered as a mixed Cl/I complex. While
the I/Cl disorder was modeled successfully, there were large peaks 1.5 -
2.0 e- near the Zr and Cl atoms, and several of the mesityl rings had
large in-plane ellipsoid excursions, likely indicative of disorder.
Attempts to model the other disorder (Zr, Co, mesityl) invariably failed.
The large range of H atom Uiso parameters arises from the ratio of H293
on a disordered mesityl group to isopropyl methine H atom H311.
;
# end Validation Reply Form
_oxford_structure_analysis_title 'CMT36_0m in P-1'
_chemical_name_systematic ?
_chemical_melting_point ?
_cell_length_a 12.2227(5)
_cell_length_b 14.2597(7)
_cell_length_c 18.3302(9)
_cell_angle_alpha 77.154(3)
_cell_angle_beta 82.246(2)
_cell_angle_gamma 79.036(2)
_cell_volume 3043.6(2)
_symmetry_cell_setting Triclinic
_symmetry_space_group_name_H-M 'P -1 '
_symmetry_space_group_name_Hall ?
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Co 0.3494 0.9721 12.2841 4.2791 7.3409 0.2784 4.0034 13.5359 2.3488 71.1692
1.0118 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Zr -2.9673 0.5597 17.8765 1.2762 10.9480 11.9160 5.4173 0.1176 3.6572 87.6627
2.0693 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
I -0.4742 1.8119 20.1472 4.3470 18.9949 0.3814 7.5138 27.7660 2.2735 66.8776
4.0712 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
_cell_formula_units_Z 2
# Given Formula = C50 H86 Cl0.85 Co1 I0.15 N3 P3 Zr1
# Dc = 1.11 Fooo = 1082.66 Mu = 6.65 M = 1021.33
# Found Formula = C50 H86 Cl0.85 Co1 I0.15 N3 P3 Zr1
# Dc = 1.11 FOOO = 1082.66 Mu = 6.65 M = 1021.32
_chemical_formula_sum 'C50 H86 Cl0.85 Co1 I0.15 N3 P3 Zr1'
_chemical_formula_moiety 'C50 H86 Cl0.85 Co1 I0.15 N3 P3 Zr1'
_chemical_compound_source ?
_chemical_formula_weight 1021.32
_cell_measurement_reflns_used 9908
_cell_measurement_theta_min 3
_cell_measurement_theta_max 30
_cell_measurement_temperature 120
_exptl_crystal_description 'prism fragment'
_exptl_crystal_colour green
_exptl_crystal_size_min 0.319
_exptl_crystal_size_mid 0.403
_exptl_crystal_size_max 0.583
_exptl_crystal_density_diffrn 1.114
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 1082.664
_exptl_absorpt_coefficient_mu 0.665
# Sheldrick geometric approximatio 0.76 0.81
_exptl_absorpt_correction_type numerical
_exptl_absorpt_process_details
;
Analytical Absorption (De Meulenaer & Tompa, 1965)
;
_exptl_absorpt_correction_T_min 0.77
_exptl_absorpt_correction_T_max 0.81
_diffrn_measurement_device-type 'Bruker Kappa Apex2'
_diffrn_measurement_device Area
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_measurement_method '\f & \w scans'
# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection 'Apex2 (Bruker AXS, 2006)'
_computing_cell_refinement 'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction 'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution 'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material 'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics 'CAMERON (Watkin et al., 1996)'
_diffrn_standards_interval_time .
_diffrn_standards_interval_count .
_diffrn_standards_number 0
_diffrn_standards_decay_% ?
_diffrn_ambient_temperature 120
_diffrn_reflns_number 17679
_reflns_number_total 17679
_diffrn_reflns_av_R_equivalents 0.049
# Number of reflections without Friedels Law is 0
# Number of reflections with Friedels Law is 17679
# Theoretical number of reflections is about 35736
_diffrn_reflns_theta_min 2.067
_diffrn_reflns_theta_max 30.070
_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full 29.468
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_k_min -19
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_limit_l_max 25
_reflns_limit_h_min -16
_reflns_limit_h_max 17
_reflns_limit_k_min -19
_reflns_limit_k_max 20
_reflns_limit_l_min 0
_reflns_limit_l_max 25
_oxford_diffrn_Wilson_B_factor 1.95
_oxford_diffrn_Wilson_scale 163.70
_atom_sites_solution_primary direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_diff_density_min -1.28
_refine_diff_density_max 2.53
# The current dictionary definitions do not cover the
# situation where the reflections used for refinement were
# selected by a user-defined sigma threshold
# The values actually used during refinement
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns 17679
_refine_ls_number_restraints 1
_refine_ls_number_parameters 542
_oxford_refine_ls_R_factor_ref 0.0943
_refine_ls_wR_factor_ref 0.2032
_refine_ls_goodness_of_fit_ref 0.9847
_refine_ls_shift/su_max 0.0040489
_refine_ls_shift/su_mean 8.1273460
# The values computed from all data
_oxford_reflns_number_all 17679
_refine_ls_R_factor_all 0.0943
_refine_ls_wR_factor_all 0.2032
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression I>2.0\s(I)
_reflns_number_gt 12534
_refine_ls_R_factor_gt 0.0669
_refine_ls_wR_factor_gt 0.1773
# choose from: rm (reference molecule of known chirality),
# ad (anomolous dispersion - Flack), rmad (rm and ad),
# syn (from synthesis), unk (unknown) or . (not applicable).
_chemical_absolute_configuration .
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_hydrogen_treatment none # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.09P)^2^ +14.84P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
# Insert your own references if required - in alphabetical order
_publ_section_references
;
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C.,
Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435.
Betteridge, P.W., Carruthers, J.R., Cooper, R.I.,
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487.
Bruker Analytical X-ray Systems, Inc., 2006. Apex2,
Version 2 User Manual, M86-E01078, Madison, WI.
De Meulenaer, J. & Tompa, H. (1965). Acta Cryst. 19, 1014.
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical
Crystallography Laboratory, Oxford, UK.
;
# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3
# Replace last . with number of unfound hydrogen atomsattached to an atom.
# ..._refinement_flags_...
# . no refinement constraints S special position constraint on site
# G rigid group refinement of site R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond) P partial occupancy constraint
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_oxford_atom_site_special_shape
_atom_site_attached_hydrogens
Zr1 Zr 0.78628(3) 0.88565(3) 0.308877(19) 0.0230 1.0000 Uani . . . . . . .
Co1 Co 0.98204(4) 0.92711(4) 0.31735(3) 0.0269 1.0000 Uani D . . . . . .
Cl1 Cl 1.1312(3) 0.9928(3) 0.3300(2) 0.0324 0.852(2) Uani . . P 1 1 . .
I1 I 1.1353(6) 1.0204(5) 0.3258(5) 0.0466 0.148(2) Uani D . P 1 2 . .
P1 P 0.96607(7) 0.77588(8) 0.39076(6) 0.0248 1.0000 Uani . . . . . . .
P2 P 0.96124(8) 0.93522(10) 0.19503(5) 0.0310 1.0000 Uani . . . . . . .
P3 P 0.56559(7) 0.88035(8) 0.34060(5) 0.0227 1.0000 Uani . . . . . . .
N1 N 0.8301(2) 0.7637(2) 0.39757(18) 0.0245 1.0000 Uani . . . . . . .
N2 N 0.8407(3) 0.8972(3) 0.19149(19) 0.0332 1.0000 Uani . . . . . . .
N3 N 0.6293(2) 0.9771(2) 0.31174(17) 0.0236 1.0000 Uani . . . . . . .
C1 C 1.0118(3) 0.7681(3) 0.4847(2) 0.0315 1.0000 Uani . . . . . . .
C2 C 0.9789(4) 0.8653(4) 0.5093(2) 0.0366 1.0000 Uani . . . . . . .
C3 C 1.1390(4) 0.7360(5) 0.4861(3) 0.0477 1.0000 Uani . . . . . . .
C4 C 1.0451(3) 0.6676(4) 0.3544(3) 0.0356 1.0000 Uani . . . . . . .
C5 C 1.0418(4) 0.5700(4) 0.4080(3) 0.0456 1.0000 Uani . . . . . . .
C6 C 1.1641(4) 0.6776(5) 0.3202(3) 0.0482 1.0000 Uani . . . . . . .
C7 C 0.7747(3) 0.6887(3) 0.4447(2) 0.0261 1.0000 Uani . . . . . . .
C8 C 0.7361(3) 0.6911(3) 0.5199(2) 0.0282 1.0000 Uani . . . . . . .
C9 C 0.6832(3) 0.6154(3) 0.5626(3) 0.0339 1.0000 Uani . . . . . . .
C10 C 0.6621(3) 0.5399(3) 0.5340(3) 0.0405 1.0000 Uani . . . . . . .
C11 C 0.6948(3) 0.5422(3) 0.4579(3) 0.0430 1.0000 Uani . . . . . . .
C12 C 0.7485(3) 0.6151(3) 0.4126(3) 0.0336 1.0000 Uani . . . . . . .
C13 C 0.7422(3) 0.7742(3) 0.5561(2) 0.0300 1.0000 Uani . . . . . . .
C14 C 0.5986(4) 0.4623(4) 0.5802(4) 0.0571 1.0000 Uani . . . . . . .
C15 C 0.7753(4) 0.6150(4) 0.3303(3) 0.0430 1.0000 Uani . . . . . . .
C16 C 0.9572(4) 1.0612(4) 0.1386(2) 0.0405 1.0000 Uani . . . . . . .
C17 C 1.0713(4) 1.0929(5) 0.1159(3) 0.0504 1.0000 Uani . . . . . . .
C18 C 0.8842(4) 1.1328(4) 0.1826(3) 0.0433 1.0000 Uani . . . . . . .
C19 C 1.0770(3) 0.8581(4) 0.1475(2) 0.0384 1.0000 Uani . . . . . . .
C20 C 1.1952(3) 0.8683(5) 0.1612(3) 0.0458 1.0000 Uani . . . . . . .
C21 C 1.0699(4) 0.8683(5) 0.0627(2) 0.0493 1.0000 Uani . . . . . . .
C22 C 0.7931(3) 0.8852(4) 0.1268(2) 0.0411 1.0000 Uani . . . . . . .
C23 C 0.8118(4) 0.7933(5) 0.1077(3) 0.0476 1.0000 Uani . . . . . . .
C24 C 0.7618(4) 0.7830(6) 0.0457(3) 0.0608 1.0000 Uani . . . . . . .
C25 C 0.6941(4) 0.8589(6) 0.0038(3) 0.0632 1.0000 Uani . . . . . . .
C26 C 0.6750(4) 0.9458(6) 0.0252(3) 0.0589 1.0000 Uani . . . . . . .
C27 C 0.7212(3) 0.9616(5) 0.0863(2) 0.0448 1.0000 Uani . . . . . . .
C28 C 0.8857(5) 0.7067(5) 0.1482(3) 0.0563 1.0000 Uani . . . . . . .
C29 C 0.6449(6) 0.8450(8) -0.0642(4) 0.0939 1.0000 Uani . . . . . . .
C30 C 0.6878(4) 1.0599(5) 0.1072(3) 0.0496 1.0000 Uani . . . . . . .
C31 C 0.4999(3) 0.8802(3) 0.4373(2) 0.0254 1.0000 Uani . . . . . . .
C32 C 0.4053(3) 0.9660(3) 0.4449(2) 0.0305 1.0000 Uani . . . . . . .
C33 C 0.4630(3) 0.7833(3) 0.4775(3) 0.0347 1.0000 Uani . . . . . . .
C34 C 0.4556(3) 0.8756(3) 0.2821(2) 0.0293 1.0000 Uani . . . . . . .
C35 C 0.4983(4) 0.8977(4) 0.1991(3) 0.0408 1.0000 Uani . . . . . . .
C36 C 0.4248(5) 0.7744(4) 0.3024(3) 0.0513 1.0000 Uani . . . . . . .
C37 C 0.6212(3) 1.0756(3) 0.31766(19) 0.0241 1.0000 Uani . . . . . . .
C38 C 0.5341(3) 1.1518(3) 0.2948(2) 0.0293 1.0000 Uani . . . . . . .
C39 C 0.5477(4) 1.2456(3) 0.2962(2) 0.0341 1.0000 Uani . . . . . . .
C40 C 0.6420(4) 1.2673(3) 0.3188(2) 0.0353 1.0000 Uani . . . . . . .
C41 C 0.7274(4) 1.1906(3) 0.3412(2) 0.0311 1.0000 Uani . . . . . . .
C42 C 0.7185(3) 1.0947(3) 0.34227(19) 0.0247 1.0000 Uani . . . . . . .
C43 C 0.4327(4) 1.1344(4) 0.2653(3) 0.0355 1.0000 Uani . . . . . . .
C44 C 0.6522(6) 1.3710(4) 0.3198(4) 0.0557 1.0000 Uani . . . . . . .
C45 C 0.8085(3) 1.0095(3) 0.3681(2) 0.0249 1.0000 Uani . . . . . . .
