# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_e16msh4
_database_code_depnum_ccdc_archive 'CCDC 1498668'
_audit_update_record             
;
2016-08-10 deposited with the CCDC.
2016-10-31 downloaded from the CCDC.
;
_audit_creation_date             2016-03-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C29 H60 N4 O3 Zr'
_chemical_formula_sum            'C29 H60 N4 O3 Zr'
_chemical_formula_weight         604.03
_chemical_melting_point          ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   10.8077(5)
_cell_length_b                   17.3778(8)
_cell_length_c                   18.1390(9)
_cell_angle_alpha                90
_cell_angle_beta                 90.090(4)
_cell_angle_gamma                90
_cell_volume                     3406.7(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7499
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      25.8560
_cell_measurement_theta_min      3.5600
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.354
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97059
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.

Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1304


_exptl_crystal_size_max          0.214
_exptl_crystal_size_mid          0.197
_exptl_crystal_size_min          0.132

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0506
_diffrn_reflns_av_unetI/netI     0.0579
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25934
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.068
_diffrn_reflns_theta_min         3.369
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1468
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -18.00   9.00   1.00   75.00    --  -14.16 -99.00  90.00   27
  2  ω    -41.00  51.00   1.00   75.00    --  -14.16  77.00  60.00   92
  3  ω    -82.00  13.00   1.00   75.00    --  -14.16 -77.00 -60.00   95
  4  ω     -7.00  22.00   1.00   75.00    --  -14.16 -99.00-180.00   29
  5  ω    -27.00  49.00   1.00   75.00    --  -14.16  38.00-150.00   76
  6  ω     -1.00  24.00   1.00   75.00    --   14.79  57.00-150.00   25
  7  ω     34.00  59.00   1.00   75.00    --   14.79-178.00-180.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5467
_reflns_number_total             6663
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         1.410
_refine_diff_density_min         -0.452
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         6663
_refine_ls_number_restraints     195
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0521
_refine_ls_restrained_S_all      1.019
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0751P)²+2.2605P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1245
_refine_ls_wR_factor_ref         0.1360
_refine_special_details          
;
 Refined as a 2-component twin.
Twinning about the 0,0,1 direction accounted for in this refinement. 
Atoms N4 and C19-C27 exhibited 70:30 disorder about an approximate 
non-crystallographic mirror containing Zn1 O1 and N3. Comparative 
chemically equivalent distances were restrained to being similar in 
both disordered components, as were the ADPs of corresponding atoms 
pairs.
;