C46 C 0.4295(15) 1.4075(14) -0.1589(10) 0.1925 1.0000 Uani . . . . . . .
C47 C 0.5218(16) 1.3566(14) -0.1266(10) 0.1855 1.0000 Uani . . . . . . .
C48 C 0.5072(15) 1.3649(11) -0.0441(9) 0.1571 1.0000 Uani . . . . . . .
C49 C 0.6057(14) 1.3052(12) 0.0033(10) 0.1765 1.0000 Uani . . . . . . .
C50 C 0.5941(15) 1.3252(12) 0.0845(7) 0.1836 1.0000 Uani . . . . . . .
H11 H 0.9760 0.7184 0.5223 0.0378 1.0000 Uiso R . . . . . .
H21 H 0.9014 0.8922 0.5028 0.0543 1.0000 Uiso R . . . . . .
H22 H 1.0247 0.9115 0.4805 0.0547 1.0000 Uiso R . . . . . .
H23 H 0.9891 0.8574 0.5620 0.0549 1.0000 Uiso R . . . . . .
H31 H 1.1759 0.7818 0.4482 0.0711 1.0000 Uiso R . . . . . .
H32 H 1.1576 0.7368 0.5360 0.0708 1.0000 Uiso R . . . . . .
H33 H 1.1622 0.6703 0.4756 0.0708 1.0000 Uiso R . . . . . .
H41 H 1.0056 0.6650 0.3120 0.0426 1.0000 Uiso R . . . . . .
H51 H 1.0663 0.5178 0.3813 0.0678 1.0000 Uiso R . . . . . .
H52 H 0.9676 0.5656 0.4311 0.0678 1.0000 Uiso R . . . . . .
H53 H 1.0911 0.5627 0.4462 0.0677 1.0000 Uiso R . . . . . .
H61 H 1.1659 0.7439 0.2930 0.0720 1.0000 Uiso R . . . . . .
H62 H 1.2130 0.6619 0.3598 0.0719 1.0000 Uiso R . . . . . .
H63 H 1.1889 0.6328 0.2862 0.0720 1.0000 Uiso R . . . . . .
H91 H 0.6618 0.6169 0.6124 0.0407 1.0000 Uiso R . . . . . .
H111 H 0.6798 0.4929 0.4364 0.0521 1.0000 Uiso R . . . . . .
H131 H 0.7480 0.8306 0.5189 0.0446 1.0000 Uiso R . . . . . .
H132 H 0.6754 0.7850 0.5884 0.0449 1.0000 Uiso R . . . . . .
H133 H 0.8047 0.7603 0.5856 0.0449 1.0000 Uiso R . . . . . .
H141 H 0.5200 0.4833 0.5749 0.0859 1.0000 Uiso R . . . . . .
H142 H 0.6239 0.4030 0.5619 0.0860 1.0000 Uiso R . . . . . .
H143 H 0.6115 0.4516 0.6321 0.0859 1.0000 Uiso R . . . . . .
H151 H 0.8553 0.5989 0.3200 0.0650 1.0000 Uiso R . . . . . .
H152 H 0.7499 0.6780 0.3007 0.0647 1.0000 Uiso R . . . . . .
H153 H 0.7402 0.5674 0.3170 0.0652 1.0000 Uiso R . . . . . .
H161 H 0.9223 1.0653 0.0929 0.0491 1.0000 Uiso R . . . . . .
H171 H 1.1111 1.0821 0.1597 0.0756 1.0000 Uiso R . . . . . .
H172 H 1.1134 1.0568 0.0798 0.0759 1.0000 Uiso R . . . . . .
H173 H 1.0591 1.1621 0.0939 0.0759 1.0000 Uiso R . . . . . .
H181 H 0.8133 1.1113 0.2021 0.0648 1.0000 Uiso R . . . . . .
H182 H 0.8679 1.1960 0.1504 0.0650 1.0000 Uiso R . . . . . .
H183 H 0.9219 1.1382 0.2237 0.0645 1.0000 Uiso R . . . . . .
H191 H 1.0678 0.7910 0.1701 0.0457 1.0000 Uiso R . . . . . .
H201 H 1.1954 0.8791 0.2112 0.0688 1.0000 Uiso R . . . . . .
H202 H 1.2203 0.9209 0.1253 0.0691 1.0000 Uiso R . . . . . .
H203 H 1.2447 0.8087 0.1569 0.0690 1.0000 Uiso R . . . . . .
H211 H 1.0852 0.9310 0.0361 0.0737 1.0000 Uiso R . . . . . .
H212 H 1.1237 0.8193 0.0431 0.0737 1.0000 Uiso R . . . . . .
H213 H 0.9982 0.8607 0.0530 0.0737 1.0000 Uiso R . . . . . .
H241 H 0.7756 0.7227 0.0324 0.0731 1.0000 Uiso R . . . . . .
H261 H 0.6265 0.9974 -0.0015 0.0708 1.0000 Uiso R . . . . . .
H281 H 0.8518 0.6494 0.1567 0.0838 1.0000 Uiso R . . . . . .
H282 H 0.8986 0.7169 0.1962 0.0840 1.0000 Uiso R . . . . . .
H283 H 0.9575 0.6946 0.1193 0.0838 1.0000 Uiso R . . . . . .
H291 H 0.6383 0.7772 -0.0581 0.1409 1.0000 Uiso R . . . . . .
H292 H 0.5719 0.8834 -0.0679 0.1411 1.0000 Uiso R . . . . . .
H293 H 0.6925 0.8637 -0.1087 0.1410 1.0000 Uiso R . . . . . .
H301 H 0.7451 1.0995 0.0873 0.0737 1.0000 Uiso R . . . . . .
H302 H 0.6188 1.0925 0.0867 0.0741 1.0000 Uiso R . . . . . .
H303 H 0.6770 1.0522 0.1611 0.0737 1.0000 Uiso R . . . . . .
H311 H 0.5598 0.8870 0.4649 0.0300 1.0000 Uiso R . . . . . .
H321 H 0.3460 0.9638 0.4168 0.0459 1.0000 Uiso R . . . . . .
H322 H 0.4347 1.0263 0.4250 0.0458 1.0000 Uiso R . . . . . .
H323 H 0.3792 0.9627 0.4966 0.0459 1.0000 Uiso R . . . . . .
H331 H 0.5160 0.7295 0.4640 0.0519 1.0000 Uiso R . . . . . .
H332 H 0.4596 0.7798 0.5309 0.0517 1.0000 Uiso R . . . . . .
H333 H 0.3906 0.7815 0.4641 0.0520 1.0000 Uiso R . . . . . .
H341 H 0.3893 0.9239 0.2919 0.0353 1.0000 Uiso R . . . . . .
H351 H 0.5229 0.9598 0.1859 0.0604 1.0000 Uiso R . . . . . .
H352 H 0.4400 0.8972 0.1690 0.0608 1.0000 Uiso R . . . . . .
H353 H 0.5598 0.8477 0.1891 0.0611 1.0000 Uiso R . . . . . .
H361 H 0.3907 0.7611 0.3535 0.0771 1.0000 Uiso R . . . . . .
H362 H 0.4909 0.7265 0.2972 0.0767 1.0000 Uiso R . . . . . .
H363 H 0.3736 0.7694 0.2683 0.0767 1.0000 Uiso R . . . . . .
H391 H 0.4905 1.2956 0.2806 0.0410 1.0000 Uiso R . . . . . .
H411 H 0.7927 1.2034 0.3552 0.0370 1.0000 Uiso R . . . . . .
H431 H 0.3839 1.1948 0.2533 0.0531 1.0000 Uiso R . . . . . .
H432 H 0.4534 1.1084 0.2208 0.0532 1.0000 Uiso R . . . . . .
H433 H 0.3954 1.0900 0.3021 0.0533 1.0000 Uiso R . . . . . .
H441 H 0.7128 1.3916 0.2849 0.0832 1.0000 Uiso R . . . . . .
H442 H 0.6649 1.3764 0.3691 0.0833 1.0000 Uiso R . . . . . .
H443 H 0.5839 1.4147 0.3062 0.0829 1.0000 Uiso R . . . . . .
H451 H 0.7788 0.9706 0.4138 0.0362 1.0000 Uiso R . . . . . .
H452 H 0.8679 1.0347 0.3827 0.0370 1.0000 Uiso R . . . . . .
H471 H 0.5877 1.3847 -0.1524 0.2191 1.0000 Uiso R . . . . . .
H472 H 0.5313 1.2881 -0.1305 0.2191 1.0000 Uiso R . . . . . .
H481 H 0.4366 1.3424 -0.0201 0.1873 1.0000 Uiso R . . . . . .
H482 H 0.5015 1.4348 -0.0431 0.1873 1.0000 Uiso R . . . . . .
H491 H 0.6769 1.3247 -0.0224 0.2111 1.0000 Uiso R . . . . . .
H492 H 0.6082 1.2344 0.0065 0.2111 1.0000 Uiso R . . . . . .
H501 H 0.6279 1.3824 0.0839 0.2741 1.0000 Uiso R . . . . . .
H502 H 0.5160 1.3380 0.1021 0.2741 1.0000 Uiso R . . . . . .
H503 H 0.6322 1.2692 0.1174 0.2740 1.0000 Uiso R . . . . . .
H461 H 0.4380 1.4023 -0.2103 0.2193 1.0000 Uiso R . . . . . .
H462 H 0.4215 1.4741 -0.1558 0.2193 1.0000 Uiso R . . . . . .
H463 H 0.3649 1.3819 -0.1343 0.2193 1.0000 Uiso R . . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zr1 0.01146(14) 0.0399(2) 0.02088(17) -0.01333(14) 0.00356(11) -0.00744(13)
Co1 0.0177(2) 0.0463(3) 0.0203(2) -0.0099(2) 0.00175(17) -0.0132(2)
Cl1 0.0205(8) 0.0504(17) 0.0306(9) -0.0120(11) 0.0017(6) -0.0152(9)
I1 0.0335(15) 0.067(4) 0.0454(17) -0.003(2) -0.0053(11) -0.031(2)
P1 0.0126(4) 0.0380(5) 0.0259(5) -0.0120(4) 0.0016(3) -0.0055(3)
P2 0.0136(4) 0.0618(7) 0.0193(4) -0.0125(4) 0.0033(3) -0.0091(4)
P3 0.0113(4) 0.0350(5) 0.0247(4) -0.0136(4) 0.0038(3) -0.0064(3)
N1 0.0118(12) 0.0354(17) 0.0297(16) -0.0165(13) 0.0035(11) -0.0042(11)
N2 0.0135(13) 0.068(3) 0.0229(15) -0.0212(16) 0.0010(11) -0.0073(14)
N3 0.0155(13) 0.0352(17) 0.0226(14) -0.0115(13) 0.0026(11) -0.0067(12)
C1 0.0207(17) 0.049(2) 0.0267(19) -0.0060(17) -0.0043(14) -0.0106(16)
C2 0.040(2) 0.046(3) 0.029(2) -0.0104(18) -0.0040(17) -0.017(2)
C3 0.030(2) 0.072(4) 0.047(3) -0.021(3) -0.012(2) -0.005(2)
C4 0.0177(17) 0.048(3) 0.042(2) -0.021(2) 0.0010(15) 0.0027(16)
C5 0.023(2) 0.044(3) 0.070(3) -0.020(2) -0.002(2) 0.0030(18)
C6 0.0178(18) 0.076(4) 0.050(3) -0.023(3) 0.0053(18) -0.001(2)
C7 0.0133(14) 0.0267(18) 0.039(2) -0.0121(16) 0.0020(13) -0.0028(13)
C8 0.0125(14) 0.0300(19) 0.040(2) -0.0083(16) 0.0028(14) -0.0014(13)
C9 0.0173(16) 0.032(2) 0.046(2) -0.0023(18) 0.0042(15) -0.0010(14)
C10 0.0169(17) 0.026(2) 0.076(3) -0.007(2) -0.0018(19) -0.0021(14)
C11 0.0177(17) 0.031(2) 0.086(4) -0.024(2) -0.001(2) -0.0043(15)
C12 0.0162(16) 0.034(2) 0.054(3) -0.0205(19) 0.0002(16) -0.0020(14)
C13 0.0234(17) 0.036(2) 0.0293(19) -0.0095(16) 0.0046(14) -0.0044(15)
C14 0.027(2) 0.030(2) 0.107(5) 0.001(3) -0.003(3) -0.0081(18)
C15 0.028(2) 0.050(3) 0.061(3) -0.036(2) -0.001(2) -0.0056(19)
C16 0.0226(18) 0.076(3) 0.0207(18) -0.004(2) 0.0022(14) -0.011(2)
C17 0.030(2) 0.081(4) 0.037(2) -0.005(2) 0.0097(18) -0.019(2)
C18 0.035(2) 0.064(3) 0.028(2) -0.004(2) 0.0051(17) -0.013(2)
C19 0.0180(17) 0.077(3) 0.0214(18) -0.017(2) 0.0023(14) -0.0052(19)
C20 0.0146(17) 0.088(4) 0.035(2) -0.017(2) 0.0007(15) -0.006(2)
C21 0.024(2) 0.100(4) 0.026(2) -0.024(2) 0.0085(16) -0.008(2)
C22 0.0174(17) 0.092(4) 0.0202(18) -0.022(2) 0.0048(13) -0.016(2)
C23 0.025(2) 0.096(4) 0.032(2) -0.033(3) 0.0055(17) -0.018(2)
C24 0.037(3) 0.121(6) 0.046(3) -0.051(3) 0.011(2) -0.037(3)
C25 0.025(2) 0.149(7) 0.030(2) -0.037(3) 0.0023(18) -0.030(3)
C26 0.0200(19) 0.141(6) 0.022(2) -0.022(3) 0.0016(15) -0.025(3)
C27 0.0169(17) 0.100(4) 0.0204(18) -0.015(2) 0.0061(14) -0.017(2)
C28 0.044(3) 0.093(5) 0.044(3) -0.043(3) 0.005(2) -0.015(3)
C29 0.044(3) 0.211(10) 0.051(4) -0.062(5) -0.003(3) -0.040(5)
C30 0.0209(19) 0.096(4) 0.028(2) -0.004(2) 0.0002(16) -0.010(2)
C31 0.0164(15) 0.034(2) 0.0261(17) -0.0102(15) 0.0041(12) -0.0053(14)
C32 0.0251(18) 0.038(2) 0.0258(18) -0.0099(16) 0.0052(14) 0.0001(16)
C33 0.0217(18) 0.037(2) 0.040(2) -0.0050(18) 0.0087(16) -0.0051(16)
C34 0.0163(15) 0.044(2) 0.033(2) -0.0183(17) 0.0005(14) -0.0084(15)
C35 0.0239(19) 0.074(3) 0.033(2) -0.025(2) 0.0030(16) -0.016(2)
C36 0.053(3) 0.054(3) 0.057(3) -0.001(2) -0.029(3) -0.030(3)
C37 0.0239(16) 0.036(2) 0.0148(15) -0.0069(14) 0.0037(12) -0.0113(14)
C38 0.0289(19) 0.040(2) 0.0187(16) -0.0055(15) 0.0021(14) -0.0098(16)
C39 0.039(2) 0.036(2) 0.0251(19) -0.0024(16) -0.0018(16) -0.0045(18)
C40 0.045(2) 0.031(2) 0.030(2) -0.0036(17) -0.0001(17) -0.0116(18)
C41 0.034(2) 0.038(2) 0.0251(18) -0.0078(16) -0.0011(15) -0.0147(17)
C42 0.0240(17) 0.037(2) 0.0156(15) -0.0082(14) 0.0039(12) -0.0119(15)
C43 0.032(2) 0.043(2) 0.031(2) -0.0059(18) -0.0041(16) -0.0051(18)
C44 0.066(4) 0.037(3) 0.068(4) -0.007(3) -0.018(3) -0.015(3)
C45 0.0220(16) 0.036(2) 0.0192(16) -0.0070(14) 0.0001(12) -0.0106(14)
C46 0.174(17) 0.215(18) 0.172(16) 0.002(13) -0.076(13) 0.002(14)
C47 0.189(17) 0.234(19) 0.165(14) -0.128(14) -0.064(13) 0.024(14)
C48 0.179(16) 0.134(11) 0.162(14) -0.027(10) -0.018(12) -0.037(11)
C49 0.136(13) 0.154(13) 0.206(18) 0.015(12) -0.045(12) 0.019(10)
C50 0.214(18) 0.220(17) 0.087(8) -0.046(10) -0.043(10) 0.073(14)
_refine_ls_extinction_method None
_oxford_refine_ls_scale 0.13780(6)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Zr1 . Co1 . 2.6036(6) yes
Zr1 . P1 . 2.8406(10) yes
Zr1 . P2 . 2.8535(10) yes
Zr1 . P3 . 2.6935(9) yes
Zr1 . N1 . 2.140(4) yes
Zr1 . N2 . 2.144(3) yes
Zr1 . N3 . 2.106(3) yes
Zr1 . C45 . 2.343(4) yes
Co1 . Cl1 . 2.262(3) yes
Co1 . P1 . 2.3018(12) yes
Co1 . P2 . 2.2656(11) yes
Co1 . C45 . 2.398(4) yes
Co1 . I1 . 2.534(5) yes
Co1 . P1 . 2.3018(12) yes
Co1 . P2 . 2.2656(11) yes
Co1 . C45 . 2.398(4) yes
P1 . N1 . 1.688(3) yes
P1 . C1 . 1.856(4) yes
P1 . C4 . 1.865(4) yes
P2 . N2 . 1.677(3) yes
P2 . C16 . 1.859(5) yes
P2 . C19 . 1.863(4) yes
P3 . N3 . 1.662(3) yes
P3 . C31 . 1.844(4) yes
P3 . C34 . 1.849(4) yes
N1 . C7 . 1.435(5) yes
N2 . C22 . 1.444(5) yes
N3 . C37 . 1.417(5) yes
C1 . C2 . 1.516(7) yes
C1 . C3 . 1.537(6) yes
C1 . H11 . 0.993 no
C2 . H21 . 0.966 no
C2 . H22 . 0.966 no
C2 . H23 . 0.969 no
C3 . H31 . 0.968 no
C3 . H32 . 0.975 no
C3 . H33 . 0.980 no
C4 . C5 . 1.518(7) yes
C4 . C6 . 1.524(6) yes
C4 . H41 . 0.980 no
C5 . H51 . 0.960 no
C5 . H52 . 0.955 no
C5 . H53 . 0.960 no
C6 . H61 . 0.969 no
C6 . H62 . 0.963 no
C6 . H63 . 0.970 no
C7 . C8 . 1.401(6) yes
C7 . C12 . 1.414(5) yes
C8 . C9 . 1.397(6) yes
C8 . C13 . 1.499(6) yes
C9 . C10 . 1.376(7) yes
C9 . H91 . 0.919 no
C10 . C11 . 1.392(8) yes
C10 . C14 . 1.509(7) yes
C11 . C12 . 1.389(7) yes
C11 . H111 . 0.935 no
C12 . C15 . 1.502(7) yes
C13 . H131 . 0.940 no
C13 . H132 . 0.950 no
C13 . H133 . 0.960 no
C14 . H141 . 0.961 no
C14 . H142 . 0.960 no
C14 . H143 . 0.960 no
C15 . H151 . 0.964 no
C15 . H152 . 0.960 no
C15 . H153 . 0.957 no
C16 . C17 . 1.523(6) yes
C16 . C18 . 1.521(7) yes
C16 . H161 . 0.976 no
C17 . H171 . 0.964 no
C17 . H172 . 0.963 no
C17 . H173 . 0.970 no
C18 . H181 . 0.970 no
C18 . H182 . 0.963 no
C18 . H183 . 0.958 no
C19 . C20 . 1.538(6) yes
C19 . C21 . 1.543(6) yes
C19 . H191 . 0.976 no
C20 . H201 . 0.963 no
C20 . H202 . 0.950 no
C20 . H203 . 0.958 no
C21 . H211 . 0.958 no
C21 . H212 . 0.960 no
C21 . H213 . 0.947 no
C22 . C23 . 1.401(8) yes
C22 . C27 . 1.401(7) yes
C23 . C24 . 1.409(6) yes
C23 . C28 . 1.497(9) yes
C24 . C25 . 1.380(10) yes
C24 . H241 . 0.925 no
C25 . C26 . 1.351(10) yes
C25 . C29 . 1.522(7) yes
C26 . C27 . 1.398(6) yes
C26 . H261 . 0.939 no
C27 . C30 . 1.502(9) yes
C28 . H281 . 0.957 no
C28 . H282 . 0.961 no
C28 . H283 . 0.969 no
C29 . H291 . 0.965 no
C29 . H292 . 0.957 no
C29 . H293 . 0.953 no
C30 . H301 . 0.965 no
C30 . H302 . 0.963 no
C30 . H303 . 0.964 no
C31 . C32 . 1.532(5) yes
C31 . C33 . 1.532(6) yes
C31 . H311 . 0.976 no
C32 . H321 . 0.954 no
C32 . H322 . 0.971 no
C32 . H323 . 0.953 no
C33 . H331 . 0.961 no
C33 . H332 . 0.963 no
C33 . H333 . 0.957 no
C34 . C35 . 1.522(6) yes
C34 . C36 . 1.514(6) yes
C34 . H341 . 0.983 no
C35 . H351 . 0.959 no
C35 . H352 . 0.960 no
C35 . H353 . 0.962 no
C36 . H361 . 0.966 no
C36 . H362 . 0.964 no
C36 . H363 . 0.965 no
C37 . C38 . 1.403(6) yes
C37 . C42 . 1.419(5) yes
C38 . C39 . 1.384(6) yes
C38 . C43 . 1.499(6) yes
C39 . C40 . 1.385(6) yes
C39 . H391 . 0.924 no
C40 . C41 . 1.391(6) yes
C40 . C44 . 1.512(7) yes
C41 . C42 . 1.389(6) yes
C41 . H411 . 0.931 no
C42 . C45 . 1.512(6) yes
C43 . H431 . 0.950 no
C43 . H432 . 0.954 no
C43 . H433 . 0.949 no
C44 . H441 . 0.957 no
C44 . H442 . 0.959 no
C44 . H443 . 0.968 no
C45 . H451 . 0.963 no
C45 . H452 . 0.960 no
C46 . C47 . 1.352(19) yes
C46 . H461 . 0.950 no
C46 . H462 . 0.950 no
C46 . H463 . 0.950 no
C47 . C48 . 1.526(19) yes
C47 . H471 . 0.984 no
C47 . H472 . 0.979 no
C48 . C49 . 1.580(19) yes
C48 . H481 . 0.991 no
C48 . H482 . 0.989 no
C49 . C50 . 1.56(2) yes
C49 . H491 . 0.989 no
C49 . H492 . 0.993 no
C50 . H501 . 0.979 no
C50 . H502 . 0.963 no
C50 . H503 . 0.968 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Co1 . Zr1 . P1 . 49.79(2) yes
Co1 . Zr1 . P2 . 48.79(2) yes
P1 . Zr1 . P2 . 83.65(3) yes
Co1 . Zr1 . P3 . 158.88(3) yes
P1 . Zr1 . P3 . 128.54(3) yes
P2 . Zr1 . P3 . 146.04(3) yes
Co1 . Zr1 . N1 . 85.20(8) yes
P1 . Zr1 . N1 . 36.30(8) yes
P2 . Zr1 . N1 . 116.56(8) yes
P3 . Zr1 . N1 . 92.85(8) yes
Co1 . Zr1 . N2 . 84.38(9) yes
P1 . Zr1 . N2 . 107.72(9) yes
P2 . Zr1 . N2 . 35.79(9) yes
P3 . Zr1 . N2 . 113.03(9) yes
N1 . Zr1 . N2 . 126.82(13) yes
Co1 . Zr1 . N3 . 128.38(9) yes
P1 . Zr1 . N3 . 147.01(9) yes
P2 . Zr1 . N3 . 120.60(9) yes
P3 . Zr1 . N3 . 38.11(9) yes
N1 . Zr1 . N3 . 122.32(12) yes
Co1 . Zr1 . C45 . 57.72(9) yes
P1 . Zr1 . C45 . 83.89(10) yes
P2 . Zr1 . C45 . 90.81(9) yes
P3 . Zr1 . C45 . 101.97(9) yes
N1 . Zr1 . C45 . 98.17(13) yes
N2 . Zr1 . N3 . 104.49(13) yes
N2 . Zr1 . C45 . 118.81(14) yes
N3 . Zr1 . C45 . 74.50(12) yes
Zr1 . Co1 . Cl1 . 168.00(10) yes
Zr1 . Co1 . P1 . 70.47(3) yes
Cl1 . Co1 . P1 . 116.85(11) yes
Zr1 . Co1 . P2 . 71.37(3) yes
Cl1 . Co1 . P2 . 111.79(11) yes
P1 . Co1 . P2 . 112.48(5) yes
Zr1 . Co1 . C45 . 55.67(9) yes
Cl1 . Co1 . C45 . 112.84(13) yes
P1 . Co1 . C45 . 95.66(10) yes
P2 . Co1 . C45 . 105.67(9) yes
Zr1 . Co1 . I1 . 161.74(19) yes