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr1 Zr 0.90357(4) 0.20022(2) 0.23773(3) 0.02394(12) Uani 1 1 d . . . . .
O1 O 0.9219(3) 0.31491(17) 0.19857(17) 0.0347(8) Uani 1 1 d . . . . .
O2 O 0.9297(2) 0.07676(14) 0.23873(19) 0.0285(7) Uani 1 1 d . . . . .
O3 O 0.9177(3) 0.23832(19) 0.34013(17) 0.0371(8) Uani 1 1 d D . . . .
N1 N 0.9154(5) 0.2310(2) 0.1108(2) 0.0363(10) Uani 1 1 d . . . . .
N2 N 1.0968(3) 0.14522(18) 0.23744(18) 0.0234(7) Uani 1 1 d . . . . .
N3 N 0.7218(3) 0.1719(2) 0.2323(3) 0.0355(9) Uani 1 1 d . . . . .
N4A N 0.8919(16) 0.2447(6) 0.4612(7) 0.0388(14) Uani 0.3 1 d D U P A 2
C1 C 0.9126(5) 0.3023(2) 0.1265(3) 0.0311(10) Uani 1 1 d . . . . .
C2 C 0.8907(6) 0.3791(3) 0.0856(3) 0.0399(13) Uani 1 1 d . . . . .
C3 C 0.9736(8) 0.4388(4) 0.1176(5) 0.086(3) Uani 1 1 d . . . . .
H3A H 0.9556 0.4448 0.1702 0.129 Uiso 1 1 calc GR . . . .
H3B H 0.9599 0.4878 0.0922 0.129 Uiso 1 1 calc GR . . . .
H3C H 1.0600 0.4230 0.1113 0.129 Uiso 1 1 calc GR . . . .
C5 C 0.8980(9) 0.3822(4) 0.0018(4) 0.079(2) Uani 1 1 d . . . . .
H5A H 0.9815 0.3678 -0.0141 0.119 Uiso 1 1 calc GR . . . .
H5B H 0.8795 0.4345 -0.0151 0.119 Uiso 1 1 calc GR . . . .
H5C H 0.8378 0.3463 -0.0194 0.119 Uiso 1 1 calc GR . . . .
C5AA C 0.6379(4) 0.2362(3) 0.2373(4) 0.0569(17) Uani 1 1 d . . . . .
H5AA H 0.5978 0.2360 0.2857 0.085 Uiso 1 1 calc GR . . . .
H5AB H 0.5748 0.2319 0.1986 0.085 Uiso 1 1 calc GR . . . .
H5AC H 0.6840 0.2843 0.2310 0.085 Uiso 1 1 calc GR . . . .
C6 C 0.9014(6) 0.1852(3) 0.0403(3) 0.0399(12) Uani 1 1 d . . . . .
C6AA C 0.7552(7) 0.4001(4) 0.1072(5) 0.081(2) Uani 1 1 d . . . . .
H6AA H 0.6977 0.3655 0.0818 0.121 Uiso 1 1 calc GR . . . .
H6AB H 0.7379 0.4534 0.0929 0.121 Uiso 1 1 calc GR . . . .
H6AC H 0.7450 0.3945 0.1606 0.121 Uiso 1 1 calc GR . . . .
C7 C 0.7663(7) 0.1934(4) 0.0136(4) 0.070(2) Uani 1 1 d . . . . .
H7A H 0.7102 0.1736 0.0515 0.105 Uiso 1 1 calc GR . . . .
H7B H 0.7550 0.1640 -0.0320 0.105 Uiso 1 1 calc GR . . . .
H7C H 0.7479 0.2478 0.0044 0.105 Uiso 1 1 calc GR . . . .
C7AA C 0.6535(5) 0.0995(3) 0.2300(4) 0.0581(17) Uani 1 1 d . . . . .
H7AA H 0.7117 0.0564 0.2322 0.087 Uiso 1 1 calc GR . . . .
H7AB H 0.6058 0.0967 0.1841 0.087 Uiso 1 1 calc GR . . . .
H7AC H 0.5970 0.0970 0.2721 0.087 Uiso 1 1 calc GR . . . .
C8 C 0.9932(7) 0.2050(4) -0.0193(4) 0.0658(19) Uani 1 1 d . . . . .
H8A H 0.9799 0.2582 -0.0354 0.099 Uiso 1 1 calc GR . . . .
H8B H 0.9819 0.1702 -0.0612 0.099 Uiso 1 1 calc GR . . . .
H8C H 1.0775 0.1996 0.0001 0.099 Uiso 1 1 calc GR . . . .
C9 C 0.9234(9) 0.1026(3) 0.0620(3) 0.078(3) Uani 1 1 d . . . . .
H9A H 1.0049 0.0979 0.0853 0.118 Uiso 1 1 calc GR . . . .
H9B H 0.9201 0.0700 0.0180 0.118 Uiso 1 1 calc GR . . . .
H9C H 0.8593 0.0863 0.0969 0.118 Uiso 1 1 calc GR . . . .
C10 C 1.0518(3) 0.0761(2) 0.2410(3) 0.0241(8) Uani 1 1 d . . . . .
C11 C 1.1066(4) -0.0055(2) 0.2448(2) 0.0313(10) Uani 1 1 d . . . . .
C12 C 1.0088(5) -0.0588(3) 0.2775(4) 0.062(2) Uani 1 1 d . . . . .
H12A H 0.9894 -0.0422 0.3279 0.094 Uiso 1 1 calc GR . . . .
H12B H 1.0405 -0.1116 0.2785 0.094 Uiso 1 1 calc GR . . . .
H12C H 0.9337 -0.0567 0.2473 0.094 Uiso 1 1 calc GR . . . .
C13 C 1.2221(6) -0.0124(3) 0.2932(4) 0.0555(16) Uani 1 1 d . . . . .
H13A H 1.2830 0.0262 0.2780 0.083 Uiso 1 1 calc GR . . . .
H13B H 1.2577 -0.0640 0.2877 0.083 Uiso 1 1 calc GR . . . .
H13C H 1.1996 -0.0039 0.3449 0.083 Uiso 1 1 calc GR . . . .
C14 C 1.1332(6) -0.0329(3) 0.1659(3) 0.0590(18) Uani 1 1 d . . . . .
H14A H 1.0561 -0.0332 0.1373 0.089 Uiso 1 1 calc GR . . . .
H14B H 1.1677 -0.0851 0.1673 0.089 Uiso 1 1 calc GR . . . .
H14C H 1.1927 0.0020 0.1426 0.089 Uiso 1 1 calc GR . . . .
C15 C 1.2246(4) 0.1774(2) 0.2355(3) 0.0294(9) Uani 1 1 d . . . . .
C16 C 1.2826(6) 0.1764(4) 0.3093(3) 0.0536(16) Uani 1 1 d . . . . .
H16A H 1.2261 0.1997 0.3452 0.080 Uiso 1 1 calc GR . . . .
H16B H 1.3599 0.2058 0.3081 0.080 Uiso 1 1 calc GR . . . .
H16C H 1.3002 0.1232 0.3237 0.080 Uiso 1 1 calc GR . . . .
C17 C 1.2077(5) 0.2616(3) 0.2131(3) 0.0485(14) Uani 1 1 d . . . . .
H17A H 1.1627 0.2642 0.1662 0.073 Uiso 1 1 calc GR . . . .
H17B H 1.2889 0.2859 0.2075 0.073 Uiso 1 1 calc GR . . . .
H17C H 1.1605 0.2886 0.2513 0.073 Uiso 1 1 calc GR . . . .
C18 C 1.3042(5) 0.1428(3) 0.1756(3) 0.0449(14) Uani 1 1 d . . . . .
H18A H 1.3270 0.0901 0.1893 0.067 Uiso 1 1 calc GR . . . .
H18B H 1.3792 0.1738 0.1696 0.067 Uiso 1 1 calc GR . . . .
H18C H 1.2579 0.1420 0.1291 0.067 Uiso 1 1 calc GR . . . .
C19A C 0.901(2) 0.3676(6) 0.4013(9) 0.040(2) Uani 0.3 1 d D U P A 2
C20A C 0.901(3) 0.2816(6) 0.4002(5) 0.0350(16) Uani 0.3 1 d D U P A 2
C21A C 0.898(2) 0.1589(7) 0.4658(9) 0.032(2) Uani 0.3 1 d D U P A 2
C22A C 0.873(2) 0.1421(13) 0.5467(9) 0.056(2) Uani 0.3 1 d D U P A 2
H22A H 0.9369 0.1671 0.5771 0.084 Uiso 0.3 1 calc GR . P A 2
H22B H 0.8758 0.0864 0.5550 0.084 Uiso 0.3 1 calc GR . P A 2
H22C H 0.7917 0.1620 0.5602 0.084 Uiso 0.3 1 calc GR . P A 2
C23A C 1.018(2) 0.1224(19) 0.439(3) 0.034(2) Uani 0.3 1 d D U P A 2
H23A H 1.0211 0.1254 0.3849 0.052 Uiso 0.3 1 calc GR U P A 2
H23B H 1.0202 0.0683 0.4541 0.052 Uiso 0.3 1 calc GR . P A 2
H23C H 1.0884 0.1498 0.4600 0.052 Uiso 0.3 1 calc GR . P A 2
C24A C 0.795(3) 0.1155(19) 0.427(3) 0.061(3) Uani 0.3 1 d D U P A 2
H24A H 0.7249 0.1500 0.4185 0.092 Uiso 0.3 1 calc GR . P A 2
H24B H 0.7690 0.0719 0.4571 0.092 Uiso 0.3 1 calc GR . P A 2
H24C H 0.8256 0.0965 0.3791 0.092 Uiso 0.3 1 calc GR U P A 2
C25A C 0.897(3) 0.3936(11) 0.4811(9) 0.065(3) Uani 0.3 1 d D U P A 2
H25A H 0.8270 0.3688 0.5061 0.098 Uiso 0.3 1 calc GR . P A 2
H25B H 0.8865 0.4496 0.4830 0.098 Uiso 0.3 1 calc GR . P A 2
H25C H 0.9741 0.3792 0.5056 0.098 Uiso 0.3 1 calc GR . P A 2
C26A C 1.014(2) 0.401(3) 0.3640(16) 0.035(6) Uani 0.3 1 d D U P A 2
H26A H 1.0889 0.3830 0.3897 0.053 Uiso 0.3 1 calc GR . P A 2
H26B H 1.0108 0.4572 0.3659 0.053 Uiso 0.3 1 calc GR . P A 2
H26C H 1.0169 0.3839 0.3125 0.053 Uiso 0.3 1 calc GR U P A 2
C27A C 0.778(3) 0.388(3) 0.365(3) 0.078(5) Uani 0.3 1 d D U P A 2
H27A H 0.7876 0.3852 0.3110 0.116 Uiso 0.3 1 calc GR U P A 2
H27B H 0.7544 0.4404 0.3788 0.116 Uiso 0.3 1 calc GR . P A 2
H27C H 0.7145 0.3518 0.3806 0.116 Uiso 0.3 1 calc GR . P A 2
N4 N 0.8807(7) 0.3062(3) 0.4488(3) 0.0388(14) Uani 0.7 1 d D U P A 1
C19 C 0.8852(10) 0.1713(4) 0.4567(4) 0.040(2) Uani 0.7 1 d D U P A 1
C20 C 0.9013(10) 0.2440(3) 0.4131(3) 0.0350(16) Uani 0.7 1 d D U P A 1
C21 C 0.8823(8) 0.3832(3) 0.4126(3) 0.032(2) Uani 0.7 1 d D U P A 1
C22 C 0.8605(10) 0.4392(5) 0.4757(4) 0.056(2) Uani 0.7 1 d D U P A 1
H22D H 0.8602 0.4920 0.4566 0.084 Uiso 0.7 1 calc R U P A 1
H22E H 0.7807 0.4281 0.4988 0.084 Uiso 0.7 1 calc R U P A 1
H22F H 0.9268 0.4337 0.5123 0.084 Uiso 0.7 1 calc R U P A 1
C23 C 0.7794(10) 0.3932(8) 0.3563(7) 0.034(2) Uani 0.7 1 d D U P A 1
H23D H 0.7849 0.4446 0.3343 0.052 Uiso 0.7 1 calc R . P A 1
H23E H 0.7880 0.3542 0.3176 0.052 Uiso 0.7 1 calc R U P A 1
H23F H 0.6991 0.3873 0.3806 0.052 Uiso 0.7 1 calc R U P A 1
C24 C 1.0060(13) 0.4020(14) 0.3773(11) 0.061(3) Uani 0.7 1 d D U P A 1
H24D H 1.0019 0.4530 0.3544 0.092 Uiso 0.7 1 calc R U P A 1
H24E H 1.0709 0.4017 0.4151 0.092 Uiso 0.7 1 calc R U P A 1
H24F H 1.0251 0.3634 0.3396 0.092 Uiso 0.7 1 calc R U P A 1
C25 C 0.8805(12) 0.1838(5) 0.5395(4) 0.065(3) Uani 0.7 1 d D U P A 1
H25D H 0.8699 0.1342 0.5644 0.098 Uiso 0.7 1 calc R U P A 1
H25E H 0.9579 0.2078 0.5560 0.098 Uiso 0.7 1 calc R U P A 1
H25F H 0.8108 0.2176 0.5516 0.098 Uiso 0.7 1 calc R U P A 1
C26 C 0.7685(11) 0.1307(7) 0.4303(11) 0.061(3) Uani 0.7 1 d D U P A 1
H26D H 0.7571 0.0830 0.4585 0.092 Uiso 0.7 1 calc R U P A 1
H26E H 0.6970 0.1644 0.4378 0.092 Uiso 0.7 1 calc R U P A 1
H26F H 0.7764 0.1184 0.3778 0.092 Uiso 0.7 1 calc R . P A 1
C27 C 0.9939(14) 0.1187(11) 0.4398(13) 0.078(5) Uani 0.7 1 d D U P A 1
H27D H 0.9853 0.0708 0.4677 0.116 Uiso 0.7 1 calc R . P A 1
H27E H 0.9952 0.1072 0.3869 0.116 Uiso 0.7 1 calc R U P A 1
H27F H 1.0712 0.1444 0.4538 0.116 Uiso 0.7 1 calc R U P A 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr1 O1 2.125(3) . ?
Zr1 O2 2.164(3) . ?
Zr1 O3 1.978(3) . ?
Zr1 N1 2.368(4) . ?
Zr1 N2 2.296(3) . ?
Zr1 N3 2.027(4) . ?
Zr1 C1 2.687(4) . ?
Zr1 C10 2.687(4) . ?
O1 C1 1.328(6) . ?
O2 C10 1.321(4) . ?
O3 C20A 1.337(8) . ?
O3 C20 1.339(7) . ?
N1 C1 1.271(6) . ?
N1 C6 1.513(6) . ?
N2 C10 1.297(5) . ?
N2 C15 1.491(5) . ?
N3 C5AA 1.443(6) . ?
N3 C7AA 1.458(6) . ?
N4A C20A 1.283(8) . ?
N4A C21A 1.495(7) . ?
C1 C2 1.546(6) . ?
C2 C3 1.487(8) . ?
C2 C5 1.524(8) . ?
C2 C6AA 1.559(9) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C5AA H5AA 0.9800 . ?
C5AA H5AB 0.9800 . ?
C5AA H5AC 0.9800 . ?
C6 C7 1.544(9) . ?
C6 C8 1.508(9) . ?
C6 C9 1.507(7) . ?
C6AA H6AA 0.9800 . ?
C6AA H6AB 0.9800 . ?
C6AA H6AC 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C7AA H7AA 0.9800 . ?
C7AA H7AB 0.9800 . ?
C7AA H7AC 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.539(5) . ?
C11 C12 1.526(7) . ?
C11 C13 1.529(7) . ?
C11 C14 1.537(7) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.478(7) . ?
C15 C17 1.529(6) . ?
C15 C18 1.511(7) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19A C20A 1.495(7) . ?
C19A C25A 1.517(5) . ?
C19A C26A 1.519(5) . ?
C19A C27A 1.518(5) . ?
C21A C22A 1.520(5) . ?
C21A C23A 1.520(5) . ?
C21A C24A 1.519(5) . ?
C22A H22A 0.9800 . ?
C22A H22B 0.9800 . ?
C22A H22C 0.9800 . ?
C23A H23A 0.9800 . ?
C23A H23B 0.9800 . ?
C23A H23C 0.9800 . ?
C24A H24A 0.9800 . ?
C24A H24B 0.9800 . ?
C24A H24C 0.9800 . ?
C25A H25A 0.9800 . ?
C25A H25B 0.9800 . ?
C25A H25C 0.9800 . ?
C26A H26A 0.9800 . ?
C26A H26B 0.9800 . ?
C26A H26C 0.9800 . ?
C27A H27A 0.9800 . ?
C27A H27B 0.9800 . ?
C27A H27C 0.9800 . ?
N4 C20 1.281(7) . ?
N4 C21 1.491(6) . ?
C19 C20 1.501(6) . ?
C19 C25 1.519(5) . ?
C19 C26 1.521(5) . ?
C19 C27 1.519(5) . ?
C21 C22 1.520(5) . ?
C21 C23 1.519(4) . ?
C21 C24 1.519(5) . ?
C22 H22D 0.9800 . ?
C22 H22E 0.9800 . ?
C22 H22F 0.9800 . ?
C23 H23D 0.9800 . ?
C23 H23E 0.9800 . ?
C23 H23F 0.9800 . ?
C24 H24D 0.9800 . ?
C24 H24E 0.9800 . ?
C24 H24F 0.9800 . ?
C25 H25D 0.9800 . ?
C25 H25E 0.9800 . ?
C25 H25F 0.9800 . ?
C26 H26D 0.9800 . ?
C26 H26E 0.9800 . ?
C26 H26F 0.9800 . ?
C27 H27D 0.9800 . ?
C27 H27E 0.9800 . ?
C27 H27F 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Zr1 O2 156.97(13) . . ?
O1 Zr1 N1 57.16(13) . . ?
O1 Zr1 N2 107.70(13) . . ?
O1 Zr1 C1 29.17(13) . . ?
O1 Zr1 C10 134.74(13) . . ?
O2 Zr1 N1 103.00(13) . . ?
O2 Zr1 N2 57.92(10) . . ?
O2 Zr1 C1 130.97(13) . . ?
O2 Zr1 C10 29.13(10) . . ?
O3 Zr1 O1 89.59(13) . . ?
O3 Zr1 O2 108.31(13) . . ?
O3 Zr1 N1 146.47(13) . . ?
O3 Zr1 N2 94.15(13) . . ?
O3 Zr1 N3 101.59(17) . . ?
O3 Zr1 C1 118.76(13) . . ?
O3 Zr1 C10 101.70(14) . . ?
N1 Zr1 C1 28.23(13) . . ?
N1 Zr1 C10 99.75(15) . . ?
N2 Zr1 N1 92.36(15) . . ?
N2 Zr1 C1 103.82(15) . . ?
N2 Zr1 C10 28.83(11) . . ?
N3 Zr1 O1 107.62(15) . . ?
N3 Zr1 O2 83.43(12) . . ?
N3 Zr1 N1 93.51(18) . . ?
N3 Zr1 N2 141.22(13) . . ?
N3 Zr1 C1 99.20(17) . . ?
N3 Zr1 C10 112.55(13) . . ?
C10 Zr1 C1 121.58(15) . . ?
C1 O1 Zr1 99.6(2) . . ?
C10 O2 Zr1 98.0(2) . . ?
C20A O3 Zr1 160.7(9) . . ?
C20 O3 Zr1 160.5(4) . . ?
C1 N1 Zr1 90.0(3) . . ?
C1 N1 C6 134.4(4) . . ?
C6 N1 Zr1 134.2(3) . . ?
C10 N2 Zr1 92.6(2) . . ?
C10 N2 C15 134.1(3) . . ?
C15 N2 Zr1 133.3(2) . . ?
C5AA N3 Zr1 114.7(3) . . ?
C5AA N3 C7AA 110.5(4) . . ?
C7AA N3 Zr1 134.6(3) . . ?
C20A N4A C21A 122.9(12) . . ?
O1 C1 Zr1 51.2(2) . . ?
O1 C1 C2 109.9(4) . . ?
N1 C1 Zr1 61.8(3) . . ?
N1 C1 O1 112.4(4) . . ?
N1 C1 C2 137.5(5) . . ?
C2 C1 Zr1 157.6(4) . . ?
C1 C2 C6AA 102.9(5) . . ?
C3 C2 C1 108.9(5) . . ?
C3 C2 C5 109.4(6) . . ?
C3 C2 C6AA 107.7(6) . . ?
C5 C2 C1 120.1(5) . . ?
C5 C2 C6AA 107.1(6) . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 C5 H5A 109.5 . . ?
C2 C5 H5B 109.5 . . ?
C2 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N3 C5AA H5AA 109.5 . . ?
N3 C5AA H5AB 109.5 . . ?
N3 C5AA H5AC 109.5 . . ?
H5AA C5AA H5AB 109.5 . . ?
H5AA C5AA H5AC 109.5 . . ?
H5AB C5AA H5AC 109.5 . . ?
N1 C6 C7 108.0(5) . . ?
C8 C6 N1 114.9(5) . . ?
C8 C6 C7 112.2(5) . . ?
C9 C6 N1 105.3(4) . . ?
C9 C6 C7 108.5(6) . . ?
C9 C6 C8 107.6(6) . . ?
C2 C6AA H6AA 109.5 . . ?
C2 C6AA H6AB 109.5 . . ?
C2 C6AA H6AC 109.5 . . ?
H6AA C6AA H6AB 109.5 . . ?
H6AA C6AA H6AC 109.5 . . ?
H6AB C6AA H6AC 109.5 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N3 C7AA H7AA 109.5 . . ?
N3 C7AA H7AB 109.5 . . ?
N3 C7AA H7AC 109.5 . . ?
H7AA C7AA H7AB 109.5 . . ?
H7AA C7AA H7AC 109.5 . . ?
H7AB C7AA H7AC 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O2 C10 Zr1 52.89(18) . . ?
O2 C10 C11 113.2(3) . . ?
N2 C10 Zr1 58.6(2) . . ?
N2 C10 O2 111.4(3) . . ?
N2 C10 C11 135.4(3) . . ?
C11 C10 Zr1 166.0(3) . . ?
C12 C11 C10 108.1(4) . . ?
C12 C11 C13 107.1(4) . . ?
C12 C11 C14 107.8(5) . . ?
C13 C11 C10 114.3(4) . . ?
C13 C11 C14 110.9(4) . . ?
C14 C11 C10 108.4(4) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N2 C15 C17 104.8(3) . . ?
N2 C15 C18 113.3(4) . . ?
C16 C15 N2 111.5(4) . . ?
C16 C15 C17 107.6(4) . . ?
C16 C15 C18 113.9(4) . . ?
C18 C15 C17 105.0(4) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20A C19A C25A 108.0(12) . . ?
C20A C19A C26A 112(2) . . ?
C20A C19A C27A 103(3) . . ?
C25A C19A C26A 110(2) . . ?
C25A C19A C27A 109(3) . . ?
C27A C19A C26A 115(3) . . ?
O3 C20A C19A 125.0(10) . . ?
N4A C20A O3 115.6(10) . . ?
N4A C20A C19A 119.3(9) . . ?
N4A C21A C22A 103.7(13) . . ?
N4A C21A C23A 116(2) . . ?
N4A C21A C24A 116(2) . . ?
C23A C21A C22A 112(3) . . ?
C24A C21A C22A 103(3) . . ?
C24A C21A C23A 105(2) . . ?
C21A C22A H22A 109.5 . . ?
C21A C22A H22B 109.5 . . ?
C21A C22A H22C 109.5 . . ?
H22A C22A H22B 109.5 . . ?
H22A C22A H22C 109.5 . . ?
H22B C22A H22C 109.5 . . ?
C21A C23A H23A 109.5 . . ?
C21A C23A H23B 109.5 . . ?
C21A C23A H23C 109.5 . . ?
H23A C23A H23B 109.5 . . ?
H23A C23A H23C 109.5 . . ?
H23B C23A H23C 109.5 . . ?
C21A C24A H24A 109.5 . . ?
C21A C24A H24B 109.5 . . ?
C21A C24A H24C 109.5 . . ?
H24A C24A H24B 109.5 . . ?
H24A C24A H24C 109.5 . . ?
H24B C24A H24C 109.5 . . ?
C19A C25A H25A 109.5 . . ?
C19A C25A H25B 109.5 . . ?
C19A C25A H25C 109.5 . . ?
H25A C25A H25B 109.5 . . ?
H25A C25A H25C 109.5 . . ?
H25B C25A H25C 109.5 . . ?
C19A C26A H26A 109.5 . . ?
C19A C26A H26B 109.5 . . ?
C19A C26A H26C 109.5 . . ?
H26A C26A H26B 109.5 . . ?
H26A C26A H26C 109.5 . . ?
H26B C26A H26C 109.5 . . ?
C19A C27A H27A 109.5 . . ?
C19A C27A H27B 109.5 . . ?
C19A C27A H27C 109.5 . . ?
H27A C27A H27B 109.5 . . ?
H27A C27A H27C 109.5 . . ?
H27B C27A H27C 109.5 . . ?
C20 N4 C21 122.2(5) . . ?
C20 C19 C25 113.8(6) . . ?
C20 C19 C26 108.8(9) . . ?
C20 C19 C27 108.0(11) . . ?
C25 C19 C26 110.4(11) . . ?
C25 C19 C27 108.2(11) . . ?
C27 C19 C26 107.3(11) . . ?
O3 C20 C19 118.3(5) . . ?
N4 C20 O3 125.9(6) . . ?
N4 C20 C19 115.1(6) . . ?
N4 C21 C22 103.9(5) . . ?
N4 C21 C23 112.9(7) . . ?
N4 C21 C24 112.9(10) . . ?
C23 C21 C22 108.6(8) . . ?
C23 C21 C24 109.6(11) . . ?
C24 C21 C22 108.5(11) . . ?
C21 C22 H22D 109.5 . . ?
C21 C22 H22E 109.5 . . ?
C21 C22 H22F 109.5 . . ?
H22D C22 H22E 109.5 . . ?
H22D C22 H22F 109.5 . . ?
H22E C22 H22F 109.5 . . ?
C21 C23 H23D 109.5 . . ?
C21 C23 H23E 109.5 . . ?
C21 C23 H23F 109.5 . . ?
H23D C23 H23E 109.5 . . ?
H23D C23 H23F 109.5 . . ?
H23E C23 H23F 109.5 . . ?
C21 C24 H24D 109.5 . . ?
C21 C24 H24E 109.5 . . ?
C21 C24 H24F 109.5 . . ?
H24D C24 H24E 109.5 . . ?
H24D C24 H24F 109.5 . . ?
H24E C24 H24F 109.5 . . ?
C19 C25 H25D 109.5 . . ?
C19 C25 H25E 109.5 . . ?
C19 C25 H25F 109.5 . . ?
H25D C25 H25E 109.5 . . ?
H25D C25 H25F 109.5 . . ?
H25E C25 H25F 109.5 . . ?
C19 C26 H26D 109.5 . . ?
C19 C26 H26E 109.5 . . ?
C19 C26 H26F 109.5 . . ?
H26D C26 H26E 109.5 . . ?
H26D C26 H26F 109.5 . . ?
H26E C26 H26F 109.5 . . ?
C19 C27 H27D 109.5 . . ?
C19 C27 H27E 109.5 . . ?
C19 C27 H27F 109.5 . . ?
H27D C27 H27E 109.5 . . ?
H27D C27 H27F 109.5 . . ?
H27E C27 H27F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Zr1 O1 C1 N1 -9.5(6) . . . . ?
Zr1 O1 C1 C2 166.0(4) . . . . ?
Zr1 O2 C10 N2 -3.5(4) . . . . ?
Zr1 O2 C10 C11 178.2(3) . . . . ?
Zr1 O3 C20A N4A 140.0(16) . . . . ?
Zr1 O3 C20A C19A -44(5) . . . . ?
Zr1 O3 C20 N4 -135.4(9) . . . . ?
Zr1 O3 C20 C19 34(2) . . . . ?
Zr1 N1 C1 O1 8.4(5) . . . . ?
Zr1 N1 C1 C2 -165.4(7) . . . . ?
Zr1 N1 C6 C7 94.8(6) . . . . ?
Zr1 N1 C6 C8 -139.2(5) . . . . ?
Zr1 N1 C6 C9 -21.0(8) . . . . ?
Zr1 N2 C10 O2 3.3(4) . . . . ?
Zr1 N2 C10 C11 -178.9(5) . . . . ?
Zr1 N2 C15 C16 101.6(5) . . . . ?
Zr1 N2 C15 C17 -14.5(6) . . . . ?
Zr1 N2 C15 C18 -128.3(4) . . . . ?
Zr1 C1 C2 C3 72.4(12) . . . . ?
Zr1 C1 C2 C5 -160.5(8) . . . . ?
Zr1 C1 C2 C6AA -41.7(11) . . . . ?
Zr1 C10 C11 C12 -18.1(15) . . . . ?
Zr1 C10 C11 C13 -137.2(12) . . . . ?
Zr1 C10 C11 C14 98.5(13) . . . . ?
O1 C1 C2 C3 42.7(7) . . . . ?
O1 C1 C2 C5 169.8(6) . . . . ?
O1 C1 C2 C6AA -71.4(6) . . . . ?
O2 C10 C11 C12 -24.1(6) . . . . ?
O2 C10 C11 C13 -143.2(5) . . . . ?
O2 C10 C11 C14 92.5(5) . . . . ?
N1 C1 C2 C3 -143.4(8) . . . . ?
N1 C1 C2 C5 -16.3(12) . . . . ?
N1 C1 C2 C6AA 102.5(9) . . . . ?
N2 C10 C11 C12 158.1(6) . . . . ?
N2 C10 C11 C13 39.0(8) . . . . ?
N2 C10 C11 C14 -85.3(7) . . . . ?
C1 N1 C6 C7 -67.6(9) . . . . ?
C1 N1 C6 C8 58.4(10) . . . . ?
C1 N1 C6 C9 176.6(7) . . . . ?
C6 N1 C1 Zr1 167.5(8) . . . . ?
C6 N1 C1 O1 175.9(6) . . . . ?
C6 N1 C1 C2 2.1(13) . . . . ?
C10 N2 C15 C16 -76.9(6) . . . . ?
C10 N2 C15 C17 167.1(5) . . . . ?
C10 N2 C15 C18 53.2(7) . . . . ?
C15 N2 C10 Zr1 178.9(5) . . . . ?
C15 N2 C10 O2 -177.8(4) . . . . ?
C15 N2 C10 C11 0.0(9) . . . . ?
C20A N4A C21A C22A -176(2) . . . . ?
C20A N4A C21A C23A 60(3) . . . . ?
C20A N4A C21A C24A -64(4) . . . . ?
C21A N4A C20A O3 0(4) . . . . ?
C21A N4A C20A C19A -177(2) . . . . ?
C25A C19A C20A O3 -172(2) . . . . ?
C25A C19A C20A N4A 4(3) . . . . ?
C26A C19A C20A O3 -52(3) . . . . ?
C26A C19A C20A N4A 124(3) . . . . ?
C27A C19A C20A O3 73(3) . . . . ?
C27A C19A C20A N4A -112(3) . . . . ?
C20 N4 C21 C22 -177.0(9) . . . . ?
C20 N4 C21 C23 65.4(12) . . . . ?
C20 N4 C21 C24 -59.6(13) . . . . ?
C21 N4 C20 O3 -5.0(15) . . . . ?
C21 N4 C20 C19 -174.9(8) . . . . ?
C25 C19 C20 O3 174.0(9) . . . . ?
C25 C19 C20 N4 -15.2(14) . . . . ?
C26 C19 C20 O3 -62.4(13) . . . . ?
C26 C19 C20 N4 108.3(11) . . . . ?
C27 C19 C20 O3 53.8(14) . . . . ?
C27 C19 C20 N4 -135.5(12) . . . . ?


loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.6292(14)
2 0.3708(14)

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_e14msh6
_database_code_depnum_ccdc_archive 'CCDC 1498669'
_audit_update_record             
;
2016-08-10 deposited with the CCDC.
2016-10-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H64 N4 O4 Zr'
_chemical_formula_weight         660.09

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   Cc

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   20.1357(5)
_cell_length_b                   15.0949(4)
_cell_length_c                   12.2443(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.836(2)
_cell_angle_gamma                90.00
_cell_volume                     3677.44(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    8965
_cell_measurement_theta_min      3.6430
_cell_measurement_theta_max      28.9400


_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.256
_exptl_crystal_size_mid          0.222
_exptl_crystal_size_min          0.046
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1424
_exptl_absorpt_coefficient_mu    0.336
_exptl_absorpt_correction_T_min  0.91456
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;


_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073

_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'

_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            EosS2
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6983
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0560
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.36
_diffrn_reflns_theta_max         27.48
_reflns_number_total             6983
_reflns_number_gt                5714
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;

_computing_structure_solution    'SHELXS-97 (Sheldrick 1990)'
_computing_structure_refinement  'SHELXL-97/2 (Sheldrick 1997)'
_computing_molecular_graphics    'ORTEX (P.McArdle 1995)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick 1997)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.

Notes:

The crystal exhibited classic non-merohedral twinning by virtue of a 
180o rotation about the direct space 1 0 0 vector. Data for both 
twinned components were integrated simultaneously to account for same.                                                                                                                      