Zr1 . Co1 . P1 . 70.47(3) yes
I1 . Co1 . P1 . 123.10(19) yes
Zr1 . Co1 . P2 . 71.37(3) yes
I1 . Co1 . P2 . 109.57(19) yes
P1 . Co1 . P2 . 112.48(5) yes
Zr1 . Co1 . C45 . 55.67(9) yes
I1 . Co1 . C45 . 108.0(2) yes
P1 . Co1 . C45 . 95.66(10) yes
P2 . Co1 . C45 . 105.67(9) yes
Zr1 . P1 . Co1 . 59.74(3) yes
Zr1 . P1 . N1 . 48.61(12) yes
Co1 . P1 . N1 . 107.03(13) yes
Zr1 . P1 . C1 . 135.51(14) yes
Co1 . P1 . C1 . 109.40(15) yes
N1 . P1 . C1 . 111.01(17) yes
Zr1 . P1 . C4 . 115.99(15) yes
Co1 . P1 . C4 . 117.13(16) yes
N1 . P1 . C4 . 105.00(18) yes
C1 . P1 . C4 . 107.2(2) yes
Zr1 . P2 . Co1 . 59.84(3) yes
Zr1 . P2 . N2 . 48.37(11) yes
Co1 . P2 . N2 . 107.90(12) yes
Zr1 . P2 . C16 . 121.45(14) yes
Co1 . P2 . C16 . 112.03(16) yes
N2 . P2 . C16 . 109.3(2) yes
Zr1 . P2 . C19 . 131.65(18) yes
Co1 . P2 . C19 . 113.42(14) yes
N2 . P2 . C19 . 108.4(2) yes
C16 . P2 . C19 . 105.7(2) yes
Zr1 . P3 . N3 . 51.43(11) yes
Zr1 . P3 . C31 . 119.85(12) yes
N3 . P3 . C31 . 108.85(17) yes
Zr1 . P3 . C34 . 132.37(13) yes
N3 . P3 . C34 . 114.49(19) yes
C31 . P3 . C34 . 107.78(17) yes
P1 . N1 . Zr1 . 95.09(15) yes
P1 . N1 . C7 . 128.6(3) yes
Zr1 . N1 . C7 . 136.1(2) yes
P2 . N2 . Zr1 . 95.84(15) yes
P2 . N2 . C22 . 128.9(3) yes
Zr1 . N2 . C22 . 135.2(3) yes
P3 . N3 . Zr1 . 90.46(15) yes
P3 . N3 . C37 . 142.6(2) yes
Zr1 . N3 . C37 . 120.4(2) yes
P1 . C1 . C2 . 111.2(3) yes
P1 . C1 . C3 . 111.9(3) yes
C2 . C1 . C3 . 108.8(4) yes
P1 . C1 . H11 . 109.5 no
C2 . C1 . H11 . 108.6 no
C3 . C1 . H11 . 106.7 no
C1 . C2 . H21 . 111.2 no
C1 . C2 . H22 . 110.5 no
H21 . C2 . H22 . 108.4 no
C1 . C2 . H23 . 110.4 no
H21 . C2 . H23 . 107.9 no
H22 . C2 . H23 . 108.3 no
C1 . C3 . H31 . 108.4 no
C1 . C3 . H32 . 107.6 no
H31 . C3 . H32 . 110.4 no
C1 . C3 . H33 . 111.0 no
H31 . C3 . H33 . 109.5 no
H32 . C3 . H33 . 109.9 no
P1 . C4 . C5 . 115.4(3) yes
P1 . C4 . C6 . 114.6(4) yes
C5 . C4 . C6 . 111.2(4) yes
P1 . C4 . H41 . 104.5 no
C5 . C4 . H41 . 105.3 no
C6 . C4 . H41 . 104.5 no
C4 . C5 . H51 . 110.1 no
C4 . C5 . H52 . 110.7 no
H51 . C5 . H52 . 108.7 no
C4 . C5 . H53 . 109.5 no
H51 . C5 . H53 . 108.5 no
H52 . C5 . H53 . 109.3 no
C4 . C6 . H61 . 109.6 no
C4 . C6 . H62 . 109.3 no
H61 . C6 . H62 . 109.7 no
C4 . C6 . H63 . 109.5 no
H61 . C6 . H63 . 109.6 no
H62 . C6 . H63 . 109.2 no
N1 . C7 . C8 . 121.9(3) yes
N1 . C7 . C12 . 119.1(4) yes
C8 . C7 . C12 . 118.7(4) yes
C7 . C8 . C9 . 118.8(4) yes
C7 . C8 . C13 . 123.4(4) yes
C9 . C8 . C13 . 117.7(4) yes
C8 . C9 . C10 . 123.5(5) yes
C8 . C9 . H91 . 117.2 no
C10 . C9 . H91 . 119.3 no
C9 . C10 . C11 . 116.7(4) yes
C9 . C10 . C14 . 122.3(5) yes
C11 . C10 . C14 . 120.8(5) yes
C10 . C11 . C12 . 122.5(4) yes
C10 . C11 . H111 . 118.8 no
C12 . C11 . H111 . 118.7 no
C7 . C12 . C11 . 119.4(4) yes
C7 . C12 . C15 . 121.6(4) yes
C11 . C12 . C15 . 119.0(4) yes
C8 . C13 . H131 . 109.5 no
C8 . C13 . H132 . 108.2 no
H131 . C13 . H132 . 109.4 no
C8 . C13 . H133 . 112.0 no
H131 . C13 . H133 . 109.3 no
H132 . C13 . H133 . 108.4 no
C10 . C14 . H141 . 108.9 no
C10 . C14 . H142 . 108.7 no
H141 . C14 . H142 . 109.7 no
C10 . C14 . H143 . 110.0 no
H141 . C14 . H143 . 109.7 no
H142 . C14 . H143 . 109.8 no
C12 . C15 . H151 . 108.5 no
C12 . C15 . H152 . 110.7 no
H151 . C15 . H152 . 109.0 no
C12 . C15 . H153 . 109.9 no
H151 . C15 . H153 . 109.4 no
H152 . C15 . H153 . 109.3 no
P2 . C16 . C17 . 114.7(4) yes
P2 . C16 . C18 . 109.3(3) yes
C17 . C16 . C18 . 108.5(5) yes
P2 . C16 . H161 . 108.1 no
C17 . C16 . H161 . 108.2 no
C18 . C16 . H161 . 107.8 no
C16 . C17 . H171 . 109.7 no
C16 . C17 . H172 . 109.8 no
H171 . C17 . H172 . 110.2 no
C16 . C17 . H173 . 107.9 no
H171 . C17 . H173 . 109.1 no
H172 . C17 . H173 . 110.1 no
C16 . C18 . H181 . 110.7 no
C16 . C18 . H182 . 110.3 no
H181 . C18 . H182 . 107.5 no
C16 . C18 . H183 . 109.9 no
H181 . C18 . H183 . 109.1 no
H182 . C18 . H183 . 109.4 no
P2 . C19 . C20 . 114.6(3) yes
P2 . C19 . C21 . 114.6(3) yes
C20 . C19 . C21 . 109.8(3) yes
P2 . C19 . H191 . 105.1 no
C20 . C19 . H191 . 106.5 no
C21 . C19 . H191 . 105.3 no
C19 . C20 . H201 . 110.4 no
C19 . C20 . H202 . 110.2 no
H201 . C20 . H202 . 109.8 no
C19 . C20 . H203 . 108.6 no
H201 . C20 . H203 . 107.9 no
H202 . C20 . H203 . 109.9 no
C19 . C21 . H211 . 110.0 no
C19 . C21 . H212 . 110.8 no
H211 . C21 . H212 . 108.2 no
C19 . C21 . H213 . 111.3 no
H211 . C21 . H213 . 109.1 no
H212 . C21 . H213 . 107.3 no
N2 . C22 . C23 . 119.4(5) yes
N2 . C22 . C27 . 121.4(5) yes
C23 . C22 . C27 . 119.0(4) yes
C22 . C23 . C24 . 118.2(6) yes
C22 . C23 . C28 . 123.2(4) yes
C24 . C23 . C28 . 118.6(5) yes
C23 . C24 . C25 . 123.0(6) yes
C23 . C24 . H241 . 118.1 no
C25 . C24 . H241 . 118.9 no
C24 . C25 . C26 . 117.3(5) yes
C24 . C25 . C29 . 121.0(7) yes
C26 . C25 . C29 . 121.7(7) yes
C25 . C26 . C27 . 123.1(6) yes
C25 . C26 . H261 . 118.1 no
C27 . C26 . H261 . 118.8 no
C22 . C27 . C26 . 119.3(6) yes
C22 . C27 . C30 . 122.7(4) yes
C26 . C27 . C30 . 117.9(5) yes
C23 . C28 . H281 . 110.7 no
C23 . C28 . H282 . 110.7 no
H281 . C28 . H282 . 108.0 no
C23 . C28 . H283 . 110.9 no
H281 . C28 . H283 . 108.3 no
H282 . C28 . H283 . 108.2 no
C25 . C29 . H291 . 109.1 no
C25 . C29 . H292 . 109.6 no
H291 . C29 . H292 . 108.6 no
C25 . C29 . H293 . 109.8 no
H291 . C29 . H293 . 109.6 no
H292 . C29 . H293 . 110.1 no
C27 . C30 . H301 . 110.2 no
C27 . C30 . H302 . 109.8 no
H301 . C30 . H302 . 108.7 no
C27 . C30 . H303 . 109.8 no
H301 . C30 . H303 . 109.6 no
H302 . C30 . H303 . 108.8 no
P3 . C31 . C32 . 114.6(3) yes
P3 . C31 . C33 . 114.1(3) yes
C32 . C31 . C33 . 110.8(3) yes
P3 . C31 . H311 . 104.6 no
C32 . C31 . H311 . 106.8 no
C33 . C31 . H311 . 105.1 no
C31 . C32 . H321 . 109.6 no
C31 . C32 . H322 . 108.5 no
H321 . C32 . H322 . 109.3 no
C31 . C32 . H323 . 109.3 no
H321 . C32 . H323 . 110.5 no
H322 . C32 . H323 . 109.6 no
C31 . C33 . H331 . 110.3 no
C31 . C33 . H332 . 107.9 no
H331 . C33 . H332 . 109.5 no
C31 . C33 . H333 . 109.4 no
H331 . C33 . H333 . 109.9 no
H332 . C33 . H333 . 109.8 no
P3 . C34 . C35 . 110.1(3) yes
P3 . C34 . C36 . 108.8(3) yes
C35 . C34 . C36 . 109.4(4) yes
P3 . C34 . H341 . 109.3 no
C35 . C34 . H341 . 109.6 no
C36 . C34 . H341 . 109.6 no
C34 . C35 . H351 . 110.7 no
C34 . C35 . H352 . 109.7 no
H351 . C35 . H352 . 110.0 no
C34 . C35 . H353 . 109.2 no
H351 . C35 . H353 . 109.2 no
H352 . C35 . H353 . 107.9 no
C34 . C36 . H361 . 111.0 no
C34 . C36 . H362 . 109.7 no
H361 . C36 . H362 . 109.0 no
C34 . C36 . H363 . 109.1 no
H361 . C36 . H363 . 109.9 no
H362 . C36 . H363 . 108.2 no
N3 . C37 . C38 . 126.0(3) yes
N3 . C37 . C42 . 112.9(3) yes
C38 . C37 . C42 . 120.7(4) yes
C37 . C38 . C39 . 117.5(4) yes
C37 . C38 . C43 . 121.9(4) yes
C39 . C38 . C43 . 120.5(4) yes
C38 . C39 . C40 . 123.5(4) yes
C38 . C39 . H391 . 117.2 no
C40 . C39 . H391 . 119.4 no
C39 . C40 . C41 . 118.1(4) yes
C39 . C40 . C44 . 121.3(5) yes
C41 . C40 . C44 . 120.6(4) yes
C40 . C41 . C42 . 121.5(4) yes
C40 . C41 . H411 . 119.8 no
C42 . C41 . H411 . 118.7 no
C37 . C42 . C41 . 118.7(4) yes
C37 . C42 . C45 . 118.5(3) yes
C41 . C42 . C45 . 122.8(3) yes
C38 . C43 . H431 . 108.7 no
C38 . C43 . H432 . 110.5 no
H431 . C43 . H432 . 108.5 no
C38 . C43 . H433 . 110.1 no
H431 . C43 . H433 . 109.8 no
H432 . C43 . H433 . 109.2 no
C40 . C44 . H441 . 110.8 no
C40 . C44 . H442 . 110.4 no
H441 . C44 . H442 . 108.8 no
C40 . C44 . H443 . 110.3 no
H441 . C44 . H443 . 108.5 no
H442 . C44 . H443 . 107.9 no
C42 . C45 . Zr1 . 105.6(2) yes
C42 . C45 . Co1 . 138.3(2) yes
Zr1 . C45 . Co1 . 66.61(10) yes
C42 . C45 . H451 . 108.2 no
Zr1 . C45 . H451 . 86.2 no
Co1 . C45 . H451 . 111.8 no
C42 . C45 . H452 . 108.0 no
Zr1 . C45 . H452 . 138.8 no
Co1 . C45 . H452 . 72.5 no
H451 . C45 . H452 . 104.9 no
C47 . C46 . H461 . 108.6 no
C47 . C46 . H462 . 109.6 no
H461 . C46 . H462 . 109.5 no
C47 . C46 . H463 . 110.1 no
H461 . C46 . H463 . 109.5 no
H462 . C46 . H463 . 109.5 no
C46 . C47 . C48 . 108.3(16) yes
C46 . C47 . H471 . 109.0 no
C48 . C47 . H471 . 109.8 no
C46 . C47 . H472 . 110.0 no
C48 . C47 . H472 . 110.2 no
H471 . C47 . H472 . 109.6 no
C47 . C48 . C49 . 114.9(15) yes
C47 . C48 . H481 . 108.9 no
C49 . C48 . H481 . 108.3 no
C47 . C48 . H482 . 107.1 no
C49 . C48 . H482 . 108.3 no
H481 . C48 . H482 . 109.2 no
C48 . C49 . C50 . 113.1(13) yes
C48 . C49 . H491 . 108.4 no
C50 . C49 . H491 . 107.4 no
C48 . C49 . H492 . 109.3 no
C50 . C49 . H492 . 108.9 no
H491 . C49 . H492 . 109.7 no
C49 . C50 . H501 . 109.5 no
C49 . C50 . H502 . 109.2 no
H501 . C50 . H502 . 108.9 no
C49 . C50 . H503 . 109.6 no
H501 . C50 . H503 . 109.2 no
H502 . C50 . H503 . 110.3 no
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.500 0.000 586 70 ' '
_platon_squeeze_details
;
During the structure solution, electron density difference
maps revealed that there were considerable disordered
solvent molecules. One pentane molecule was located
and successfully refined. From history, the remaining
solvate was likely pentane or toluene in a volume of
588.8 \%A3 per unit cell (19.3%); the remaining peaks
could not be modeled successfully. It appeared that
the cavity area contained about two pentane molecules,
located near the center of symmetry at (0, 1/2, 0).