;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1113P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_chemical_absolute_configuration unk
_refine_ls_number_parameters     391
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0517
_refine_ls_wR_factor_ref         0.1553
_refine_ls_wR_factor_gt          0.1460
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr1 Zr 0.01608(4) 0.24331(2) 0.57769(6) 0.01271(13) Uani 1 1 d . . .
O1 O -0.0079(2) 0.2883(3) 0.4057(3) 0.0160(9) Uani 1 1 d . . .
O2 O 0.0676(2) 0.1213(2) 0.6428(4) 0.0195(9) Uani 1 1 d . . .
O3 O 0.05698(19) 0.3786(2) 0.5820(4) 0.0176(8) Uani 1 1 d . . .
O4 O -0.0544(2) 0.1862(3) 0.6789(4) 0.0208(9) Uani 1 1 d . . .
N1 N -0.0364(2) 0.1527(3) 0.4379(4) 0.0167(10) Uani 1 1 d . . .
N2 N 0.1184(3) 0.2028(3) 0.5341(4) 0.0169(11) Uani 1 1 d . . .
N3 N 0.0667(3) 0.3078(3) 0.7396(4) 0.0162(10) Uani 1 1 d . . .
N4 N -0.0848(3) 0.3109(3) 0.5953(4) 0.0176(11) Uani 1 1 d . . .
C1 C -0.0367(3) 0.2155(4) 0.3654(5) 0.0148(11) Uani 1 1 d . . .
C2 C -0.0647(4) 0.2126(4) 0.2411(5) 0.0249(14) Uani 1 1 d . . .
C3 C -0.0549(4) 0.3033(4) 0.1916(6) 0.0321(15) Uani 1 1 d . . .
H3A H -0.0776 0.3047 0.1148 0.048 Uiso 1 1 calc R . .
H3B H -0.0068 0.3145 0.1936 0.048 Uiso 1 1 calc R . .
H3C H -0.0741 0.3489 0.2344 0.048 Uiso 1 1 calc R . .
C4 C -0.1394(4) 0.1924(5) 0.2211(6) 0.0370(17) Uani 1 1 d . . .
H4A H -0.1628 0.2330 0.2647 0.056 Uiso 1 1 calc R . .
H4B H -0.1468 0.1312 0.2432 0.056 Uiso 1 1 calc R . .
H4C H -0.1569 0.1998 0.1424 0.056 Uiso 1 1 calc R . .
C5 C -0.0256(4) 0.1448(4) 0.1812(6) 0.0324(16) Uani 1 1 d . . .
H5A H -0.0266 0.0867 0.2168 0.049 Uiso 1 1 calc R . .
H5B H 0.0211 0.1643 0.1851 0.049 Uiso 1 1 calc R . .
H5C H -0.0464 0.1402 0.1036 0.049 Uiso 1 1 calc R . .
C6 C -0.0617(3) 0.0616(3) 0.4163(6) 0.0222(13) Uani 1 1 d . . .
H6 H -0.0843 0.0580 0.3377 0.027 Uiso 1 1 calc R . .
C7 C -0.1133(4) 0.0397(5) 0.4914(7) 0.0379(17) Uani 1 1 d . . .
H7A H -0.0914 0.0401 0.5687 0.057 Uiso 1 1 calc R . .
H7B H -0.1323 -0.0191 0.4727 0.057 Uiso 1 1 calc R . .
H7C H -0.1493 0.0840 0.4812 0.057 Uiso 1 1 calc R . .
C8 C -0.0048(4) -0.0039(4) 0.4327(7) 0.0344(17) Uani 1 1 d . . .
H8A H 0.0274 0.0106 0.3829 0.052 Uiso 1 1 calc R . .
H8B H -0.0224 -0.0637 0.4165 0.052 Uiso 1 1 calc R . .
H8C H 0.0178 -0.0011 0.5095 0.052 Uiso 1 1 calc R . .
C9 C 0.1206(3) 0.1305(3) 0.5946(5) 0.0139(10) Uani 1 1 d . . .
C10 C 0.1751(3) 0.0593(4) 0.6139(5) 0.0213(12) Uani 1 1 d . . .
C11 C 0.1536(4) -0.0137(4) 0.6882(6) 0.0353(18) Uani 1 1 d . . .
H11A H 0.1397 0.0131 0.7540 0.053 Uiso 1 1 calc R . .
H11B H 0.1915 -0.0539 0.7106 0.053 Uiso 1 1 calc R . .
H11C H 0.1159 -0.0470 0.6474 0.053 Uiso 1 1 calc R . .
C12 C 0.2405(3) 0.1002(5) 0.6738(6) 0.0325(16) Uani 1 1 d . . .
H12A H 0.2540 0.1494 0.6299 0.049 Uiso 1 1 calc R . .
H12B H 0.2759 0.0551 0.6833 0.049 Uiso 1 1 calc R . .
H12C H 0.2333 0.1221 0.7464 0.049 Uiso 1 1 calc R . .
C13 C 0.1871(4) 0.0160(4) 0.5059(6) 0.0284(14) Uani 1 1 d . . .
H13A H 0.1446 -0.0074 0.4669 0.043 Uiso 1 1 calc R . .
H13B H 0.2195 -0.0324 0.5221 0.043 Uiso 1 1 calc R . .
H13C H 0.2049 0.0602 0.4593 0.043 Uiso 1 1 calc R . .
C14 C 0.1698(4) 0.2311(4) 0.4717(6) 0.0222(13) Uani 1 1 d . . .
H14 H 0.2074 0.1871 0.4833 0.027 Uiso 1 1 calc R . .
C15 C 0.1411(4) 0.2330(5) 0.3485(6) 0.0337(16) Uani 1 1 d . . .
H15A H 0.1329 0.1723 0.3215 0.051 Uiso 1 1 calc R . .
H15B H 0.1733 0.2617 0.3075 0.051 Uiso 1 1 calc R . .
H15C H 0.0988 0.2662 0.3375 0.051 Uiso 1 1 calc R . .
C16 C 0.1979(4) 0.3224(4) 0.5140(7) 0.0361(17) Uani 1 1 d . . .
H16A H 0.1618 0.3665 0.5031 0.054 Uiso 1 1 calc R . .
H16B H 0.2338 0.3403 0.4728 0.054 Uiso 1 1 calc R . .
H16C H 0.2160 0.3182 0.5928 0.054 Uiso 1 1 calc R . .
C17 C 0.0777(3) 0.3805(3) 0.6889(5) 0.0180(12) Uani 1 1 d . . .
C18 C 0.1104(3) 0.4676(4) 0.7357(5) 0.0260(14) Uani 1 1 d . . .
C19 C 0.1113(5) 0.5350(4) 0.6432(6) 0.0394(19) Uani 1 1 d . . .
H19A H 0.1414 0.5142 0.5928 0.059 Uiso 1 1 calc R . .
H19B H 0.1274 0.5921 0.6749 0.059 Uiso 1 1 calc R . .
H19C H 0.0658 0.5419 0.6024 0.059 Uiso 1 1 calc R . .
C20 C 0.0708(4) 0.5075(4) 0.8222(6) 0.0398(19) Uani 1 1 d . . .
H20A H 0.0240 0.5171 0.7884 0.060 Uiso 1 1 calc R . .
H20B H 0.0910 0.5642 0.8484 0.060 Uiso 1 1 calc R . .
H20C H 0.0722 0.4666 0.8847 0.060 Uiso 1 1 calc R . .
C21 C 0.1847(4) 0.4500(5) 0.7898(6) 0.0405(18) Uani 1 1 d . . .
H21A H 0.1854 0.4074 0.8503 0.061 Uiso 1 1 calc R . .
H21B H 0.2053 0.5057 0.8188 0.061 Uiso 1 1 calc R . .
H21C H 0.2099 0.4260 0.7341 0.061 Uiso 1 1 calc R . .
C22 C 0.0831(3) 0.2924(4) 0.8591(5) 0.0238(13) Uani 1 1 d . . .
H22 H 0.1099 0.3439 0.8933 0.029 Uiso 1 1 calc R . .
C23 C 0.1249(5) 0.2096(5) 0.8812(6) 0.047(2) Uani 1 1 d . . .
H23A H 0.1000 0.1590 0.8452 0.071 Uiso 1 1 calc R . .
H23B H 0.1347 0.1991 0.9610 0.071 Uiso 1 1 calc R . .
H23C H 0.1671 0.2168 0.8516 0.071 Uiso 1 1 calc R . .
C24 C 0.0208(4) 0.2847(6) 0.9103(6) 0.0451(19) Uani 1 1 d . . .
H24A H -0.0050 0.3397 0.8984 0.068 Uiso 1 1 calc R . .
H24B H 0.0330 0.2739 0.9898 0.068 Uiso 1 1 calc R . .
H24C H -0.0064 0.2352 0.8763 0.068 Uiso 1 1 calc R . .
C25 C -0.0992(3) 0.2468(3) 0.6581(5) 0.0196(12) Uani 1 1 d . . .
C26 C -0.1636(4) 0.2342(5) 0.7122(7) 0.0330(17) Uani 1 1 d . . .
C27 C -0.1591(4) 0.1483(5) 0.7750(8) 0.047(2) Uani 1 1 d . . .
H27A H -0.1521 0.0995 0.7253 0.070 Uiso 1 1 calc R . .
H27B H -0.2010 0.1386 0.8049 0.070 Uiso 1 1 calc R . .
H27C H -0.1214 0.1509 0.8359 0.070 Uiso 1 1 calc R . .
C28 C -0.1712(4) 0.3113(6) 0.7917(7) 0.0426(19) Uani 1 1 d . . .
H28A H -0.2143 0.3059 0.8191 0.064 Uiso 1 1 calc R . .
H28B H -0.1698 0.3677 0.7525 0.064 Uiso 1 1 calc R . .
H28C H -0.1344 0.3093 0.8542 0.064 Uiso 1 1 calc R . .
C29 C -0.2265(4) 0.2285(6) 0.6164(8) 0.046(2) Uani 1 1 d . . .
H29A H -0.2203 0.1792 0.5669 0.069 Uiso 1 1 calc R . .
H29B H -0.2306 0.2841 0.5744 0.069 Uiso 1 1 calc R . .
H29C H -0.2675 0.2187 0.6489 0.069 Uiso 1 1 calc R . .
C30 C -0.1253(3) 0.3897(4) 0.5591(5) 0.0254(14) Uani 1 1 d . . .
H30 H -0.1679 0.3858 0.5912 0.031 Uiso 1 1 calc R . .
C31 C -0.1435(6) 0.3887(7) 0.4360(7) 0.069(3) Uani 1 1 d . . .
H31A H -0.1025 0.3884 0.4021 0.103 Uiso 1 1 calc R . .
H31B H -0.1701 0.4415 0.4119 0.103 Uiso 1 1 calc R . .
H31C H -0.1700 0.3354 0.4133 0.103 Uiso 1 1 calc R . .
C32 C -0.0899(5) 0.4728(5) 0.6019(11) 0.070(3) Uani 1 1 d . . .
H32A H -0.0881 0.4758 0.6822 0.105 Uiso 1 1 calc R . .
H32B H -0.1143 0.5243 0.5675 0.105 Uiso 1 1 calc R . .
H32C H -0.0441 0.4726 0.5840 0.105 Uiso 1 1 calc R . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr1 O1 2.194(4) . ?
Zr1 O4 2.198(4) . ?
Zr1 O3 2.200(3) . ?
Zr1 O2 2.202(4) . ?
Zr1 N2 2.289(5) . ?
Zr1 N3 2.301(5) . ?
Zr1 N4 2.313(5) . ?
Zr1 N1 2.315(5) . ?
Zr1 C25 2.659(7) . ?
Zr1 C17 2.676(6) . ?
Zr1 C1 2.685(6) . ?
Zr1 C9 2.690(5) . ?
O1 C1 1.303(7) . ?
O2 C9 1.304(7) . ?
O3 C17 1.312(7) . ?
O4 C25 1.283(7) . ?
N1 C1 1.299(7) . ?
N1 C6 1.476(7) . ?
N2 C9 1.316(7) . ?
N2 C14 1.443(9) . ?
N3 C17 1.297(7) . ?
N3 C22 1.468(8) . ?
N4 C25 1.297(8) . ?
N4 C30 1.471(7) . ?
C1 C2 1.540(8) . ?
C2 C4 1.518(10) . ?
C2 C3 1.523(9) . ?
C2 C5 1.544(9) . ?
C6 C8 1.504(8) . ?
C6 C7 1.526(10) . ?
C9 C10 1.529(7) . ?
C10 C13 1.527(9) . ?
C10 C11 1.533(9) . ?
C10 C12 1.535(8) . ?
C14 C15 1.530(10) . ?
C14 C16 1.548(9) . ?
C17 C18 1.541(8) . ?
C18 C19 1.525(9) . ?
C18 C20 1.543(10) . ?
C18 C21 1.562(10) . ?
C22 C24 1.491(10) . ?
C22 C23 1.508(10) . ?
C25 C26 1.554(10) . ?
C26 C27 1.504(11) . ?
C26 C28 1.540(11) . ?
C26 C29 1.591(12) . ?
C30 C31 1.495(11) . ?
C30 C32 1.497(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Zr1 O4 126.62(17) . . ?
O1 Zr1 O3 76.24(15) . . ?
O4 Zr1 O3 128.48(16) . . ?
O1 Zr1 O2 128.91(16) . . ?
O4 Zr1 O2 77.08(16) . . ?
O3 Zr1 O2 127.91(16) . . ?
O1 Zr1 N2 86.10(17) . . ?
O4 Zr1 N2 135.14(16) . . ?
O3 Zr1 N2 84.63(16) . . ?
O2 Zr1 N2 58.05(16) . . ?
O1 Zr1 N3 134.34(16) . . ?
O4 Zr1 N3 85.35(18) . . ?
O3 Zr1 N3 58.14(16) . . ?
O2 Zr1 N3 85.42(17) . . ?
N2 Zr1 N3 91.05(19) . . ?
O1 Zr1 N4 83.45(17) . . ?
O4 Zr1 N4 57.89(17) . . ?
O3 Zr1 N4 85.34(15) . . ?
O2 Zr1 N4 134.97(17) . . ?
N2 Zr1 N4 166.96(18) . . ?
N3 Zr1 N4 90.71(18) . . ?
O1 Zr1 N1 57.69(15) . . ?
O4 Zr1 N1 85.67(17) . . ?
O3 Zr1 N1 133.86(17) . . ?
O2 Zr1 N1 84.79(16) . . ?
N2 Zr1 N1 89.68(19) . . ?
N3 Zr1 N1 167.97(17) . . ?
N4 Zr1 N1 91.28(17) . . ?
O1 Zr1 C25 105.87(17) . . ?
O4 Zr1 C25 28.69(16) . . ?
O3 Zr1 C25 108.52(15) . . ?
O2 Zr1 C25 105.77(16) . . ?
N2 Zr1 C25 163.80(17) . . ?
N3 Zr1 C25 88.22(19) . . ?
N4 Zr1 C25 29.20(16) . . ?
N1 Zr1 C25 87.73(19) . . ?
O1 Zr1 C17 105.38(16) . . ?
O4 Zr1 C17 107.80(18) . . ?
O3 Zr1 C17 29.17(17) . . ?
O2 Zr1 C17 107.89(17) . . ?
N2 Zr1 C17 87.79(19) . . ?
N3 Zr1 C17 28.97(17) . . ?
N4 Zr1 C17 87.51(17) . . ?
N1 Zr1 C17 163.03(17) . . ?
C25 Zr1 C17 99.17(18) . . ?
O1 Zr1 C1 28.79(16) . . ?
O4 Zr1 C1 106.92(16) . . ?
O3 Zr1 C1 105.02(16) . . ?
O2 Zr1 C1 108.29(17) . . ?
N2 Zr1 C1 88.21(18) . . ?
N3 Zr1 C1 163.12(16) . . ?
N4 Zr1 C1 86.37(18) . . ?
N1 Zr1 C1 28.91(17) . . ?
C25 Zr1 C1 97.11(18) . . ?
C17 Zr1 C1 134.17(17) . . ?
O1 Zr1 C9 108.90(16) . . ?
O4 Zr1 C9 105.86(16) . . ?
O3 Zr1 C9 107.47(14) . . ?
O2 Zr1 C9 28.78(16) . . ?
N2 Zr1 C9 29.28(16) . . ?
N3 Zr1 C9 87.90(16) . . ?
N4 Zr1 C9 163.75(17) . . ?
N1 Zr1 C9 86.88(16) . . ?
C25 Zr1 C9 134.55(17) . . ?
C17 Zr1 C9 98.87(16) . . ?
C1 Zr1 C9 99.44(17) . . ?
C1 O1 Zr1 97.0(3) . . ?
C9 O2 Zr1 96.8(3) . . ?
C17 O3 Zr1 96.0(3) . . ?
C25 O4 Zr1 96.0(4) . . ?
C1 N1 C6 126.3(5) . . ?
C1 N1 Zr1 91.6(3) . . ?
C6 N1 Zr1 142.1(4) . . ?
C9 N2 C14 125.4(5) . . ?
C9 N2 Zr1 92.5(4) . . ?
C14 N2 Zr1 142.1(4) . . ?
C17 N3 C22 125.6(5) . . ?
C17 N3 Zr1 91.8(4) . . ?
C22 N3 Zr1 142.6(4) . . ?
C25 N4 C30 128.1(6) . . ?
C25 N4 Zr1 90.3(4) . . ?
C30 N4 Zr1 141.5(4) . . ?
N1 C1 O1 113.7(5) . . ?
N1 C1 C2 128.1(5) . . ?
O1 C1 C2 118.2(5) . . ?
N1 C1 Zr1 59.5(3) . . ?
O1 C1 Zr1 54.2(3) . . ?
C2 C1 Zr1 172.4(4) . . ?
C4 C2 C3 107.6(5) . . ?
C4 C2 C1 111.7(6) . . ?
C3 C2 C1 108.5(5) . . ?
C4 C2 C5 110.8(6) . . ?
C3 C2 C5 107.5(6) . . ?
C1 C2 C5 110.6(5) . . ?
N1 C6 C8 110.6(5) . . ?
N1 C6 C7 110.0(5) . . ?
C8 C6 C7 110.6(6) . . ?
O2 C9 N2 112.7(5) . . ?
O2 C9 C10 118.3(5) . . ?
N2 C9 C10 129.1(5) . . ?
O2 C9 Zr1 54.4(2) . . ?
N2 C9 Zr1 58.3(3) . . ?
C10 C9 Zr1 172.7(4) . . ?
C13 C10 C9 111.9(5) . . ?
C13 C10 C11 107.6(5) . . ?
C9 C10 C11 109.6(5) . . ?
C13 C10 C12 110.3(6) . . ?
C9 C10 C12 109.5(4) . . ?
C11 C10 C12 107.7(6) . . ?
N2 C14 C15 109.5(6) . . ?
N2 C14 C16 110.0(6) . . ?
C15 C14 C16 112.1(6) . . ?
N3 C17 O3 114.1(5) . . ?
N3 C17 C18 129.7(6) . . ?
O3 C17 C18 116.2(5) . . ?
N3 C17 Zr1 59.3(3) . . ?
O3 C17 Zr1 54.8(2) . . ?
C18 C17 Zr1 171.0(4) . . ?
C19 C18 C17 110.2(5) . . ?
C19 C18 C20 108.4(6) . . ?
C17 C18 C20 110.6(5) . . ?
C19 C18 C21 107.9(6) . . ?
C17 C18 C21 109.8(5) . . ?
C20 C18 C21 109.8(6) . . ?
N3 C22 C24 110.9(5) . . ?
N3 C22 C23 110.1(5) . . ?
C24 C22 C23 110.0(6) . . ?
O4 C25 N4 115.7(6) . . ?
O4 C25 C26 115.8(5) . . ?
N4 C25 C26 128.4(6) . . ?
O4 C25 Zr1 55.3(3) . . ?
N4 C25 Zr1 60.4(4) . . ?
C26 C25 Zr1 171.1(4) . . ?
C27 C26 C28 109.4(7) . . ?
C27 C26 C25 109.6(6) . . ?
C28 C26 C25 110.3(6) . . ?
C27 C26 C29 108.0(7) . . ?
C28 C26 C29 111.2(6) . . ?
C25 C26 C29 108.3(7) . . ?
N4 C30 C31 109.5(5) . . ?
N4 C30 C32 111.1(5) . . ?
C31 C30 C32 113.1(8) . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         1.570
_refine_diff_density_min         -1.785
_refine_diff_density_rms         0.101

_cell_oxdiff_twin_number         2
loop_
_cell_oxdiff_twin_id
_cell_oxdiff_twin_matrix_11
_cell_oxdiff_twin_matrix_12
_cell_oxdiff_twin_matrix_13
_cell_oxdiff_twin_matrix_21
_cell_oxdiff_twin_matrix_22
_cell_oxdiff_twin_matrix_23
_cell_oxdiff_twin_matrix_31
_cell_oxdiff_twin_matrix_32
_cell_oxdiff_twin_matrix_33
1 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000
2 -1.0001 -0.0002 -0.5055 0.0003 -0.9996 -0.0001 0.0006 0.0003 1.0004
loop_
_diffrn_oxdiff_twin_id
_diffrn_oxdiff_twin_ratio
_diffrn_oxdiff_twin_reflns_isolated
_diffrn_oxdiff_twin_reflns_overlapped
1 0.6164 10306 7114
2 0.3836 10274 7114
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_e16msh10
_database_code_depnum_ccdc_archive 'CCDC 1498670'
_audit_update_record             
;
2016-08-10 deposited with the CCDC.
2016-10-31 downloaded from the CCDC.
;
_audit_creation_date             2016-05-16
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C28 H56 N4 O4 Zr'
_chemical_formula_sum            'C28 H56 N4 O4 Zr'
_chemical_formula_weight         603.98
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C28 H56 N4 O4 Zr'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.7212(6)
_cell_length_b                   16.1788(9)
_cell_length_c                   19.0915(10)
_cell_angle_alpha                68.599(5)
_cell_angle_beta                 79.594(4)
_cell_angle_gamma                81.912(5)
_cell_volume                     3304.3(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6713
_cell_measurement_temperature    150.0(3)
_cell_measurement_theta_max      27.0050
_cell_measurement_theta_min      3.8150
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.367
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98127
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.

Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.171
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0587
_diffrn_reflns_av_unetI/netI     0.1557
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            28277
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.301
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.0(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0734
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7659
_reflns_number_total             13381
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.564
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.810
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     699
_refine_ls_number_reflns         13381
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0924
_refine_ls_R_factor_gt           0.0464
_refine_ls_restrained_S_all      0.810
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0220P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0701
_refine_ls_wR_factor_ref         0.0756
_refine_special_details          
;
The asymmetric unit comprises 2 crystallographically independent 
molecules. There was some evidence for non-merohedral twinning in 
the collected frames of data, and integration os same was pursued. 
However, as the refined level of twinning refined top a value of 
5%, it was abandoned and the data presented herein reflect 
integration as a single crystal.
;