Modeling with or without restraints was unsuccessful,
as was step by step acquisition of peaks using successive
electron density difference maps. Thus, the structure
factors were modified using the PLATON SQUEEZE technique,
in order to produce a ?solvate-free? structure factor set
(only for the second independent pentane molecule.)
PLATON reported a total electron density of 70 e- per
unit cell, likely representing two pentane molecules,
consistent with our earlier observations. Use of the
SQUEEZE technique resulted in a decrease of ca 1.3 % in R.
;
#===END
data_8
_database_code_depnum_ccdc_archive 'CCDC 776343'
#TrackingRef '- combined_rev.cif'
_audit_creation_date 10-01-31
_audit_creation_method CRYSTALS_ver_14.01
_oxford_structure_analysis_title 'CMT35_0m in P-1'
_chemical_name_systematic ?
_chemical_melting_point ?
_cell_length_a 11.4036(3)
_cell_length_b 12.3007(3)
_cell_length_c 18.7536(5)
_cell_angle_alpha 94.3420(10)
_cell_angle_beta 105.8890(10)
_cell_angle_gamma 108.4810(10)
_cell_volume 2361.24(11)
_symmetry_cell_setting Triclinic
_symmetry_space_group_name_H-M 'P -1 '
_symmetry_space_group_name_Hall '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Co 0.3494 0.9721 12.2841 4.2791 7.3409 0.2784 4.0034 13.5359 2.3488 71.1692
1.0118 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Zr -2.9673 0.5597 17.8765 1.2762 10.9480 11.9160 5.4173 0.1176 3.6572 87.6627
2.0693 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
_cell_formula_units_Z 2
# Given Formula = C45 H79 Co1 N3 P3 Zr1
# Dc = 1.27 Fooo = 964.00 Mu = 7.06 M = 905.22
# Found Formula = C45 H79 Co1 N3 P3 Zr1
# Dc = 1.27 FOOO = 964.00 Mu = 7.06 M = 905.22
_chemical_formula_sum 'C45 H79 Co1 N3 P3 Zr1'
_chemical_formula_moiety 'C45 H79 Co1 N3 P3 Zr1'
_chemical_compound_source ?
_chemical_formula_weight 905.22
_cell_measurement_reflns_used 9855
_cell_measurement_theta_min 3
_cell_measurement_theta_max 30
_cell_measurement_temperature 100
_exptl_crystal_description prism
_exptl_crystal_colour orange
_exptl_crystal_size_min 0.070
_exptl_crystal_size_mid 0.138
_exptl_crystal_size_max 0.302
_exptl_crystal_density_diffrn 1.273
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 964
_exptl_absorpt_coefficient_mu 0.706
# Sheldrick geometric approximatio 0.91 0.95
_exptl_absorpt_correction_type numerical
_exptl_absorpt_process_details
;
Analytical Absorption (De Meulenaer & Tompa, 1965)
;
_exptl_absorpt_correction_T_min 0.91
_exptl_absorpt_correction_T_max 0.95
_diffrn_measurement_device-type 'Bruker Kappa Apex2'
_diffrn_measurement_device Area
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_measurement_method '\f & \w scans'
# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection 'Apex2 (Bruker AXS, 2006)'
_computing_cell_refinement 'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction 'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution 'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material 'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics 'CAMERON (Watkin et al., 1996)'
_diffrn_standards_interval_time .
_diffrn_standards_interval_count .
_diffrn_standards_number 0
_diffrn_standards_decay_% ?
_diffrn_ambient_temperature 100
_diffrn_reflns_number 66346
_reflns_number_total 13803
_diffrn_reflns_av_R_equivalents 0.046
# Number of reflections without Friedels Law is 13891
# Number of reflections with Friedels Law is 13803
# Theoretical number of reflections is about 13851
_diffrn_reflns_theta_min 1.147
_diffrn_reflns_theta_max 30.061
_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full 30.061
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_h_max 16
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_l_min -26
_diffrn_reflns_limit_l_max 26
_reflns_limit_h_min -16
_reflns_limit_h_max 15
_reflns_limit_k_min -17
_reflns_limit_k_max 17
_reflns_limit_l_min 0
_reflns_limit_l_max 26
_oxford_diffrn_Wilson_B_factor 1.04
_oxford_diffrn_Wilson_scale 2.68
_atom_sites_solution_primary direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_diff_density_min -0.58
_refine_diff_density_max 0.74
# The current dictionary definitions do not cover the
# situation where the reflections used for refinement were
# selected by a user-defined sigma threshold
# The values actually used during refinement
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns 13778
_refine_ls_number_restraints 0
_refine_ls_number_parameters 499
_oxford_refine_ls_R_factor_ref 0.0399
_refine_ls_wR_factor_ref 0.0655
_refine_ls_goodness_of_fit_ref 0.9591
_refine_ls_shift/su_max 0.0008121
_refine_ls_shift/su_mean 0.0081071
# The values computed from all data
_oxford_reflns_number_all 13778
_refine_ls_R_factor_all 0.0399
_refine_ls_wR_factor_all 0.0655
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression I>2.0\s(I)
_reflns_number_gt 10842
_refine_ls_R_factor_gt 0.0272
_refine_ls_wR_factor_gt 0.0612
# choose from: rm (reference molecule of known chirality),
# ad (anomolous dispersion - Flack), rmad (rm and ad),
# syn (from synthesis), unk (unknown) or . (not applicable).
_chemical_absolute_configuration .
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_hydrogen_treatment none # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.03P)^2^ + 1.08P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
# Insert your own references if required - in alphabetical order
_publ_section_references
;
Betteridge, P.W., Carruthers, J.R., Cooper, R.I.,
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487.
Bruker Analytical X-ray Systems, Inc., 2006. Apex2,
Version 2 User Manual, M86-E01078, Madison, WI.
De Meulenaer, J. & Tompa, H. (1965). Acta Cryst. 19, 1014.
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical
Crystallography Laboratory, Oxford, UK.
;
# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3
# Replace last . with number of unfound hydrogen atomsattached to an atom.
# ..._refinement_flags_...
# . no refinement constraints S special position constraint on site
# G rigid group refinement of site R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond) P partial occupancy constraint
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_oxford_atom_site_special_shape
_atom_site_attached_hydrogens
Zr1 Zr 0.140181(13) 0.237323(11) 0.247693(7) 0.0097 1.0000 Uani . . . . . . .
Co1 Co 0.230477(18) 0.081965(16) 0.260591(10) 0.0102 1.0000 Uani . . . . . . .
P1 P 0.36821(4) 0.22696(3) 0.23061(2) 0.0114 1.0000 Uani . . . . . . .
P2 P 0.15391(4) 0.09386(3) 0.35460(2) 0.0115 1.0000 Uani . . . . . . .
P3 P 0.23632(9) -0.08277(6) 0.21131(5) 0.0130 0.958(6) Uani . . P 1 1 . .
P301 P 0.206(3) -0.1002(17) 0.2258(13) 0.022(4) 0.042(6) Uiso . . P 1 2 . .
N1 N 0.31577(11) 0.34368(10) 0.23319(7) 0.0120 1.0000 Uani . . . . . . .
N2 N 0.10901(11) 0.21557(10) 0.35125(7) 0.0117 1.0000 Uani . . . . . . .
N3 N -0.03480(12) 0.21668(11) 0.16251(7) 0.0140 1.0000 Uani . . . . . . .
C1 C 0.38302(16) 0.20309(13) 0.13442(9) 0.0173 1.0000 Uani . . . . . . .
C2 C 0.24919(16) 0.13508(14) 0.07644(9) 0.0211 1.0000 Uani . . . . . . .
C3 C 0.47589(17) 0.13793(14) 0.12905(10) 0.0230 1.0000 Uani . . . . . . .
C4 C 0.53972(14) 0.26725(13) 0.29122(9) 0.0156 1.0000 Uani . . . . . . .
C5 C 0.64001(15) 0.36843(13) 0.27293(10) 0.0201 1.0000 Uani . . . . . . .
C6 C 0.55694(15) 0.28109(14) 0.37578(9) 0.0192 1.0000 Uani . . . . . . .
C7 C 0.36851(14) 0.45408(12) 0.21143(8) 0.0122 1.0000 Uani . . . . . . .
C8 C 0.31805(14) 0.47365(12) 0.13768(8) 0.0142 1.0000 Uani . . . . . . .
C9 C 0.37672(15) 0.57915(13) 0.11735(8) 0.0162 1.0000 Uani . . . . . . .
C10 C 0.48309(15) 0.66848(12) 0.16678(9) 0.0161 1.0000 Uani . . . . . . .
C11 C 0.52405(14) 0.65243(12) 0.24051(8) 0.0153 1.0000 Uani . . . . . . .
C12 C 0.46661(14) 0.54959(12) 0.26440(8) 0.0132 1.0000 Uani . . . . . . .
C13 C 0.19990(16) 0.38791(14) 0.07888(9) 0.0219 1.0000 Uani . . . . . . .
C14 C 0.54699(17) 0.77907(14) 0.14120(10) 0.0238 1.0000 Uani . . . . . . .
C15 C 0.50717(15) 0.54897(13) 0.34749(8) 0.0173 1.0000 Uani . . . . . . .
C16 C 0.00405(14) -0.02677(12) 0.35194(9) 0.0161 1.0000 Uani . . . . . . .
C17 C -0.09626(15) -0.06042(14) 0.27357(9) 0.0204 1.0000 Uani . . . . . . .
C18 C 0.03188(17) -0.13554(14) 0.37376(11) 0.0250 1.0000 Uani . . . . . . .
C19 C 0.26426(15) 0.11957(14) 0.45362(8) 0.0166 1.0000 Uani . . . . . . .
C20 C 0.35290(16) 0.04728(15) 0.46793(9) 0.0226 1.0000 Uani . . . . . . .
C21 C 0.19560(18) 0.11164(16) 0.51425(9) 0.0245 1.0000 Uani . . . . . . .
C22 C 0.07579(14) 0.27200(12) 0.40801(8) 0.0123 1.0000 Uani . . . . . . .
C23 C -0.05369(14) 0.23963(12) 0.40947(8) 0.0141 1.0000 Uani . . . . . . .
C24 C -0.07835(15) 0.28900(13) 0.47082(9) 0.0161 1.0000 Uani . . . . . . .
C25 C 0.01841(16) 0.37219(13) 0.52890(8) 0.0166 1.0000 Uani . . . . . . .
C26 C 0.14262(15) 0.41242(13) 0.52211(8) 0.0162 1.0000 Uani . . . . . . .
C27 C 0.17238(14) 0.36586(12) 0.46241(8) 0.0146 1.0000 Uani . . . . . . .
C28 C -0.16791(15) 0.15790(14) 0.34572(9) 0.0196 1.0000 Uani . . . . . . .
C29 C -0.00956(17) 0.42130(14) 0.59588(9) 0.0205 1.0000 Uani . . . . . . .
C30 C 0.30578(16) 0.42055(14) 0.45565(9) 0.0225 1.0000 Uani . . . . . . .
C31 C -0.10762(14) 0.28880(12) 0.14446(8) 0.0126 1.0000 Uani . . . . . . .
C32 C -0.22604(14) 0.25307(13) 0.08486(8) 0.0151 1.0000 Uani . . . . . . .
C33 C -0.29403(15) 0.32914(14) 0.07077(9) 0.0178 1.0000 Uani . . . . . . .
C34 C -0.25004(16) 0.44034(14) 0.11286(9) 0.0192 1.0000 Uani . . . . . . .
C35 C -0.13288(15) 0.47485(13) 0.17101(9) 0.0177 1.0000 Uani . . . . . . .
C36 C -0.06154(14) 0.40155(12) 0.18728(8) 0.0138 1.0000 Uani . . . . . . .
C37 C -0.27847(16) 0.13301(14) 0.03811(9) 0.0214 1.0000 Uani . . . . . . .
C38 C -0.32831(18) 0.51950(16) 0.09773(11) 0.0282 1.0000 Uani . . . . . . .
C39 C 0.06464(15) 0.44127(13) 0.25053(9) 0.0167 1.0000 Uani . . . . . . .
C40 C 0.34848(15) -0.15349(13) 0.26267(9) 0.0186 1.0000 Uani . . . . . . .
C41 C 0.48710(16) -0.06564(14) 0.29603(10) 0.0226 1.0000 Uani . . . . . . .
C42 C 0.30246(18) -0.21475(15) 0.32293(10) 0.0260 1.0000 Uani . . . . . . .
C43 C 0.08459(15) -0.20956(13) 0.16167(9) 0.0199 1.0000 Uani . . . . . . .
C44 C -0.00711(17) -0.16981(15) 0.10210(10) 0.0259 1.0000 Uani . . . . . . .
C45 C 0.10919(18) -0.31198(14) 0.12423(10) 0.0257 1.0000 Uani . . . . . . .
H1 H 0.337(2) 0.085(2) 0.3159(13) 0.044(6) 1.0000 Uiso . . . . . . .
H2 H 0.1056(19) 0.0765(17) 0.1986(11) 0.027(5) 1.0000 Uiso . . . . . . .
H3 H 0.2786(18) -0.0760(16) 0.1522(10) 0.021(5) 1.0000 Uiso . . . . . . .
H4 H -0.0688(19) 0.1561(18) 0.1339(11) 0.023(5) 1.0000 Uiso . . . . . . .
H11 H 0.4169 0.2791 0.1225 0.0211 1.0000 Uiso R . . . . . .
H21 H 0.2222 0.0540 0.0808 0.0316 1.0000 Uiso R . . . . . .
H22 H 0.1830 0.1652 0.0829 0.0308 1.0000 Uiso R . . . . . .
H23 H 0.2526 0.1400 0.0248 0.0306 1.0000 Uiso R . . . . . .
H31 H 0.4677 0.1186 0.0759 0.0347 1.0000 Uiso R . . . . . .
H32 H 0.4534 0.0666 0.1485 0.0349 1.0000 Uiso R . . . . . .
H33 H 0.5644 0.1813 0.1560 0.0338 1.0000 Uiso R . . . . . .
H41 H 0.5581 0.1989 0.2780 0.0176 1.0000 Uiso R . . . . . .
H51 H 0.6363 0.4406 0.2900 0.0291 1.0000 Uiso R . . . . . .
H52 H 0.6254 0.3619 0.2196 0.0303 1.0000 Uiso R . . . . . .
H53 H 0.7277 0.3690 0.2951 0.0305 1.0000 Uiso R . . . . . .
H61 H 0.5272 0.2071 0.3899 0.0311 1.0000 Uiso R . . . . . .
H62 H 0.5142 0.3269 0.3914 0.0316 1.0000 Uiso R . . . . . .
H63 H 0.6456 0.3184 0.4045 0.0310 1.0000 Uiso R . . . . . .
H91 H 0.3411 0.5911 0.0696 0.0183 1.0000 Uiso R . . . . . .
H111 H 0.5910 0.7128 0.2763 0.0173 1.0000 Uiso R . . . . . .
H131 H 0.2230 0.3392 0.0463 0.0338 1.0000 Uiso R . . . . . .
H132 H 0.1433 0.3381 0.1011 0.0321 1.0000 Uiso R . . . . . .
H133 H 0.1531 0.4288 0.0475 0.0339 1.0000 Uiso R . . . . . .
H141 H 0.6105 0.8365 0.1819 0.0368 1.0000 Uiso R . . . . . .
H142 H 0.4845 0.8112 0.1171 0.0376 1.0000 Uiso R . . . . . .
H143 H 0.5885 0.7674 0.1055 0.0377 1.0000 Uiso R . . . . . .
H151 H 0.5979 0.5832 0.3698 0.0278 1.0000 Uiso R . . . . . .
H152 H 0.4800 0.4725 0.3582 0.0264 1.0000 Uiso R . . . . . .
H153 H 0.4703 0.5931 0.3711 0.0269 1.0000 Uiso R . . . . . .
H161 H -0.0300 0.0029 0.3885 0.0189 1.0000 Uiso R . . . . . .
H171 H -0.0684 -0.1021 0.2387 0.0300 1.0000 Uiso R . . . . . .
H172 H -0.1061 0.0077 0.2537 0.0295 1.0000 Uiso R . . . . . .
H173 H -0.1796 -0.1118 0.2763 0.0316 1.0000 Uiso R . . . . . .
H181 H 0.0743 -0.1594 0.3414 0.0357 1.0000 Uiso R . . . . . .
H182 H 0.0868 -0.1224 0.4255 0.0363 1.0000 Uiso R . . . . . .
H183 H -0.0494 -0.1983 0.3675 0.0371 1.0000 Uiso R . . . . . .
H191 H 0.3217 0.2001 0.4594 0.0193 1.0000 Uiso R . . . . . .
H201 H 0.3045 -0.0317 0.4689 0.0333 1.0000 Uiso R . . . . . .
H202 H 0.3965 0.0468 0.4303 0.0326 1.0000 Uiso R . . . . . .
H203 H 0.4189 0.0793 0.5165 0.0331 1.0000 Uiso R . . . . . .
H211 H 0.2604 0.1428 0.5629 0.0371 1.0000 Uiso R . . . . . .
H212 H 0.1462 0.0310 0.5138 0.0364 1.0000 Uiso R . . . . . .
H213 H 0.1352 0.1533 0.5072 0.0352 1.0000 Uiso R . . . . . .
H241 H -0.1624 0.2662 0.4725 0.0190 1.0000 Uiso R . . . . . .
H261 H 0.2081 0.4722 0.5578 0.0196 1.0000 Uiso R . . . . . .
H281 H -0.1844 0.0776 0.3512 0.0282 1.0000 Uiso R . . . . . .
H282 H -0.1526 0.1673 0.2987 0.0276 1.0000 Uiso R . . . . . .
H283 H -0.2454 0.1742 0.3447 0.0286 1.0000 Uiso R . . . . . .
H291 H 0.0096 0.5006 0.6001 0.0311 1.0000 Uiso R . . . . . .
H292 H 0.0401 0.4086 0.6416 0.0319 1.0000 Uiso R . . . . . .
H293 H -0.0983 0.3883 0.5918 0.0317 1.0000 Uiso R . . . . . .
H301 H 0.3102 0.4055 0.4081 0.0367 1.0000 Uiso R . . . . . .
H302 H 0.3419 0.5005 0.4736 0.0364 1.0000 Uiso R . . . . . .
H303 H 0.3655 0.3906 0.4848 0.0371 1.0000 Uiso R . . . . . .
H331 H -0.3756 0.3028 0.0318 0.0202 1.0000 Uiso R . . . . . .
H351 H -0.1015 0.5483 0.2000 0.0204 1.0000 Uiso R . . . . . .
H371 H -0.2163 0.1213 0.0147 0.0309 1.0000 Uiso R . . . . . .
H372 H -0.3587 0.1217 -0.0007 0.0316 1.0000 Uiso R . . . . . .
H373 H -0.2954 0.0737 0.0693 0.0319 1.0000 Uiso R . . . . . .
H381 H -0.3969 0.5033 0.1188 0.0452 1.0000 Uiso R . . . . . .
H382 H -0.2755 0.5957 0.1168 0.0456 1.0000 Uiso R . . . . . .
H383 H -0.3664 0.5186 0.0458 0.0451 1.0000 Uiso R . . . . . .
H391 H 0.1356 0.4373 0.2317 0.0235 1.0000 Uiso R . . . . . .
H392 H 0.0878 0.5218 0.2742 0.0238 1.0000 Uiso R . . . . . .
H393 H 0.0608 0.3947 0.2892 0.0245 1.0000 Uiso R . . . . . .
H401 H 0.3468 -0.2120 0.2248 0.0209 1.0000 Uiso R . . . . . .
H411 H 0.5180 -0.0300 0.2567 0.0333 1.0000 Uiso R . . . . . .
H412 H 0.5464 -0.1044 0.3193 0.0337 1.0000 Uiso R . . . . . .
H413 H 0.4920 -0.0061 0.3334 0.0330 1.0000 Uiso R . . . . . .
H421 H 0.3582 -0.2553 0.3439 0.0393 1.0000 Uiso R . . . . . .
H422 H 0.3036 -0.1610 0.3628 0.0370 1.0000 Uiso R . . . . . .
H423 H 0.2159 -0.2700 0.3032 0.0380 1.0000 Uiso R . . . . . .
H431 H 0.0399 -0.2375 0.1986 0.0239 1.0000 Uiso R . . . . . .
H441 H -0.0913 -0.2312 0.0785 0.0384 1.0000 Uiso R . . . . . .
H442 H -0.0197 -0.1023 0.1229 0.0378 1.0000 Uiso R . . . . . .
H443 H 0.0304 -0.1512 0.0626 0.0366 1.0000 Uiso R . . . . . .
H451 H 0.1578 -0.2852 0.0917 0.0351 1.0000 Uiso R . . . . . .
H452 H 0.0262 -0.3710 0.0962 0.0363 1.0000 Uiso R . . . . . .