_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr1 Zr 0.70377(3) 0.78263(2) 0.25462(2) 0.01577(9) Uani 1 1 d . . . . .
O1 O 0.52019(17) 0.81939(13) 0.29114(12) 0.0216(5) Uani 1 1 d . . . . .
O2 O 0.83672(17) 0.71808(13) 0.32965(11) 0.0179(5) Uani 1 1 d . . . . .
O3 O 0.67666(18) 0.91909(13) 0.17507(12) 0.0213(5) Uani 1 1 d . . . . .
O4 O 0.78185(18) 0.67689(13) 0.21078(12) 0.0231(5) Uani 1 1 d . . . . .
N1 N 0.5894(2) 0.68208(17) 0.34643(15) 0.0202(6) Uani 1 1 d . . . . .
N2 N 0.7396(2) 0.83995(16) 0.34014(14) 0.0188(6) Uani 1 1 d . . . . .
N3 N 0.8560(2) 0.85970(16) 0.17543(15) 0.0209(6) Uani 1 1 d . . . . .
N4 N 0.6241(2) 0.75094(17) 0.16692(15) 0.0230(7) Uani 1 1 d . . . . .
C1 C 0.4994(3) 0.7401(2) 0.33865(19) 0.0228(8) Uani 1 1 d . . . . .
C2 C 0.3766(3) 0.7240(2) 0.3793(2) 0.0356(10) Uani 1 1 d . . . . .
H2 H 0.3600 0.6645 0.3837 0.043 Uiso 1 1 calc R . . . .
C3 C 0.2876(3) 0.7921(2) 0.3350(3) 0.0495(12) Uani 1 1 d . . . . .
H3A H 0.3076 0.8512 0.3255 0.074 Uiso 1 1 calc GR . . . .
H3B H 0.2116 0.7838 0.3641 0.074 Uiso 1 1 calc GR . . . .
H3C H 0.2878 0.7842 0.2875 0.074 Uiso 1 1 calc GR . . . .
C4 C 0.3682(3) 0.7267(3) 0.4595(2) 0.0566(12) Uani 1 1 d . . . . .
H4A H 0.4285 0.6865 0.4850 0.085 Uiso 1 1 calc GR . . . .
H4B H 0.2936 0.7092 0.4876 0.085 Uiso 1 1 calc GR . . . .
H4C H 0.3774 0.7861 0.4563 0.085 Uiso 1 1 calc GR . . . .
C5 C 0.5856(3) 0.5872(2) 0.3964(2) 0.0302(9) Uani 1 1 d . . . . .
H5 H 0.5059 0.5771 0.4223 0.036 Uiso 1 1 calc R . . . .
C6 C 0.6660(3) 0.5654(2) 0.4554(2) 0.0446(11) Uani 1 1 d . . . . .
H6A H 0.6665 0.5031 0.4854 0.067 Uiso 1 1 calc GR . . . .
H6B H 0.6392 0.5999 0.4877 0.067 Uiso 1 1 calc GR . . . .
H6C H 0.7433 0.5793 0.4306 0.067 Uiso 1 1 calc GR . . . .
C7 C 0.6186(4) 0.5291(2) 0.3476(2) 0.0551(12) Uani 1 1 d . . . . .
H7A H 0.6956 0.5399 0.3205 0.083 Uiso 1 1 calc GR . . . .
H7B H 0.5643 0.5430 0.3120 0.083 Uiso 1 1 calc GR . . . .
H7C H 0.6168 0.4675 0.3795 0.083 Uiso 1 1 calc GR . . . .
C8 C 0.8204(3) 0.7760(2) 0.36412(17) 0.0178(7) Uani 1 1 d . . . . .
C9 C 0.8915(3) 0.7628(2) 0.42622(18) 0.0232(8) Uani 1 1 d . . . . .
H9 H 0.9227 0.8195 0.4172 0.028 Uiso 1 1 calc R . . . .
C10 C 0.8131(3) 0.7364(2) 0.50363(19) 0.0361(9) Uani 1 1 d . . . . .
H10A H 0.7505 0.7818 0.5028 0.054 Uiso 1 1 calc GR . . . .
H10B H 0.8581 0.7302 0.5429 0.054 Uiso 1 1 calc GR . . . .
H10C H 0.7819 0.6809 0.5135 0.054 Uiso 1 1 calc GR . . . .
C11 C 0.9930(3) 0.6927(2) 0.42783(19) 0.0290(9) Uani 1 1 d . . . . .
H11A H 0.9639 0.6358 0.4401 0.044 Uiso 1 1 calc GR . . . .
H11B H 1.0393 0.6897 0.4655 0.044 Uiso 1 1 calc GR . . . .
H11C H 1.0401 0.7083 0.3789 0.044 Uiso 1 1 calc GR . . . .
C12 C 0.7102(3) 0.9147(2) 0.36863(19) 0.0261(8) Uani 1 1 d . . . . .
H12 H 0.7615 0.9077 0.4060 0.031 Uiso 1 1 calc R . . . .
C13 C 0.5856(3) 0.9131(2) 0.4076(2) 0.0336(9) Uani 1 1 d . . . . .
H13A H 0.5664 0.9631 0.4245 0.050 Uiso 1 1 calc GR . . . .
H13B H 0.5771 0.8589 0.4505 0.050 Uiso 1 1 calc GR . . . .
H13C H 0.5344 0.9163 0.3726 0.050 Uiso 1 1 calc GR . . . .
C14 C 0.7308(3) 1.0017(2) 0.3037(2) 0.0360(10) Uani 1 1 d . . . . .
H14A H 0.6838 1.0082 0.2654 0.054 Uiso 1 1 calc GR . . . .
H14B H 0.8115 1.0018 0.2822 0.054 Uiso 1 1 calc GR . . . .
H14C H 0.7102 1.0504 0.3222 0.054 Uiso 1 1 calc GR . . . .
C15 C 0.7844(3) 0.9245(2) 0.14311(18) 0.0207(8) Uani 1 1 d . . . . .
C16 C 0.8118(3) 1.0014(2) 0.06902(18) 0.0247(8) Uani 1 1 d . . . . .
H16 H 0.8891 1.0196 0.0667 0.030 Uiso 1 1 calc R . . . .
C17 C 0.7225(3) 1.0807(2) 0.0632(2) 0.0368(10) Uani 1 1 d . . . . .
H17A H 0.6483 1.0653 0.0594 0.055 Uiso 1 1 calc GR . . . .
H17B H 0.7466 1.1303 0.0188 0.055 Uiso 1 1 calc GR . . . .
H17C H 0.7164 1.0965 0.1076 0.055 Uiso 1 1 calc GR . . . .
C18 C 0.8132(3) 0.9682(2) 0.00318(19) 0.0415(10) Uani 1 1 d . . . . .
H18A H 0.8750 0.9221 0.0047 0.062 Uiso 1 1 calc GR . . . .
H18B H 0.8253 1.0168 -0.0442 0.062 Uiso 1 1 calc GR . . . .
H18C H 0.7401 0.9450 0.0078 0.062 Uiso 1 1 calc GR . . . .
C19 C 0.9836(3) 0.8544(2) 0.1528(2) 0.0288(9) Uani 1 1 d . . . . .
H19 H 1.0013 0.8949 0.1004 0.035 Uiso 1 1 calc R . . . .
C20 C 1.0411(3) 0.8834(2) 0.2037(2) 0.0436(10) Uani 1 1 d . . . . .
H20A H 1.0184 0.8478 0.2558 0.065 Uiso 1 1 calc GR . . . .
H20B H 1.0175 0.9449 0.1964 0.065 Uiso 1 1 calc GR . . . .
H20C H 1.1242 0.8760 0.1914 0.065 Uiso 1 1 calc GR . . . .
C21 C 1.0302(3) 0.7613(3) 0.1569(3) 0.0711(16) Uani 1 1 d . . . . .
H21A H 1.1134 0.7590 0.1443 0.107 Uiso 1 1 calc GR . . . .
H21B H 0.9974 0.7452 0.1216 0.107 Uiso 1 1 calc GR . . . .
H21C H 1.0096 0.7205 0.2075 0.107 Uiso 1 1 calc GR . . . .
C22 C 0.7091(3) 0.6909(2) 0.16373(19) 0.0231(8) Uani 1 1 d . . . . .
C23 C 0.7340(3) 0.6426(2) 0.1073(2) 0.0308(9) Uani 1 1 d . . . . .
H23 H 0.6618 0.6451 0.0872 0.037 Uiso 1 1 calc R . . . .
C24 C 0.7749(3) 0.5457(2) 0.1448(2) 0.0419(11) Uani 1 1 d . . . . .
H24A H 0.8427 0.5420 0.1678 0.063 Uiso 1 1 calc GR . . . .
H24B H 0.7937 0.5176 0.1073 0.063 Uiso 1 1 calc GR . . . .
H24C H 0.7143 0.5162 0.1831 0.063 Uiso 1 1 calc GR . . . .
C25 C 0.8234(4) 0.6904(3) 0.0416(2) 0.0565(13) Uani 1 1 d . . . . .
H25A H 0.7970 0.7522 0.0208 0.085 Uiso 1 1 calc GR . . . .
H25B H 0.8332 0.6641 0.0030 0.085 Uiso 1 1 calc GR . . . .
H25C H 0.8964 0.6850 0.0597 0.085 Uiso 1 1 calc GR . . . .
C26 C 0.5288(3) 0.7730(2) 0.1206(2) 0.0330(9) Uani 1 1 d . . . . .
H26 H 0.5609 0.7708 0.0702 0.040 Uiso 1 1 calc R . . . .
C27 C 0.4380(3) 0.7061(2) 0.1568(2) 0.0472(12) Uani 1 1 d . . . . .
H27A H 0.4071 0.7067 0.2067 0.071 Uiso 1 1 calc GR . . . .
H27B H 0.4731 0.6476 0.1603 0.071 Uiso 1 1 calc GR . . . .
H27C H 0.3763 0.7215 0.1262 0.071 Uiso 1 1 calc GR . . . .
C28 C 0.4744(3) 0.8666(2) 0.1117(2) 0.0437(11) Uani 1 1 d . . . . .
H28A H 0.4118 0.8805 0.0820 0.065 Uiso 1 1 calc GR . . . .
H28B H 0.5322 0.9085 0.0867 0.065 Uiso 1 1 calc GR . . . .
H28C H 0.4448 0.8701 0.1610 0.065 Uiso 1 1 calc GR . . . .
Zr2 Zr 0.18975(3) 0.28117(2) 0.24148(2) 0.01429(9) Uani 1 1 d . . . . .
O5 O 0.14851(18) 0.35575(13) 0.31997(12) 0.0205(5) Uani 1 1 d . . . . .
O6 O 0.31706(17) 0.31354(13) 0.13663(11) 0.0174(5) Uani 1 1 d . . . . .
O7 O 0.19116(18) 0.17610(13) 0.35362(11) 0.0200(5) Uani 1 1 d . . . . .
O8 O 0.09308(18) 0.27302(13) 0.15697(12) 0.0187(5) Uani 1 1 d . . . . .
N5 N 0.1443(2) 0.43117(16) 0.19903(15) 0.0179(6) Uani 1 1 d . . . . .
N6 N 0.3805(2) 0.29804(17) 0.24207(15) 0.0193(6) Uani 1 1 d . . . . .
N7 N 0.2547(2) 0.13586(16) 0.25446(14) 0.0178(6) Uani 1 1 d . . . . .
N8 N -0.0062(2) 0.25824(16) 0.26921(14) 0.0184(6) Uani 1 1 d . . . . .
C29 C 0.1297(3) 0.4328(2) 0.2677(2) 0.0225(8) Uani 1 1 d . . . . .
C30 C 0.0913(3) 0.5128(2) 0.2920(2) 0.0291(9) Uani 1 1 d . . . . .
H30 H 0.0850 0.5656 0.2463 0.035 Uiso 1 1 calc R . . . .
C31 C -0.0258(3) 0.5022(3) 0.3395(3) 0.0529(13) Uani 1 1 d . . . . .
H31A H -0.0808 0.4939 0.3114 0.079 Uiso 1 1 calc GR . . . .
H31B H -0.0507 0.5546 0.3524 0.079 Uiso 1 1 calc GR . . . .
H31C H -0.0211 0.4513 0.3851 0.079 Uiso 1 1 calc GR . . . .
C32 C 0.1809(3) 0.5262(3) 0.3344(3) 0.0620(14) Uani 1 1 d . . . . .
H32A H 0.1911 0.4738 0.3782 0.093 Uiso 1 1 calc GR . . . .
H32B H 0.1545 0.5763 0.3504 0.093 Uiso 1 1 calc GR . . . .
H32C H 0.2537 0.5371 0.3016 0.093 Uiso 1 1 calc GR . . . .
C33 C 0.1292(3) 0.5105(2) 0.13191(18) 0.0256(8) Uani 1 1 d . . . . .
H33 H 0.0625 0.5486 0.1452 0.031 Uiso 1 1 calc R . . . .
C34 C 0.1023(4) 0.4829(2) 0.0697(2) 0.0482(12) Uani 1 1 d . . . . .
H34A H 0.0918 0.5348 0.0256 0.072 Uiso 1 1 calc GR . . . .
H34B H 0.0324 0.4523 0.0868 0.072 Uiso 1 1 calc GR . . . .
H34C H 0.1657 0.4439 0.0571 0.072 Uiso 1 1 calc GR . . . .
C35 C 0.2356(3) 0.5631(2) 0.1060(2) 0.0428(10) Uani 1 1 d . . . . .
H35A H 0.3001 0.5289 0.0881 0.064 Uiso 1 1 calc GR . . . .
H35B H 0.2543 0.5756 0.1479 0.064 Uiso 1 1 calc GR . . . .
H35C H 0.2200 0.6180 0.0657 0.064 Uiso 1 1 calc GR . . . .
C36 C 0.4042(3) 0.3109(2) 0.16989(19) 0.0192(8) Uani 1 1 d . . . . .
C37 C 0.5236(3) 0.3248(2) 0.12155(19) 0.0250(8) Uani 1 1 d . . . . .
H37 H 0.5817 0.2842 0.1513 0.030 Uiso 1 1 calc R . . . .
C38 C 0.5274(3) 0.3039(2) 0.04978(19) 0.0368(10) Uani 1 1 d . . . . .
H38A H 0.5059 0.2444 0.0631 0.055 Uiso 1 1 calc GR . . . .
H38B H 0.6047 0.3089 0.0223 0.055 Uiso 1 1 calc GR . . . .
H38C H 0.4739 0.3453 0.0186 0.055 Uiso 1 1 calc GR . . . .
C39 C 0.5532(3) 0.4208(2) 0.1025(2) 0.0382(10) Uani 1 1 d . . . . .
H39A H 0.4953 0.4616 0.0749 0.057 Uiso 1 1 calc GR . . . .
H39B H 0.6281 0.4296 0.0720 0.057 Uiso 1 1 calc GR . . . .
H39C H 0.5544 0.4313 0.1487 0.057 Uiso 1 1 calc GR . . . .
C40 C 0.4677(3) 0.2913(2) 0.29067(18) 0.0258(8) Uani 1 1 d . . . . .
H40 H 0.5436 0.3021 0.2590 0.031 Uiso 1 1 calc R . . . .
C41 C 0.4756(3) 0.1988(2) 0.3505(2) 0.0434(11) Uani 1 1 d . . . . .
H41A H 0.5330 0.1953 0.3818 0.065 Uiso 1 1 calc GR . . . .
H41B H 0.4975 0.1554 0.3261 0.065 Uiso 1 1 calc GR . . . .
H41C H 0.4014 0.1872 0.3815 0.065 Uiso 1 1 calc GR . . . .
C42 C 0.4362(3) 0.3614(2) 0.3273(2) 0.0387(10) Uani 1 1 d . . . . .
H42A H 0.3610 0.3525 0.3575 0.058 Uiso 1 1 calc GR . . . .
H42B H 0.4343 0.4194 0.2885 0.058 Uiso 1 1 calc GR . . . .
H42C H 0.4931 0.3570 0.3591 0.058 Uiso 1 1 calc GR . . . .
C43 C 0.2263(3) 0.1124(2) 0.32732(19) 0.0202(8) Uani 1 1 d . . . . .
C44 C 0.2226(3) 0.0169(2) 0.38422(19) 0.0277(8) Uani 1 1 d . . . . .
H44 H 0.2837 -0.0209 0.3655 0.033 Uiso 1 1 calc R . . . .
C45 C 0.1038(3) -0.0159(2) 0.3880(2) 0.0446(11) Uani 1 1 d . . . . .
H45A H 0.0428 0.0226 0.4037 0.067 Uiso 1 1 calc GR . . . .
H45B H 0.0995 -0.0755 0.4239 0.067 Uiso 1 1 calc GR . . . .
H45C H 0.0950 -0.0151 0.3387 0.067 Uiso 1 1 calc GR . . . .
C46 C 0.2433(4) 0.0111(2) 0.46242(19) 0.0427(11) Uani 1 1 d . . . . .