H453 H 0.1559 -0.3455 0.1608 0.0372 1.0000 Uiso R . . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zr1 0.01072(6) 0.00952(6) 0.01001(6) 0.00212(5) 0.00306(5) 0.00502(5)
Co1 0.01075(9) 0.00956(8) 0.01109(9) 0.00206(7) 0.00320(7) 0.00469(7)
P1 0.01216(16) 0.01089(15) 0.01263(16) 0.00250(13) 0.00502(13) 0.00508(13)
P2 0.01276(16) 0.01207(16) 0.01205(16) 0.00412(13) 0.00472(13) 0.00625(13)
P3 0.0139(3) 0.0101(2) 0.0159(3) 0.00160(17) 0.0053(2) 0.00520(19)
N1 0.0135(6) 0.0105(5) 0.0130(6) 0.0024(4) 0.0048(5) 0.0050(4)
N2 0.0128(5) 0.0121(5) 0.0124(5) 0.0020(4) 0.0051(4) 0.0063(4)
N3 0.0152(6) 0.0121(6) 0.0139(6) -0.0003(5) 0.0010(5) 0.0075(5)
C1 0.0245(8) 0.0141(7) 0.0177(7) 0.0045(6) 0.0119(6) 0.0077(6)
C2 0.0283(8) 0.0217(7) 0.0134(7) 0.0021(6) 0.0059(6) 0.0095(6)
C3 0.0263(8) 0.0195(7) 0.0286(9) 0.0020(6) 0.0179(7) 0.0077(6)
C4 0.0118(6) 0.0138(6) 0.0223(7) 0.0036(6) 0.0054(6) 0.0058(5)
C5 0.0143(7) 0.0185(7) 0.0287(8) 0.0035(6) 0.0091(6) 0.0054(6)
C6 0.0175(7) 0.0188(7) 0.0182(7) 0.0030(6) 0.0002(6) 0.0071(6)
C7 0.0132(6) 0.0116(6) 0.0143(6) 0.0031(5) 0.0065(5) 0.0058(5)
C8 0.0150(7) 0.0141(6) 0.0153(7) 0.0033(5) 0.0052(5) 0.0069(5)
C9 0.0199(7) 0.0167(7) 0.0148(7) 0.0058(5) 0.0057(6) 0.0093(6)
C10 0.0184(7) 0.0125(6) 0.0212(7) 0.0056(6) 0.0092(6) 0.0076(5)
C11 0.0157(7) 0.0123(6) 0.0183(7) 0.0017(5) 0.0056(6) 0.0055(5)
C12 0.0145(7) 0.0132(6) 0.0139(6) 0.0025(5) 0.0048(5) 0.0073(5)
C13 0.0235(8) 0.0189(7) 0.0165(7) 0.0054(6) 0.0002(6) 0.0031(6)
C14 0.0274(9) 0.0166(7) 0.0241(8) 0.0075(6) 0.0079(7) 0.0026(6)
C15 0.0205(7) 0.0151(7) 0.0151(7) 0.0024(5) 0.0044(6) 0.0059(6)
C16 0.0169(7) 0.0137(6) 0.0215(7) 0.0060(6) 0.0100(6) 0.0063(5)
C17 0.0166(7) 0.0166(7) 0.0251(8) 0.0006(6) 0.0069(6) 0.0025(6)
C18 0.0266(9) 0.0185(7) 0.0374(10) 0.0143(7) 0.0163(8) 0.0107(7)
C19 0.0187(7) 0.0204(7) 0.0130(6) 0.0050(6) 0.0047(6) 0.0097(6)
C20 0.0232(8) 0.0311(9) 0.0189(7) 0.0100(7) 0.0052(6) 0.0168(7)
C21 0.0339(9) 0.0334(9) 0.0156(7) 0.0104(7) 0.0105(7) 0.0208(8)
C22 0.0161(7) 0.0135(6) 0.0109(6) 0.0042(5) 0.0056(5) 0.0083(5)
C23 0.0143(7) 0.0130(6) 0.0167(7) 0.0043(5) 0.0046(5) 0.0069(5)
C24 0.0163(7) 0.0177(7) 0.0202(7) 0.0074(6) 0.0102(6) 0.0093(6)
C25 0.0257(8) 0.0162(7) 0.0155(7) 0.0067(6) 0.0111(6) 0.0128(6)
C26 0.0214(7) 0.0134(6) 0.0130(7) 0.0010(5) 0.0047(6) 0.0059(6)
C27 0.0152(7) 0.0154(6) 0.0145(7) 0.0040(5) 0.0056(5) 0.0062(5)
C28 0.0139(7) 0.0215(7) 0.0223(8) -0.0003(6) 0.0034(6) 0.0077(6)
C29 0.0320(9) 0.0197(7) 0.0179(7) 0.0047(6) 0.0145(7) 0.0139(7)
C30 0.0181(7) 0.0231(8) 0.0217(8) -0.0030(6) 0.0087(6) 0.0007(6)
C31 0.0142(6) 0.0144(6) 0.0125(6) 0.0053(5) 0.0062(5) 0.0070(5)
C32 0.0150(7) 0.0192(7) 0.0127(6) 0.0048(5) 0.0050(5) 0.0073(6)
C33 0.0146(7) 0.0267(8) 0.0165(7) 0.0103(6) 0.0058(6) 0.0106(6)
C34 0.0219(8) 0.0242(8) 0.0224(8) 0.0140(6) 0.0129(6) 0.0155(6)
C35 0.0230(8) 0.0166(7) 0.0209(7) 0.0075(6) 0.0131(6) 0.0108(6)
C36 0.0146(7) 0.0148(6) 0.0143(6) 0.0042(5) 0.0062(5) 0.0064(5)
C37 0.0178(7) 0.0232(8) 0.0185(7) -0.0011(6) -0.0001(6) 0.0072(6)
C38 0.0332(10) 0.0337(9) 0.0331(9) 0.0157(8) 0.0152(8) 0.0260(8)
C39 0.0203(7) 0.0132(6) 0.0172(7) 0.0016(5) 0.0042(6) 0.0085(6)
C40 0.0208(7) 0.0155(7) 0.0224(8) 0.0029(6) 0.0065(6) 0.0107(6)
C41 0.0194(8) 0.0213(8) 0.0284(9) 0.0027(7) 0.0040(7) 0.0120(6)
C42 0.0321(9) 0.0215(8) 0.0310(9) 0.0102(7) 0.0116(8) 0.0153(7)
C43 0.0203(8) 0.0149(7) 0.0218(8) -0.0008(6) 0.0070(6) 0.0034(6)
C44 0.0231(8) 0.0219(8) 0.0246(8) -0.0040(7) -0.0009(7) 0.0064(7)
C45 0.0299(9) 0.0155(7) 0.0294(9) -0.0025(7) 0.0098(7) 0.0060(7)
_refine_ls_extinction_method None
_oxford_refine_ls_scale 0.125626(18)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Zr1 . Co1 . 2.4397(2) yes
Zr1 . P1 . 2.7460(4) yes
Zr1 . P2 . 2.7745(4) yes
Zr1 . N1 . 2.1180(12) yes
Zr1 . N2 . 2.0895(12) yes
Zr1 . N3 . 2.1142(12) yes
Zr1 . C39 . 2.9005(15) yes
Zr1 . H2 . 1.987(19) no
Co1 . P1 . 2.1963(4) yes
Co1 . P2 . 2.1856(4) yes
Co1 . P3 . 2.1910(5) yes
Co1 . H1 . 1.36(2) no
Co1 . H2 . 1.551(19) no
Co1 . P1 . 2.1963(4) yes
Co1 . P2 . 2.1856(4) yes
Co1 . P301 . 2.194(15) yes
Co1 . H1 . 1.36(2) no
Co1 . H2 . 1.551(19) no
P1 . N1 . 1.7236(12) yes
P1 . C1 . 1.8673(15) yes
P1 . C4 . 1.8563(15) yes
P2 . N2 . 1.7292(12) yes
P2 . C16 . 1.8598(15) yes
P2 . C19 . 1.8737(15) yes
P3 . C40 . 1.8649(16) yes
P3 . C43 . 1.8655(17) yes
P3 . H3 . 1.322(19) no
P301 . C40 . 1.913(17) yes
P301 . C43 . 1.686(17) yes
N1 . C7 . 1.4397(17) yes
N2 . C22 . 1.4263(18) yes
N3 . C31 . 1.3964(18) yes
N3 . H4 . 0.80(2) no
C1 . C2 . 1.535(2) yes
C1 . C3 . 1.536(2) yes
C1 . H11 . 0.961 no
C2 . H21 . 0.963 no
C2 . H22 . 0.972 no
C2 . H23 . 0.986 no
C3 . H31 . 0.978 no
C3 . H32 . 0.962 no
C3 . H33 . 0.947 no
C4 . C5 . 1.534(2) yes
C4 . C6 . 1.533(2) yes
C4 . H41 . 0.960 no
C5 . H51 . 0.939 no
C5 . H52 . 0.961 no
C5 . H53 . 0.969 no
C6 . H61 . 0.951 no
C6 . H62 . 0.932 no
C6 . H63 . 0.945 no
C7 . C8 . 1.416(2) yes
C7 . C12 . 1.4142(19) yes
C8 . C9 . 1.393(2) yes
C8 . C13 . 1.501(2) yes
C9 . C10 . 1.387(2) yes
C9 . H91 . 0.921 no
C10 . C11 . 1.384(2) yes
C10 . C14 . 1.508(2) yes
C11 . C12 . 1.397(2) yes
C11 . H111 . 0.932 no
C12 . C15 . 1.501(2) yes
C13 . H131 . 0.966 no
C13 . H132 . 0.949 no
C13 . H133 . 0.963 no
C14 . H141 . 0.947 no
C14 . H142 . 0.948 no
C14 . H143 . 0.946 no
C15 . H151 . 0.940 no
C15 . H152 . 0.949 no
C15 . H153 . 0.937 no
C16 . C17 . 1.525(2) yes
C16 . C18 . 1.530(2) yes
C16 . H161 . 0.976 no
C17 . H171 . 0.979 no
C17 . H172 . 0.968 no
C17 . H173 . 0.977 no
C18 . H181 . 0.956 no
C18 . H182 . 0.969 no
C18 . H183 . 0.971 no
C19 . C20 . 1.530(2) yes
C19 . C21 . 1.540(2) yes
C19 . H191 . 0.978 no
C20 . H201 . 0.957 no
C20 . H202 . 0.969 no
C20 . H203 . 0.966 no
C21 . H211 . 0.961 no
C21 . H212 . 0.971 no
C21 . H213 . 0.969 no
C22 . C23 . 1.411(2) yes
C22 . C27 . 1.410(2) yes
C23 . C24 . 1.397(2) yes
C23 . C28 . 1.507(2) yes
C24 . C25 . 1.381(2) yes
C24 . H241 . 0.919 no
C25 . C26 . 1.390(2) yes
C25 . C29 . 1.507(2) yes
C26 . C27 . 1.390(2) yes
C26 . H261 . 0.922 no
C27 . C30 . 1.501(2) yes
C28 . H281 . 0.964 no
C28 . H282 . 0.953 no
C28 . H283 . 0.961 no
C29 . H291 . 0.921 no
C29 . H292 . 0.944 no
C29 . H293 . 0.942 no
C30 . H301 . 0.914 no
C30 . H302 . 0.931 no
C30 . H303 . 0.940 no
C31 . C32 . 1.410(2) yes
C31 . C36 . 1.408(2) yes
C32 . C33 . 1.390(2) yes
C32 . C37 . 1.505(2) yes
C33 . C34 . 1.389(2) yes
C33 . H331 . 0.951 no
C34 . C35 . 1.388(2) yes
C34 . C38 . 1.510(2) yes
C35 . C36 . 1.392(2) yes
C35 . H351 . 0.924 no
C36 . C39 . 1.499(2) yes
C37 . H371 . 0.970 no
C37 . H372 . 0.962 no
C37 . H373 . 0.974 no
C38 . H381 . 0.944 no
C38 . H382 . 0.918 no
C38 . H383 . 0.950 no
C39 . H391 . 0.981 no
C39 . H392 . 0.975 no
C39 . H393 . 0.960 no
C40 . C41 . 1.527(2) yes
C40 . C42 . 1.524(2) yes
C40 . H401 . 0.964 no
C40 . C41 . 1.527(2) yes
C40 . C42 . 1.524(2) yes
C40 . H401 . 0.964 no
C41 . H411 . 0.977 no
C41 . H412 . 0.975 no
C41 . H413 . 0.952 no
C42 . H421 . 0.950 no
C42 . H422 . 0.954 no
C42 . H423 . 0.954 no
C43 . C44 . 1.532(2) yes
C43 . C45 . 1.535(2) yes
C43 . H431 . 0.988 no
C43 . C44 . 1.532(2) yes
C43 . C45 . 1.535(2) yes
C43 . H431 . 0.988 no
C44 . H441 . 0.972 no
C44 . H442 . 0.958 no
C44 . H443 . 0.960 no
C45 . H451 . 0.943 no
C45 . H452 . 0.966 no
C45 . H453 . 0.951 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Co1 . Zr1 . P1 . 49.684(9) yes
Co1 . Zr1 . P2 . 49.049(9) yes
P1 . Zr1 . P2 . 89.898(11) yes
Co1 . Zr1 . N1 . 88.20(3) yes
P2 . Zr1 . N1 . 118.54(3) yes
Co1 . Zr1 . N2 . 87.20(3) yes
P1 . Zr1 . N2 . 118.16(3) yes
N1 . Zr1 . N2 . 125.37(5) yes
Co1 . Zr1 . N3 . 121.90(3) yes
P1 . Zr1 . N3 . 128.01(4) yes
P2 . Zr1 . N3 . 122.85(4) yes
N1 . Zr1 . N3 . 116.87(5) yes
N2 . Zr1 . N3 . 111.41(5) yes
Co1 . Zr1 . C39 . 171.86(3) yes
P1 . Zr1 . C39 . 126.44(3) yes
P2 . Zr1 . C39 . 128.09(3) yes
N1 . Zr1 . C39 . 87.57(4) yes
N2 . Zr1 . C39 . 89.59(4) yes
P1 . Zr1 . H2 . 71.8(6) no
P2 . Zr1 . H2 . 69.9(6) no
N1 . Zr1 . H2 . 106.3(6) no
N2 . Zr1 . H2 . 103.7(6) no
N3 . Zr1 . C39 . 66.24(4) yes
N3 . Zr1 . H2 . 82.6(6) no
C39 . Zr1 . H2 . 148.8(6) no
Zr1 . Co1 . P1 . 72.430(11) yes
Zr1 . Co1 . P2 . 73.487(11) yes
P1 . Co1 . P2 . 125.761(16) yes
Zr1 . Co1 . P3 . 148.937(16) yes
P1 . Co1 . P3 . 109.07(4) yes
P2 . Co1 . P3 . 121.76(4) yes
Zr1 . Co1 . H1 . 125.9(10) no
P1 . Co1 . H1 . 84.4(9) no
P2 . Co1 . H1 . 82.9(10) no
P3 . Co1 . H1 . 84.5(10) no
Zr1 . Co1 . H2 . 54.4(7) no
P1 . Co1 . H2 . 97.3(7) no
P2 . Co1 . H2 . 95.7(7) no
P3 . Co1 . H2 . 95.4(7) no
H1 . Co1 . H2 . 178.3(12) no
Zr1 . Co1 . P1 . 72.430(11) yes
Zr1 . Co1 . P2 . 73.487(11) yes
P1 . Co1 . P2 . 125.761(16) yes
Zr1 . Co1 . P301 . 148.4(4) yes
P1 . Co1 . P301 . 122.1(10) yes
P2 . Co1 . P301 . 109.0(9) yes
Zr1 . Co1 . H1 . 125.9(10) no
P1 . Co1 . H1 . 84.4(9) no
P2 . Co1 . H1 . 82.9(10) no
P301 . Co1 . H1 . 85.2(10) no
P1 . Co1 . H2 . 97.3(7) no
P2 . Co1 . H2 . 95.7(7) no
P301 . Co1 . H2 . 94.4(8) no
H1 . Co1 . H2 . 178.3(12) no
Zr1 . P1 . Co1 . 57.885(10) yes
Zr1 . P1 . N1 . 50.47(4) yes
Co1 . P1 . N1 . 107.83(4) yes
Zr1 . P1 . C1 . 120.18(5) yes
Co1 . P1 . C1 . 116.65(5) yes
N1 . P1 . C1 . 105.18(6) yes
Zr1 . P1 . C4 . 136.77(5) yes
Co1 . P1 . C4 . 113.78(5) yes
N1 . P1 . C4 . 111.34(6) yes
C1 . P1 . C4 . 101.71(7) yes
Zr1 . P2 . Co1 . 57.464(10) yes
Zr1 . P2 . N2 . 48.79(4) yes
Co1 . P2 . N2 . 105.76(4) yes
Zr1 . P2 . C16 . 119.32(5) yes
Co1 . P2 . C16 . 117.34(5) yes
N2 . P2 . C16 . 104.60(6) yes
Zr1 . P2 . C19 . 132.02(5) yes
Co1 . P2 . C19 . 119.63(5) yes
N2 . P2 . C19 . 103.57(6) yes
C16 . P2 . C19 . 104.18(7) yes
Co1 . P3 . C40 . 122.42(5) yes
Co1 . P3 . C43 . 121.80(7) yes
C40 . P3 . C43 . 102.67(8) yes
Co1 . P3 . H3 . 113.9(8) no
C40 . P3 . H3 . 95.6(8) no
C43 . P3 . H3 . 94.1(8) no
Co1 . P301 . C40 . 119.9(9) yes
Co1 . P301 . C43 . 131.8(8) yes
C40 . P301 . C43 . 107.9(7) yes
P1 . N1 . Zr1 . 90.66(5) yes
P1 . N1 . C7 . 127.73(9) yes
Zr1 . N1 . C7 . 139.46(9) yes
P2 . N2 . Zr1 . 92.71(5) yes
P2 . N2 . C22 . 126.99(9) yes
Zr1 . N2 . C22 . 140.12(9) yes
Zr1 . N3 . C31 . 133.16(10) yes
Zr1 . N3 . H4 . 116.6(14) no
C31 . N3 . H4 . 110.3(14) no
P1 . C1 . C2 . 110.64(11) yes
P1 . C1 . C3 . 113.72(11) yes
C2 . C1 . C3 . 108.36(13) yes
P1 . C1 . H11 . 106.3 no
C2 . C1 . H11 . 109.3 no
C3 . C1 . H11 . 108.4 no
C1 . C2 . H21 . 110.5 no
C1 . C2 . H22 . 111.8 no
H21 . C2 . H22 . 108.4 no
C1 . C2 . H23 . 110.6 no
H21 . C2 . H23 . 107.7 no
H22 . C2 . H23 . 107.7 no
C1 . C3 . H31 . 108.3 no
C1 . C3 . H32 . 110.9 no
H31 . C3 . H32 . 108.3 no
C1 . C3 . H33 . 113.7 no
H31 . C3 . H33 . 108.6 no
H32 . C3 . H33 . 106.9 no
P1 . C4 . C5 . 115.95(11) yes
P1 . C4 . C6 . 113.85(10) yes
C5 . C4 . C6 . 111.72(12) yes
P1 . C4 . H41 . 101.3 no
C5 . C4 . H41 . 105.8 no
C6 . C4 . H41 . 106.9 no
C4 . C5 . H51 . 111.6 no
C4 . C5 . H52 . 111.4 no
H51 . C5 . H52 . 107.2 no
C4 . C5 . H53 . 111.2 no
H51 . C5 . H53 . 108.9 no
H52 . C5 . H53 . 106.3 no
C4 . C6 . H61 . 110.6 no
C4 . C6 . H62 . 114.0 no
H61 . C6 . H62 . 108.4 no
C4 . C6 . H63 . 110.9 no
H61 . C6 . H63 . 107.7 no
H62 . C6 . H63 . 105.1 no
N1 . C7 . C8 . 121.34(12) yes
N1 . C7 . C12 . 121.14(12) yes
C8 . C7 . C12 . 117.38(12) yes
C7 . C8 . C9 . 119.67(13) yes
C7 . C8 . C13 . 123.82(13) yes
C9 . C8 . C13 . 116.48(13) yes
C8 . C9 . C10 . 122.90(14) yes
C8 . C9 . H91 . 118.4 no
C10 . C9 . H91 . 118.6 no
C9 . C10 . C11 . 116.81(13) yes
C9 . C10 . C14 . 120.97(14) yes
C11 . C10 . C14 . 122.18(14) yes
C10 . C11 . C12 . 122.53(14) yes
C10 . C11 . H111 . 119.4 no
C12 . C11 . H111 . 118.1 no
C7 . C12 . C11 . 119.91(13) yes
C7 . C12 . C15 . 122.68(13) yes
C11 . C12 . C15 . 117.29(13) yes
C8 . C13 . H131 . 111.8 no
C8 . C13 . H132 . 111.4 no
H131 . C13 . H132 . 107.5 no
C8 . C13 . H133 . 109.8 no
H131 . C13 . H133 . 107.3 no
H132 . C13 . H133 . 108.9 no
C10 . C14 . H141 . 112.0 no
C10 . C14 . H142 . 110.9 no
H141 . C14 . H142 . 107.7 no
C10 . C14 . H143 . 113.1 no
H141 . C14 . H143 . 107.2 no
H142 . C14 . H143 . 105.6 no
C12 . C15 . H151 . 111.8 no
C12 . C15 . H152 . 111.9 no
H151 . C15 . H152 . 108.4 no
C12 . C15 . H153 . 109.6 no
H151 . C15 . H153 . 106.6 no
H152 . C15 . H153 . 108.3 no
P2 . C16 . C17 . 110.87(10) yes
P2 . C16 . C18 . 112.39(11) yes
C17 . C16 . C18 . 108.34(13) yes
P2 . C16 . H161 . 105.9 no
C17 . C16 . H161 . 110.2 no
C18 . C16 . H161 . 109.2 no
C16 . C17 . H171 . 110.0 no
C16 . C17 . H172 . 111.3 no
H171 . C17 . H172 . 107.4 no
C16 . C17 . H173 . 109.0 no
H171 . C17 . H173 . 108.7 no
H172 . C17 . H173 . 110.3 no
C16 . C18 . H181 . 109.1 no
C16 . C18 . H182 . 112.6 no
H181 . C18 . H182 . 108.5 no
C16 . C18 . H183 . 109.8 no
H181 . C18 . H183 . 108.5 no
H182 . C18 . H183 . 108.2 no
P2 . C19 . C20 . 115.95(11) yes
P2 . C19 . C21 . 114.70(11) yes
C20 . C19 . C21 . 109.01(12) yes
P2 . C19 . H191 . 101.5 no
C20 . C19 . H191 . 106.0 no
C21 . C19 . H191 . 108.8 no
C19 . C20 . H201 . 110.9 no
C19 . C20 . H202 . 112.7 no
H201 . C20 . H202 . 108.2 no
C19 . C20 . H203 . 109.2 no
H201 . C20 . H203 . 107.7 no
H202 . C20 . H203 . 108.0 no
C19 . C21 . H211 . 108.8 no
C19 . C21 . H212 . 110.4 no
H211 . C21 . H212 . 108.3 no
C19 . C21 . H213 . 113.1 no
H211 . C21 . H213 . 108.9 no
H212 . C21 . H213 . 107.1 no
N2 . C22 . C23 . 121.55(12) yes
N2 . C22 . C27 . 119.97(13) yes
C23 . C22 . C27 . 118.42(13) yes
C22 . C23 . C24 . 118.96(13) yes
C22 . C23 . C28 . 122.69(13) yes
C24 . C23 . C28 . 118.29(13) yes
C23 . C24 . C25 . 122.62(14) yes
C23 . C24 . H241 . 119.0 no
C25 . C24 . H241 . 118.4 no
C24 . C25 . C26 . 117.39(13) yes
C24 . C25 . C29 . 121.74(14) yes
C26 . C25 . C29 . 120.83(14) yes
C25 . C26 . C27 . 122.10(14) yes
C25 . C26 . H261 . 119.8 no
C27 . C26 . H261 . 118.1 no
C22 . C27 . C26 . 119.65(13) yes
C22 . C27 . C30 . 121.45(13) yes
C26 . C27 . C30 . 118.85(13) yes
C23 . C28 . H281 . 111.8 no
C23 . C28 . H282 . 110.3 no
H281 . C28 . H282 . 108.6 no
C23 . C28 . H283 . 109.9 no
H281 . C28 . H283 . 107.5 no
H282 . C28 . H283 . 108.5 no
C25 . C29 . H291 . 111.5 no
C25 . C29 . H292 . 112.0 no
H291 . C29 . H292 . 106.8 no
C25 . C29 . H293 . 111.4 no
H291 . C29 . H293 . 106.6 no
H292 . C29 . H293 . 108.2 no
C27 . C30 . H301 . 114.1 no
C27 . C30 . H302 . 113.2 no
H301 . C30 . H302 . 109.6 no
C27 . C30 . H303 . 111.4 no
H301 . C30 . H303 . 103.3 no
H302 . C30 . H303 . 104.4 no
N3 . C31 . C32 . 122.51(13) yes
N3 . C31 . C36 . 118.97(13) yes
C32 . C31 . C36 . 118.52(13) yes
C31 . C32 . C33 . 119.30(14) yes
C31 . C32 . C37 . 119.96(13) yes
C33 . C32 . C37 . 120.74(13) yes
C32 . C33 . C34 . 122.76(14) yes
C32 . C33 . H331 . 118.5 no
C34 . C33 . H331 . 118.7 no
C33 . C34 . C35 . 117.41(14) yes
C33 . C34 . C38 . 121.48(15) yes
C35 . C34 . C38 . 121.08(15) yes
C34 . C35 . C36 . 121.84(14) yes
C34 . C35 . H351 . 119.2 no
C36 . C35 . H351 . 118.9 no
C31 . C36 . C35 . 120.17(13) yes
C31 . C36 . C39 . 119.23(13) yes
C35 . C36 . C39 . 120.59(13) yes
C32 . C37 . H371 . 110.8 no
C32 . C37 . H372 . 110.5 no
H371 . C37 . H372 . 108.8 no
C32 . C37 . H373 . 110.6 no
H371 . C37 . H373 . 107.8 no
H372 . C37 . H373 . 108.3 no
C34 . C38 . H381 . 114.0 no
C34 . C38 . H382 . 110.4 no
H381 . C38 . H382 . 107.2 no
C34 . C38 . H383 . 114.0 no
H381 . C38 . H383 . 106.2 no
H382 . C38 . H383 . 104.4 no
C36 . C39 . Zr1 . 102.35(9) yes
C36 . C39 . H391 . 110.4 no
Zr1 . C39 . H391 . 57.6 no
C36 . C39 . H392 . 111.3 no
Zr1 . C39 . H392 . 146.3 no
H391 . C39 . H392 . 107.4 no
C36 . C39 . H393 . 112.0 no
Zr1 . C39 . H393 . 58.7 no
H391 . C39 . H393 . 108.3 no
H392 . C39 . H393 . 107.2 no
P3 . C40 . C41 . 110.75(11) yes
P3 . C40 . C42 . 112.89(12) yes
C41 . C40 . C42 . 111.03(14) yes
P3 . C40 . H401 . 105.0 no
C41 . C40 . H401 . 109.1 no
C42 . C40 . H401 . 107.8 no
P301 . C40 . C41 . 119.9(7) yes
P301 . C40 . C42 . 97.8(11) yes
C41 . C40 . C42 . 111.03(14) yes
P301 . C40 . H401 . 110.2 no
C41 . C40 . H401 . 109.1 no
C42 . C40 . H401 . 107.8 no
C40 . C41 . H411 . 110.7 no
C40 . C41 . H412 . 110.3 no
H411 . C41 . H412 . 107.1 no
C40 . C41 . H413 . 111.3 no
H411 . C41 . H413 . 109.1 no
H412 . C41 . H413 . 108.2 no
C40 . C42 . H421 . 109.4 no
C40 . C42 . H422 . 111.9 no
H421 . C42 . H422 . 108.1 no
C40 . C42 . H423 . 112.3 no
H421 . C42 . H423 . 107.8 no
H422 . C42 . H423 . 107.2 no
P3 . C43 . C44 . 109.30(11) yes
P3 . C43 . C45 . 113.63(12) yes
C44 . C43 . C45 . 109.41(14) yes
P3 . C43 . H431 . 108.6 no
C44 . C43 . H431 . 107.5 no
C45 . C43 . H431 . 108.2 no
P301 . C43 . C44 . 114.5(6) yes
P301 . C43 . C45 . 121.5(7) yes
C44 . C43 . C45 . 109.41(14) yes
P301 . C43 . H431 . 93.5 no
C44 . C43 . H431 . 107.5 no
C45 . C43 . H431 . 108.2 no
C43 . C44 . H441 . 112.1 no
C43 . C44 . H442 . 111.6 no
H441 . C44 . H442 . 109.3 no
C43 . C44 . H443 . 108.6 no
H441 . C44 . H443 . 106.3 no
H442 . C44 . H443 . 108.8 no
C43 . C45 . H451 . 109.1 no
C43 . C45 . H452 . 108.7 no
H451 . C45 . H452 . 110.3 no
C43 . C45 . H453 . 111.3 no
H451 . C45 . H453 . 109.1 no
H452 . C45 . H453 . 108.4 no
Zr1 . H2 . Co1 . 86.3(9) no
#===END