H46A H 0.3160 0.0346 0.4581 0.064 Uiso 1 1 calc GR . . . .
H46B H 0.2457 -0.0501 0.4956 0.064 Uiso 1 1 calc GR . . . .
H46C H 0.1813 0.0449 0.4828 0.064 Uiso 1 1 calc GR . . . .
C47 C 0.3093(3) 0.0735(2) 0.21610(18) 0.0241(8) Uani 1 1 d . . . . .
H47 H 0.2748 0.0164 0.2418 0.029 Uiso 1 1 calc R . . . .
C48 C 0.4395(3) 0.0589(2) 0.2207(2) 0.0346(9) Uani 1 1 d . . . . .
H48A H 0.4742 0.0155 0.1981 0.052 Uiso 1 1 calc GR . . . .
H48B H 0.4516 0.0380 0.2729 0.052 Uiso 1 1 calc GR . . . .
H48C H 0.4745 0.1141 0.1938 0.052 Uiso 1 1 calc GR . . . .
C49 C 0.2882(3) 0.1094(2) 0.13365(19) 0.0341(9) Uani 1 1 d . . . . .
H49A H 0.3131 0.1685 0.1097 0.051 Uiso 1 1 calc GR . . . .
H49B H 0.2068 0.1107 0.1315 0.051 Uiso 1 1 calc GR . . . .
H49C H 0.3316 0.0715 0.1077 0.051 Uiso 1 1 calc GR . . . .
C50 C -0.0028(3) 0.25218(19) 0.20290(18) 0.0192(8) Uani 1 1 d . . . . .
C51 C -0.0957(3) 0.2203(2) 0.17525(19) 0.0233(8) Uani 1 1 d . . . . .
H51 H -0.1617 0.2041 0.2158 0.028 Uiso 1 1 calc R . . . .
C52 C -0.0444(3) 0.1386(2) 0.1551(2) 0.0428(11) Uani 1 1 d . . . . .
H52A H 0.0155 0.1555 0.1121 0.064 Uiso 1 1 calc GR . . . .
H52B H -0.1046 0.1138 0.1427 0.064 Uiso 1 1 calc GR . . . .
H52C H -0.0118 0.0950 0.1976 0.064 Uiso 1 1 calc GR . . . .
C53 C -0.1369(3) 0.2938(2) 0.1061(2) 0.0376(10) Uani 1 1 d . . . . .
H53A H -0.1707 0.3443 0.1199 0.056 Uiso 1 1 calc GR . . . .
H53B H -0.1941 0.2726 0.0881 0.056 Uiso 1 1 calc GR . . . .
H53C H -0.0720 0.3111 0.0668 0.056 Uiso 1 1 calc GR . . . .
C54 C -0.1080(3) 0.2387(2) 0.32877(19) 0.0243(8) Uani 1 1 d . . . . .
H54 H -0.1369 0.1835 0.3316 0.029 Uiso 1 1 calc R . . . .
C55 C -0.2053(3) 0.3137(2) 0.3089(2) 0.0378(10) Uani 1 1 d . . . . .
H55A H -0.2716 0.2994 0.3476 0.057 Uiso 1 1 calc GR . . . .
H55B H -0.2270 0.3201 0.2609 0.057 Uiso 1 1 calc GR . . . .
H55C H -0.1783 0.3685 0.3057 0.057 Uiso 1 1 calc GR . . . .
C56 C -0.0742(3) 0.2254(2) 0.40522(19) 0.0357(10) Uani 1 1 d . . . . .
H56A H -0.0459 0.2791 0.4035 0.054 Uiso 1 1 calc GR . . . .
H56B H -0.0143 0.1775 0.4171 0.054 Uiso 1 1 calc GR . . . .
H56C H -0.1409 0.2111 0.4435 0.054 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr1 O1 2.207(2) . ?
Zr1 O2 2.197(2) . ?
Zr1 O3 2.194(2) . ?
Zr1 O4 2.1893(19) . ?
Zr1 N1 2.280(3) . ?
Zr1 N2 2.272(2) . ?
Zr1 N3 2.302(3) . ?
Zr1 N4 2.295(2) . ?
Zr1 C1 2.656(3) . ?
Zr1 C8 2.660(3) . ?
Zr1 C15 2.648(3) . ?
Zr1 C22 2.652(3) . ?
O1 C1 1.298(4) . ?
O2 C8 1.304(3) . ?
O3 C15 1.299(4) . ?
O4 C22 1.288(4) . ?
N1 C1 1.301(4) . ?
N1 C5 1.485(4) . ?
N2 C8 1.309(4) . ?
N2 C12 1.474(3) . ?
N3 C15 1.286(4) . ?
N3 C19 1.479(4) . ?
N4 C22 1.300(4) . ?
N4 C26 1.474(4) . ?
C1 C2 1.516(4) . ?
C2 H2 0.9800 . ?
C2 C3 1.528(5) . ?
C2 C4 1.533(5) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 H5 0.9800 . ?
C5 C6 1.511(5) . ?
C5 C7 1.518(4) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 C9 1.506(4) . ?
C9 H9 0.9800 . ?
C9 C10 1.540(4) . ?
C9 C11 1.520(4) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12 0.9800 . ?
C12 C13 1.513(4) . ?
C12 C14 1.514(4) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 C16 1.522(4) . ?
C16 H16 0.9800 . ?
C16 C17 1.521(4) . ?
C16 C18 1.533(4) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19 0.9800 . ?
C19 C20 1.510(4) . ?
C19 C21 1.507(4) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 C23 1.515(4) . ?
C23 H23 0.9800 . ?
C23 C24 1.514(5) . ?
C23 C25 1.521(5) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26 0.9800 . ?
C26 C27 1.515(4) . ?
C26 C28 1.520(4) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
Zr2 O5 2.1975(19) . ?
Zr2 O6 2.210(2) . ?
Zr2 O7 2.196(2) . ?
Zr2 O8 2.1820(18) . ?
Zr2 N5 2.278(2) . ?
Zr2 N6 2.292(2) . ?
Zr2 N7 2.304(2) . ?
Zr2 N8 2.313(2) . ?
Zr2 C29 2.655(3) . ?
Zr2 C36 2.652(3) . ?
Zr2 C43 2.642(3) . ?
Zr2 C50 2.647(3) . ?
O5 C29 1.301(4) . ?
O6 C36 1.284(3) . ?
O7 C43 1.291(3) . ?
O8 C50 1.296(4) . ?
N5 C29 1.301(4) . ?
N5 C33 1.463(4) . ?
N6 C36 1.299(4) . ?
N6 C40 1.468(4) . ?
N7 C43 1.293(4) . ?
N7 C47 1.467(4) . ?
N8 C50 1.298(4) . ?
N8 C54 1.474(4) . ?
C29 C30 1.513(4) . ?
C30 H30 0.9800 . ?
C30 C31 1.496(5) . ?
C30 C32 1.519(5) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33 0.9800 . ?
C33 C34 1.508(4) . ?
C33 C35 1.514(4) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 C37 1.527(4) . ?
C37 H37 0.9800 . ?
C37 C38 1.518(4) . ?
C37 C39 1.536(4) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
C40 H40 0.9800 . ?
C40 C41 1.518(5) . ?
C40 C42 1.510(4) . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 C44 1.531(4) . ?
C44 H44 0.9800 . ?
C44 C45 1.539(4) . ?
C44 C46 1.523(4) . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C47 H47 0.9800 . ?
C47 C48 1.525(4) . ?
C47 C49 1.519(4) . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
C49 H49A 0.9600 . ?
C49 H49B 0.9600 . ?
C49 H49C 0.9600 . ?
C50 C51 1.515(4) . ?
C51 H51 0.9800 . ?
C51 C52 1.524(4) . ?
C51 C53 1.521(4) . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?
C53 H53A 0.9600 . ?
C53 H53B 0.9600 . ?
C53 H53C 0.9600 . ?
C54 H54 0.9800 . ?
C54 C55 1.531(4) . ?
C54 C56 1.513(4) . ?
C55 H55A 0.9600 . ?
C55 H55B 0.9600 . ?
C55 H55C 0.9600 . ?
C56 H56A 0.9600 . ?
C56 H56B 0.9600 . ?
C56 H56C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Zr1 N1 58.42(8) . . ?
O1 Zr1 N2 83.71(8) . . ?
O1 Zr1 N3 134.79(9) . . ?
O1 Zr1 N4 82.58(9) . . ?
O1 Zr1 C1 29.14(8) . . ?
O1 Zr1 C8 105.98(9) . . ?
O1 Zr1 C15 106.91(9) . . ?
O1 Zr1 C22 108.36(9) . . ?
O2 Zr1 O1 125.92(8) . . ?
O2 Zr1 N1 83.24(8) . . ?
O2 Zr1 N2 58.67(8) . . ?
O2 Zr1 N3 83.32(9) . . ?
O2 Zr1 N4 136.16(9) . . ?
O2 Zr1 C1 106.47(9) . . ?
O2 Zr1 C8 29.20(8) . . ?
O2 Zr1 C15 109.62(9) . . ?
O2 Zr1 C22 107.58(9) . . ?
O3 Zr1 O1 77.78(8) . . ?
O3 Zr1 O2 131.96(7) . . ?
O3 Zr1 N1 135.89(9) . . ?
O3 Zr1 N2 88.67(8) . . ?
O3 Zr1 N3 58.10(9) . . ?
O3 Zr1 N4 81.68(8) . . ?
O3 Zr1 C1 106.64(10) . . ?
O3 Zr1 C8 111.82(8) . . ?
O3 Zr1 C15 29.25(8) . . ?
O3 Zr1 C22 100.58(9) . . ?
O4 Zr1 O1 130.72(7) . . ?
O4 Zr1 O2 78.84(7) . . ?
O4 Zr1 O3 119.50(8) . . ?
O4 Zr1 N1 88.88(8) . . ?
O4 Zr1 N2 137.14(9) . . ?
O4 Zr1 N3 83.85(8) . . ?
O4 Zr1 N4 58.17(9) . . ?
O4 Zr1 C1 110.48(9) . . ?
O4 Zr1 C8 107.90(9) . . ?
O4 Zr1 C15 100.73(9) . . ?
O4 Zr1 C22 28.89(9) . . ?
N1 Zr1 N3 165.73(9) . . ?
N1 Zr1 N4 87.40(9) . . ?
N1 Zr1 C1 29.32(9) . . ?
N1 Zr1 C8 86.87(9) . . ?
N1 Zr1 C15 165.11(10) . . ?
N1 Zr1 C22 89.28(9) . . ?
N2 Zr1 N1 91.31(9) . . ?
N2 Zr1 N3 85.77(9) . . ?
N2 Zr1 N4 164.64(9) . . ?
N2 Zr1 C1 88.37(9) . . ?
N2 Zr1 C8 29.46(9) . . ?
N2 Zr1 C15 89.31(9) . . ?
N2 Zr1 C22 166.01(10) . . ?
N3 Zr1 C1 163.72(10) . . ?
N3 Zr1 C8 83.73(9) . . ?
N3 Zr1 C15 29.05(9) . . ?
N3 Zr1 C22 90.23(9) . . ?
N4 Zr1 N3 99.05(9) . . ?
N4 Zr1 C1 83.02(10) . . ?
N4 Zr1 C8 165.05(10) . . ?
N4 Zr1 C15 88.07(9) . . ?
N4 Zr1 C22 29.34(9) . . ?
C1 Zr1 C8 98.45(9) . . ?
C15 Zr1 C1 135.88(11) . . ?
C15 Zr1 C8 100.75(9) . . ?
C15 Zr1 C22 93.69(9) . . ?
C22 Zr1 C1 98.84(9) . . ?
C22 Zr1 C8 136.73(11) . . ?
C1 O1 Zr1 94.97(19) . . ?
C8 O2 Zr1 95.50(17) . . ?
C15 O3 Zr1 95.16(19) . . ?
C22 O4 Zr1 95.91(19) . . ?
C1 N1 Zr1 91.6(2) . . ?
C1 N1 C5 124.2(3) . . ?
C5 N1 Zr1 143.9(2) . . ?
C8 N2 Zr1 91.92(18) . . ?
C8 N2 C12 123.2(2) . . ?
C12 N2 Zr1 144.8(2) . . ?
C15 N3 Zr1 90.6(2) . . ?
C15 N3 C19 125.2(3) . . ?
C19 N3 Zr1 144.1(2) . . ?
C22 N4 Zr1 90.76(19) . . ?
C22 N4 C26 123.0(3) . . ?
C26 N4 Zr1 146.2(2) . . ?
O1 C1 Zr1 55.88(15) . . ?
O1 C1 N1 114.9(3) . . ?
O1 C1 C2 118.5(3) . . ?
N1 C1 Zr1 59.12(17) . . ?
N1 C1 C2 126.7(3) . . ?
C2 C1 Zr1 173.5(3) . . ?
C1 C2 H2 108.4 . . ?
C1 C2 C3 111.2(3) . . ?
C1 C2 C4 109.3(3) . . ?
C3 C2 H2 108.4 . . ?
C3 C2 C4 111.0(3) . . ?
C4 C2 H2 108.4 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N1 C5 H5 108.7 . . ?
N1 C5 C6 110.1(2) . . ?
N1 C5 C7 108.9(3) . . ?
C6 C5 H5 108.7 . . ?
C6 C5 C7 111.6(3) . . ?
C7 C5 H5 108.7 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O2 C8 Zr1 55.30(13) . . ?
O2 C8 N2 113.9(3) . . ?
O2 C8 C9 118.9(3) . . ?
N2 C8 Zr1 58.61(15) . . ?
N2 C8 C9 127.2(3) . . ?
C9 C8 Zr1 174.1(2) . . ?
C8 C9 H9 108.3 . . ?
C8 C9 C10 109.7(3) . . ?
C8 C9 C11 112.3(2) . . ?
C10 C9 H9 108.3 . . ?
C11 C9 H9 108.3 . . ?
C11 C9 C10 109.8(3) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N2 C12 H12 108.4 . . ?
N2 C12 C13 110.0(2) . . ?
N2 C12 C14 109.7(3) . . ?
C13 C12 H12 108.4 . . ?
C13 C12 C14 111.8(3) . . ?
C14 C12 H12 108.4 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O3 C15 Zr1 55.60(15) . . ?
O3 C15 C16 117.8(3) . . ?
N3 C15 Zr1 60.40(18) . . ?
N3 C15 O3 115.4(3) . . ?
N3 C15 C16 126.5(3) . . ?
C16 C15 Zr1 166.8(2) . . ?
C15 C16 H16 109.0 . . ?
C15 C16 C18 108.1(2) . . ?
C17 C16 C15 111.3(3) . . ?
C17 C16 H16 109.0 . . ?
C17 C16 C18 110.4(3) . . ?
C18 C16 H16 109.0 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N3 C19 H19 108.7 . . ?
N3 C19 C20 109.5(3) . . ?
N3 C19 C21 111.1(3) . . ?
C20 C19 H19 108.7 . . ?
C21 C19 H19 108.7 . . ?
C21 C19 C20 110.2(3) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O4 C22 Zr1 55.20(14) . . ?
O4 C22 N4 114.9(3) . . ?
O4 C22 C23 118.5(3) . . ?
N4 C22 Zr1 59.90(16) . . ?
N4 C22 C23 126.4(3) . . ?
C23 C22 Zr1 170.0(2) . . ?
C22 C23 H23 108.4 . . ?
C22 C23 C25 109.1(3) . . ?
C24 C23 C22 111.3(3) . . ?
C24 C23 H23 108.4 . . ?
C24 C23 C25 111.4(3) . . ?
C25 C23 H23 108.4 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N4 C26 H26 108.7 . . ?
N4 C26 C27 110.4(3) . . ?
N4 C26 C28 109.8(2) . . ?
C27 C26 H26 108.7 . . ?
C27 C26 C28 110.5(3) . . ?
C28 C26 H26 108.7 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O5 Zr2 O6 126.48(7) . . ?
O5 Zr2 N5 58.53(8) . . ?
O5 Zr2 N6 85.61(8) . . ?
O5 Zr2 N7 134.31(8) . . ?
O5 Zr2 N8 84.88(8) . . ?
O5 Zr2 C29 29.20(9) . . ?
O5 Zr2 C36 108.28(8) . . ?
O5 Zr2 C43 105.84(9) . . ?
O5 Zr2 C50 110.71(9) . . ?
O6 Zr2 N5 82.98(8) . . ?
O6 Zr2 N6 58.11(8) . . ?
O6 Zr2 N7 84.06(8) . . ?
O6 Zr2 N8 134.51(8) . . ?
O6 Zr2 C29 105.94(9) . . ?
O6 Zr2 C36 28.83(8) . . ?
O6 Zr2 C43 110.22(9) . . ?
O6 Zr2 C50 105.72(9) . . ?
O7 Zr2 O5 76.84(7) . . ?
O7 Zr2 O6 132.60(8) . . ?
O7 Zr2 N5 135.15(8) . . ?
O7 Zr2 N6 88.47(8) . . ?
O7 Zr2 N7 58.32(8) . . ?
O7 Zr2 N8 81.28(8) . . ?
O7 Zr2 C29 105.93(9) . . ?
O7 Zr2 C36 111.24(9) . . ?
O7 Zr2 C43 29.12(8) . . ?
O7 Zr2 C50 100.54(9) . . ?
O8 Zr2 O5 131.23(8) . . ?
O8 Zr2 O6 76.56(7) . . ?
O8 Zr2 O7 121.78(7) . . ?
O8 Zr2 N5 88.32(8) . . ?
O8 Zr2 N6 134.20(9) . . ?
O8 Zr2 N7 84.20(8) . . ?
O8 Zr2 N8 58.30(8) . . ?
O8 Zr2 C29 111.03(9) . . ?
O8 Zr2 C36 105.01(9) . . ?
O8 Zr2 C43 102.77(8) . . ?
O8 Zr2 C50 29.16(8) . . ?
N5 Zr2 N6 92.12(9) . . ?
N5 Zr2 N7 166.25(9) . . ?
N5 Zr2 N8 89.98(9) . . ?
N5 Zr2 C29 29.33(9) . . ?
N5 Zr2 C36 88.40(9) . . ?
N5 Zr2 C43 164.27(9) . . ?
N5 Zr2 C50 91.78(9) . . ?
N6 Zr2 N7 84.91(9) . . ?
N6 Zr2 N8 167.37(9) . . ?
N6 Zr2 C29 88.98(9) . . ?
N6 Zr2 C36 29.33(9) . . ?
N6 Zr2 C43 88.07(9) . . ?
N6 Zr2 C50 162.69(9) . . ?
N7 Zr2 N8 95.84(8) . . ?
N7 Zr2 C29 163.16(10) . . ?
N7 Zr2 C36 82.44(9) . . ?
N7 Zr2 C43 29.31(9) . . ?
N7 Zr2 C50 87.31(9) . . ?
N8 Zr2 C29 86.77(9) . . ?
N8 Zr2 C36 163.28(9) . . ?
N8 Zr2 C43 86.55(9) . . ?
N8 Zr2 C50 29.37(9) . . ?
C36 Zr2 C29 99.71(9) . . ?
C43 Zr2 C29 135.01(10) . . ?
C43 Zr2 C36 99.23(10) . . ?
C43 Zr2 C50 92.68(9) . . ?
C50 Zr2 C29 102.50(9) . . ?
C50 Zr2 C36 134.05(10) . . ?
C29 O5 Zr2 95.30(17) . . ?
C36 O6 Zr2 95.08(18) . . ?
C43 O7 Zr2 94.99(18) . . ?
C50 O8 Zr2 95.72(17) . . ?
C29 N5 Zr2 91.6(2) . . ?
C29 N5 C33 123.4(3) . . ?
C33 N5 Zr2 144.95(18) . . ?
C36 N6 Zr2 90.88(19) . . ?
C36 N6 C40 124.3(3) . . ?
C40 N6 Zr2 144.5(2) . . ?
C43 N7 Zr2 90.03(19) . . ?
C43 N7 C47 123.3(3) . . ?
C47 N7 Zr2 146.7(2) . . ?
C50 N8 Zr2 89.7(2) . . ?
C50 N8 C54 123.5(3) . . ?
C54 N8 Zr2 145.96(19) . . ?
O5 C29 Zr2 55.50(14) . . ?
O5 C29 N5 114.5(3) . . ?
O5 C29 C30 118.3(3) . . ?
N5 C29 Zr2 59.03(16) . . ?
N5 C29 C30 127.2(3) . . ?
C30 C29 Zr2 173.5(2) . . ?
C29 C30 H30 108.3 . . ?
C29 C30 C32 110.4(3) . . ?
C31 C30 C29 110.4(3) . . ?
C31 C30 H30 108.3 . . ?
C31 C30 C32 111.1(3) . . ?
C32 C30 H30 108.3 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N5 C33 H33 108.4 . . ?
N5 C33 C34 109.1(2) . . ?
N5 C33 C35 111.3(3) . . ?
C34 C33 H33 108.4 . . ?
C34 C33 C35 111.3(3) . . ?
C35 C33 H33 108.4 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
O6 C36 Zr2 56.09(15) . . ?
O6 C36 N6 115.7(3) . . ?
O6 C36 C37 117.8(3) . . ?
N6 C36 Zr2 59.79(17) . . ?
N6 C36 C37 126.4(3) . . ?
C37 C36 Zr2 173.3(2) . . ?
C36 C37 H37 108.4 . . ?
C36 C37 C39 109.5(3) . . ?
C38 C37 C36 111.0(3) . . ?
C38 C37 H37 108.4 . . ?
C38 C37 C39 111.1(3) . . ?
C39 C37 H37 108.4 . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C37 C39 H39A 109.5 . . ?
C37 C39 H39B 109.5 . . ?
C37 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
N6 C40 H40 108.7 . . ?
N6 C40 C41 110.3(2) . . ?
N6 C40 C42 109.5(3) . . ?
C41 C40 H40 108.7 . . ?
C42 C40 H40 108.7 . . ?
C42 C40 C41 110.8(3) . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C40 C42 H42A 109.5 . . ?
C40 C42 H42B 109.5 . . ?
C40 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
O7 C43 Zr2 55.89(15) . . ?
O7 C43 N7 116.2(3) . . ?
O7 C43 C44 117.2(3) . . ?
N7 C43 Zr2 60.67(17) . . ?
N7 C43 C44 126.4(3) . . ?
C44 C43 Zr2 168.7(2) . . ?
C43 C44 H44 108.5 . . ?
C43 C44 C45 108.3(3) . . ?
C45 C44 H44 108.5 . . ?
C46 C44 C43 111.7(2) . . ?
C46 C44 H44 108.5 . . ?
C46 C44 C45 111.1(3) . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C44 C46 H46A 109.5 . . ?
C44 C46 H46B 109.5 . . ?
C44 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
N7 C47 H47 108.9 . . ?
N7 C47 C48 109.6(2) . . ?
N7 C47 C49 110.2(3) . . ?
C48 C47 H47 108.9 . . ?
C49 C47 H47 108.9 . . ?
C49 C47 C48 110.2(3) . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C47 C49 H49A 109.5 . . ?
C47 C49 H49B 109.5 . . ?
C47 C49 H49C 109.5 . . ?
H49A C49 H49B 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
O8 C50 Zr2 55.12(13) . . ?
O8 C50 N8 115.3(3) . . ?
O8 C50 C51 117.4(3) . . ?
N8 C50 Zr2 60.90(16) . . ?
N8 C50 C51 127.3(3) . . ?
C51 C50 Zr2 167.4(2) . . ?
C50 C51 H51 109.3 . . ?
C50 C51 C52 108.6(3) . . ?
C50 C51 C53 110.0(3) . . ?
C52 C51 H51 109.3 . . ?
C53 C51 H51 109.3 . . ?
C53 C51 C52 110.3(3) . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C51 C53 H53A 109.5 . . ?
C51 C53 H53B 109.5 . . ?
C51 C53 H53C 109.5 . . ?
H53A C53 H53B 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
N8 C54 H54 108.4 . . ?
N8 C54 C55 110.4(3) . . ?
N8 C54 C56 110.5(3) . . ?
C55 C54 H54 108.4 . . ?
C56 C54 H54 108.4 . . ?
C56 C54 C55 110.7(3) . . ?
C54 C55 H55A 109.5 . . ?
C54 C55 H55B 109.5 . . ?
C54 C55 H55C 109.5 . . ?
H55A C55 H55B 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C54 C56 H56A 109.5 . . ?
C54 C56 H56B 109.5 . . ?
C54 C56 H56C 109.5 . . ?
H56A C56 H56B 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Zr1 O1 C1 N1 4.2(3) . . . . ?
Zr1 O1 C1 C2 -176.2(2) . . . . ?
Zr1 O2 C8 N2 0.0(3) . . . . ?
Zr1 O2 C8 C9 178.9(2) . . . . ?
Zr1 O3 C15 N3 -8.6(3) . . . . ?
Zr1 O3 C15 C16 166.7(2) . . . . ?
Zr1 O4 C22 N4 -4.8(3) . . . . ?
Zr1 O4 C22 C23 170.8(3) . . . . ?
Zr1 N1 C1 O1 -4.0(3) . . . . ?
Zr1 N1 C1 C2 176.4(3) . . . . ?
Zr1 N1 C5 C6 68.8(4) . . . . ?
Zr1 N1 C5 C7 -53.8(4) . . . . ?
Zr1 N2 C8 O2 0.0(3) . . . . ?
Zr1 N2 C8 C9 -178.8(3) . . . . ?
Zr1 N2 C12 C13 67.5(4) . . . . ?
Zr1 N2 C12 C14 -55.8(4) . . . . ?
Zr1 N3 C15 O3 8.2(3) . . . . ?
Zr1 N3 C15 C16 -166.6(2) . . . . ?
Zr1 N3 C19 C20 -87.9(4) . . . . ?
Zr1 N3 C19 C21 34.0(5) . . . . ?
Zr1 N4 C22 O4 4.6(3) . . . . ?
Zr1 N4 C22 C23 -170.6(3) . . . . ?
Zr1 N4 C26 C27 -100.9(4) . . . . ?
Zr1 N4 C26 C28 21.2(5) . . . . ?
Zr1 C15 C16 C17 83.1(10) . . . . ?
Zr1 C15 C16 C18 -38.3(12) . . . . ?
Zr1 C22 C23 C24 92.4(14) . . . . ?
Zr1 C22 C23 C25 -30.8(15) . . . . ?
O1 C1 C2 C3 23.4(4) . . . . ?
O1 C1 C2 C4 -99.6(4) . . . . ?
O2 C8 C9 C10 -109.6(3) . . . . ?
O2 C8 C9 C11 12.8(4) . . . . ?
O3 C15 C16 C17 26.3(3) . . . . ?
O3 C15 C16 C18 -95.0(3) . . . . ?
O4 C22 C23 C24 43.6(4) . . . . ?
O4 C22 C23 C25 -79.7(4) . . . . ?
N1 C1 C2 C3 -157.1(3) . . . . ?
N1 C1 C2 C4 80.0(4) . . . . ?
N2 C8 C9 C10 69.1(4) . . . . ?
N2 C8 C9 C11 -168.5(3) . . . . ?
N3 C15 C16 C17 -159.0(3) . . . . ?
N3 C15 C16 C18 79.7(4) . . . . ?
N4 C22 C23 C24 -141.4(3) . . . . ?
N4 C22 C23 C25 95.4(4) . . . . ?
C1 N1 C5 C6 -120.3(3) . . . . ?
C1 N1 C5 C7 117.1(3) . . . . ?
C5 N1 C1 Zr1 -174.7(3) . . . . ?
C5 N1 C1 O1 -178.7(3) . . . . ?
C5 N1 C1 C2 1.8(5) . . . . ?
C8 N2 C12 C13 -117.3(3) . . . . ?
C8 N2 C12 C14 119.4(3) . . . . ?
C12 N2 C8 Zr1 -177.2(3) . . . . ?
C12 N2 C8 O2 -177.2(2) . . . . ?
C12 N2 C8 C9 4.0(5) . . . . ?
C15 N3 C19 C20 98.2(4) . . . . ?
C15 N3 C19 C21 -139.9(3) . . . . ?
C19 N3 C15 Zr1 176.4(3) . . . . ?
C19 N3 C15 O3 -175.4(2) . . . . ?
C19 N3 C15 C16 9.8(5) . . . . ?
C22 N4 C26 C27 81.3(4) . . . . ?
C22 N4 C26 C28 -156.6(3) . . . . ?
C26 N4 C22 Zr1 178.8(3) . . . . ?
C26 N4 C22 O4 -176.7(3) . . . . ?
C26 N4 C22 C23 8.1(5) . . . . ?
Zr2 O5 C29 N5 -0.9(3) . . . . ?
Zr2 O5 C29 C30 177.5(2) . . . . ?
Zr2 O6 C36 N6 -4.3(3) . . . . ?
Zr2 O6 C36 C37 176.9(2) . . . . ?
Zr2 O7 C43 N7 6.5(3) . . . . ?
Zr2 O7 C43 C44 -169.5(2) . . . . ?
Zr2 O8 C50 N8 9.5(3) . . . . ?
Zr2 O8 C50 C51 -168.1(2) . . . . ?
Zr2 N5 C29 O5 0.9(3) . . . . ?
Zr2 N5 C29 C30 -177.4(3) . . . . ?
Zr2 N5 C33 C34 23.5(5) . . . . ?
Zr2 N5 C33 C35 -99.7(4) . . . . ?
Zr2 N6 C36 O6 4.2(3) . . . . ?
Zr2 N6 C36 C37 -177.2(3) . . . . ?
Zr2 N6 C40 C41 55.6(4) . . . . ?
Zr2 N6 C40 C42 -66.7(4) . . . . ?
Zr2 N7 C43 O7 -6.1(3) . . . . ?
Zr2 N7 C43 C44 169.4(3) . . . . ?
Zr2 N7 C47 C48 96.5(4) . . . . ?
Zr2 N7 C47 C49 -25.1(5) . . . . ?
Zr2 N8 C50 O8 -8.9(3) . . . . ?
Zr2 N8 C50 C51 168.5(3) . . . . ?
Zr2 N8 C54 C55 120.6(3) . . . . ?
Zr2 N8 C54 C56 -2.3(5) . . . . ?
Zr2 C43 C44 C45 40.8(12) . . . . ?
Zr2 C43 C44 C46 -81.9(11) . . . . ?
Zr2 C50 C51 C52 7.6(12) . . . . ?
Zr2 C50 C51 C53 -113.2(10) . . . . ?
O5 C29 C30 C31 -64.7(4) . . . . ?
O5 C29 C30 C32 58.6(4) . . . . ?
O6 C36 C37 C38 -22.3(4) . . . . ?
O6 C36 C37 C39 100.8(3) . . . . ?
O7 C43 C44 C45 90.8(3) . . . . ?
O7 C43 C44 C46 -31.9(4) . . . . ?
O8 C50 C51 C52 58.1(4) . . . . ?
O8 C50 C51 C53 -62.7(4) . . . . ?
N5 C29 C30 C31 113.6(4) . . . . ?
N5 C29 C30 C32 -123.1(4) . . . . ?
N6 C36 C37 C38 159.1(3) . . . . ?
N6 C36 C37 C39 -77.8(4) . . . . ?
N7 C43 C44 C45 -84.7(4) . . . . ?
N7 C43 C44 C46 152.6(3) . . . . ?
N8 C50 C51 C52 -119.2(4) . . . . ?
N8 C50 C51 C53 120.0(4) . . . . ?
C29 N5 C33 C34 -156.3(3) . . . . ?
C29 N5 C33 C35 80.5(4) . . . . ?
C33 N5 C29 Zr2 179.9(3) . . . . ?
C33 N5 C29 O5 -179.2(3) . . . . ?
C33 N5 C29 C30 2.5(5) . . . . ?
C36 N6 C40 C41 -115.4(3) . . . . ?
C36 N6 C40 C42 122.4(3) . . . . ?
C40 N6 C36 Zr2 174.8(3) . . . . ?
C40 N6 C36 O6 178.9(3) . . . . ?
C40 N6 C36 C37 -2.5(5) . . . . ?
C43 N7 C47 C48 -81.0(4) . . . . ?
C43 N7 C47 C49 157.5(3) . . . . ?
C47 N7 C43 Zr2 178.6(3) . . . . ?
C47 N7 C43 O7 172.5(2) . . . . ?
C47 N7 C43 C44 -12.0(5) . . . . ?
C50 N8 C54 C55 -73.8(4) . . . . ?
C50 N8 C54 C56 163.4(3) . . . . ?
C54 N8 C50 Zr2 -172.0(3) . . . . ?
C54 N8 C50 O8 179.0(3) . . . . ?
C54 N8 C50 C51 -3.6(5) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_k14msh32
_database_code_depnum_ccdc_archive 'CCDC 1498671'
_audit_update_record             
;
2016-08-10 deposited with the CCDC.
2016-10-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H64 N4 O4 Zr'
_chemical_formula_sum            'C32 H64 N4 O4 Zr'
_chemical_formula_weight         660.09

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_H-M_alt        'C 2'
_space_group_name_Hall           'C 2y'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'

_cell_length_a                   18.3482(7)
_cell_length_b                   11.9920(5)
_cell_length_c                   8.9002(4)
_cell_angle_alpha                90
_cell_angle_beta                 112.527(2)
_cell_angle_gamma                90
_cell_volume                     1808.90(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    107564
_cell_measurement_theta_min      5.097
_cell_measurement_theta_max      27.485

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_F_000             712
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    0.341
_shelx_estimated_absorpt_T_min   0.920
_shelx_estimated_absorpt_T_max   0.951
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.818
_exptl_absorpt_correction_T_max  0.952
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       '287 2.0 degree images with φ and \v scans'
_diffrn_reflns_number            13994
_diffrn_reflns_av_unetI/netI     0.0480
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.398
_diffrn_reflns_theta_max         27.090
_diffrn_reflns_theta_full        25.240
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3951
_reflns_number_gt                3833
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.909
_reflns_Friedel_fraction_max     0.998
_reflns_Friedel_fraction_full    0.999

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_reduction        
;
 DENZO-SCALEPACK Z. Otwinowski and W. Minor, " 
 Processing of X-ray Diffraction Data Collected in Oscillation Mode ", 
 Methods in Enzymology, Volume 276: Macromolecular Crystallography, 
 part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press.
;
_computing_structure_solution    
; 
 SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , 
 Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. 
 (1999) J. Appl. Cryst. 32, 115-119
;
_computing_structure_refinement  
;
SHELXL-2014/6 (Sheldrick, 2014)
Sheldrick GM (2008) Acta Crystallogr A64:112--122 and 
 C. B. Hübschle, G. M. Sheldrick and B. Dittrich
 ShelXle: a Qt graphical user interface for SHELXL
 J. Appl. Cryst., 44, (2011) 1281-1284.
;
_computing_molecular_graphics    
'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565'

_computing_publication_material  
;
 'WinGX publication routines, Farrugia, 
 L. J., J. Appl. Crystallogr., 1999, 32, 837-838
;
_refine_special_details          
;
 Refined as a 2-component perfect inversion twin in the ratio 1:1.
 The centre atom of the complex is sitting on a 2 fold axis which 
 leads to complete disorder of the entire complex because 
 the ligand is not symmetrical. 
 The asymmetric unit shows the full complex but with 50% occupation.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0145P)²+1.3590P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.47(9)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3951
_refine_ls_number_parameters     342
_refine_ls_number_restraints     80
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0318
_refine_ls_wR_factor_ref         0.0643
_refine_ls_wR_factor_gt          0.0631
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.075
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr Zr 0.5000 0.9792(2) 0.0000 0.02099(12) Uani 1 2 d S T P . .
N1 N 0.5144(7) 0.7882(9) 0.024(2) 0.019(3) Uiso 0.5 1 d . . P A -1
N2 N 0.5079(9) 1.1724(9) 0.0348(15) 0.012(3) Uiso 0.5 1 d . . P A -1
N3 N 0.3692(5) 0.977(3) -0.0358(9) 0.0197(19) Uani 0.5 1 d D U P A -1
N4 N 0.6158(5) 0.979(3) -0.0594(10) 0.024(2) Uani 0.5 1 d D U P A -1
O1 O 0.4618(8) 0.8610(9) -0.2080(14) 0.020(3) Uani 0.5 1 d . . P A -1
O2 O 0.4553(7) 1.0967(10) -0.2179(14) 0.020(3) Uani 0.5 1 d . U P A -1
O3 O 0.46763(17) 0.9806(18) 0.2009(3) 0.0201(7) Uani 0.5 1 d . . P A -1
O4 O 0.61693(18) 0.9765(16) 0.1871(4) 0.0201(8) Uani 0.5 1 d . . P A -1
C1 C 0.4814(11) 0.7696(14) -0.119(2) 0.019(3) Uani 0.5 1 d . U P A -1
C2 C 0.4724(11) 1.1881(16) -0.131(2) 0.021(4) Uani 0.5 1 d . . P A -1
C3 C 0.3919(7) 0.984(2) 0.1196(10) 0.018(2) Uani 0.5 1 d D U P A -1
C4 C 0.6577(5) 0.981(3) 0.0961(12) 0.0220(19) Uani 0.5 1 d . . P A -1
C11 C 0.4640(11) 0.6606(16) -0.213(2) 0.029(4) Uani 0.5 1 d . U P A -1
H11 H 0.4856 0.5971 -0.1361 0.035 Uiso 0.5 1 calc R U P A -1
C12 C 0.3676(15) 0.6509(18) -0.296(3) 0.063(7) Uani 0.5 1 d . . P A -1
H12A H 0.3460 0.6547 -0.2113 0.095 Uiso 0.5 1 calc R U P A -1
H12B H 0.3463 0.7124 -0.3732 0.095 Uiso 0.5 1 calc R U P A -1
H12C H 0.3527 0.5797 -0.3541 0.095 Uiso 0.5 1 calc R U P A -1
C13 C 0.4948(16) 0.6547(13) -0.341(3) 0.051(6) Uani 0.5 1 d . . P A -1
H13A H 0.4813 0.5824 -0.3962 0.077 Uiso 0.5 1 calc R U P A -1
H13B H 0.4716 0.7146 -0.4201 0.077 Uiso 0.5 1 calc R U P A -1
H13C H 0.5523 0.6633 -0.2937 0.077 Uiso 0.5 1 calc R U P A -1
C14 C 0.5435(10) 0.7019(14) 0.161(2) 0.023(3) Uani 0.5 1 d . U P A -1
C15 C 0.4696(14) 0.6305(18) 0.154(2) 0.045(5) Uani 0.5 1 d . . P A -1
H15A H 0.4289 0.6803 0.1617 0.067 Uiso 0.5 1 calc R U P A -1
H15B H 0.4485 0.5895 0.0508 0.067 Uiso 0.5 1 calc R U P A -1
H15C H 0.4858 0.5776 0.2446 0.067 Uiso 0.5 1 calc R U P A -1
C16 C 0.6049(12) 0.6286(17) 0.149(2) 0.035(4) Uani 0.5 1 d . . P A -1
H16A H 0.5852 0.5911 0.0433 0.053 Uiso 0.5 1 calc R U P A -1
H16B H 0.6516 0.6729 0.1604 0.053 Uiso 0.5 1 calc R U P A -1
H16C H 0.6191 0.5727 0.2361 0.053 Uiso 0.5 1 calc R U P A -1
C17 C 0.5732(12) 0.7609(16) 0.325(2) 0.033(5) Uani 0.5 1 d . . P A -1
H17A H 0.5317 0.8097 0.3313 0.049 Uiso 0.5 1 calc R U P A -1
H17B H 0.5873 0.7054 0.4121 0.049 Uiso 0.5 1 calc R U P A -1
H17C H 0.6198 0.8056 0.3364 0.049 Uiso 0.5 1 calc R U P A -1
C21 C 0.4488(10) 1.2954(14) -0.226(2) 0.027(4) Uani 0.5 1 d . U P A -1
H21 H 0.4659 1.3587 -0.1464 0.033 Uiso 0.5 1 calc R U P A -1
C22 C 0.3663(12) 1.3060(17) -0.316(3) 0.050(5) Uani 0.5 1 d . . P A -1
H22A H 0.3555 1.3774 -0.3739 0.075 Uiso 0.5 1 calc R U P A -1
H22B H 0.3482 1.2448 -0.3945 0.075 Uiso 0.5 1 calc R U P A -1
H22C H 0.3384 1.3031 -0.2416 0.075 Uiso 0.5 1 calc R U P A -1
C23 C 0.4990(17) 1.3022(18) -0.343(3) 0.062(7) Uani 0.5 1 d . . P A -1
H23A H 0.5554 1.2946 -0.2763 0.093 Uiso 0.5 1 calc R U P A -1
H23B H 0.4823 1.2418 -0.4229 0.093 Uiso 0.5 1 calc R U P A -1
H23C H 0.4893 1.3742 -0.3989 0.093 Uiso 0.5 1 calc R U P A -1
C24 C 0.5326(10) 1.2619(16) 0.155(2) 0.021(3) Uiso 0.5 1 d . . P A -1
C25 C 0.5706(11) 1.2029(17) 0.322(2) 0.029(4) Uiso 0.5 1 d . . P A -1
H25A H 0.5885 1.2589 0.4089 0.043 Uiso 0.5 1 calc R U P A -1
H25B H 0.5315 1.1542 0.3392 0.043 Uiso 0.5 1 calc R U P A -1
H25C H 0.6157 1.1582 0.3244 0.043 Uiso 0.5 1 calc R U P A -1
C26 C 0.6051(11) 1.3269(18) 0.130(2) 0.037(4) Uani 0.5 1 d . . P A -1
H26A H 0.6234 1.3879 0.2089 0.056 Uiso 0.5 1 calc R U P A -1
H26B H 0.6485 1.2747 0.1466 0.056 Uiso 0.5 1 calc R U P A -1
H26C H 0.5869 1.3573 0.0195 0.056 Uiso 0.5 1 calc R U P A -1
C27 C 0.4697(9) 1.3380(16) 0.159(2) 0.030(4) Uani 0.5 1 d . . P A -1
H27A H 0.4927 1.3944 0.2439 0.045 Uiso 0.5 1 calc R U P A -1
H27B H 0.4447 1.3747 0.0534 0.045 Uiso 0.5 1 calc R U P A -1
H27C H 0.4300 1.2950 0.1833 0.045 Uiso 0.5 1 calc R U P A -1
C31 C 0.3413(5) 0.9839(17) 0.2201(11) 0.024(2) Uiso 0.5 1 d D . P A -1
H31 H 0.2845 0.9860 0.1452 0.028 Uiso 0.5 1 calc R U P A -1
C32 C 0.3603(10) 1.0874(14) 0.325(2) 0.032(4) Uani 0.5 1 d D . P A -1
H32A H 0.3281 1.0887 0.3907 0.048 Uiso 0.5 1 calc R U P A -1
H32B H 0.4163 1.0870 0.3962 0.048 Uiso 0.5 1 calc R U P A -1
H32C H 0.3488 1.1536 0.2549 0.048 Uiso 0.5 1 calc R U P A -1
C33 C 0.3559(13) 0.8785(17) 0.332(2) 0.042(5) Uani 0.5 1 d D . P A -1
H33A H 0.3436 0.8110 0.2646 0.063 Uiso 0.5 1 calc R U P A -1
H33B H 0.4112 0.8765 0.4073 0.063 Uiso 0.5 1 calc R U P A -1
H33C H 0.3218 0.8819 0.3940 0.063 Uiso 0.5 1 calc R U P A -1
C34 C 0.2869(5) 0.978(2) -0.1573(9) 0.029(2) Uani 0.5 1 d D . P A -1
C35 C 0.2907(3) 0.982(3) -0.3264(6) 0.0413(19) Uani 0.5 1 d D . P A -1
H35A H 0.2370 0.9827 -0.4098 0.062 Uiso 0.5 1 calc R U P A -1
H35B H 0.3189 1.0489 -0.3361 0.062 Uiso 0.5 1 calc R U P A -1
H35C H 0.3186 0.9155 -0.3413 0.062 Uiso 0.5 1 calc R U P A -1
C36 C 0.2393(11) 0.8717(19) -0.155(2) 0.045(4) Uani 0.5 1 d D U P A -1
H36A H 0.1857 0.8781 -0.2382 0.067 Uiso 0.5 1 calc R U P A -1
H36B H 0.2653 0.8063 -0.1786 0.067 Uiso 0.5 1 calc R U P A -1
H36C H 0.2367 0.8633 -0.0479 0.067 Uiso 0.5 1 calc R U P A -1
C37 C 0.2480(13) 1.085(2) -0.130(2) 0.061(5) Uani 0.5 1 d D U P A -1
H37A H 0.1934 1.0883 -0.2094 0.092 Uiso 0.5 1 calc R U P A -1
H37B H 0.2486 1.0851 -0.0199 0.092 Uiso 0.5 1 calc R U P A -1
H37C H 0.2772 1.1498 -0.1450 0.092 Uiso 0.5 1 calc R U P A -1
C41 C 0.7471(4) 0.9699(17) 0.1841(10) 0.028(2) Uani 0.5 1 d D U P A -1
H41 H 0.7705 0.9431 0.1061 0.033 Uiso 0.5 1 calc R U P A -1
C42 C 0.7714(4) 0.8908(7) 0.3322(11) 0.0390(19) Uani 0.5 1 d D . P A -1
H42A H 0.8291 0.8869 0.3834 0.058 Uiso 0.5 1 calc R U P A -1
H42B H 0.7505 0.9190 0.4109 0.058 Uiso 0.5 1 calc R U P A -1
H42C H 0.7501 0.8161 0.2962 0.058 Uiso 0.5 1 calc R U P A -1
C43 C 0.7756(5) 1.0887(9) 0.2390(13) 0.039(2) Uani 0.5 1 d D . P A -1
H43A H 0.8331 1.0885 0.2971 0.059 Uiso 0.5 1 calc R U P A -1
H43B H 0.7614 1.1374 0.1436 0.059 Uiso 0.5 1 calc R U P A -1
H43C H 0.7506 1.1162 0.3113 0.059 Uiso 0.5 1 calc R U P A -1
C44 C 0.6450(5) 0.9612(13) -0.1957(10) 0.032(4) Uani 0.5 1 d D . P A -1
C45 C 0.7039(5) 1.0502(8) -0.1875(10) 0.042(2) Uani 0.5 1 d D . P A -1
H45A H 0.7230 1.0390 -0.2754 0.062 Uiso 0.5 1 calc R U P A -1
H45B H 0.6788 1.1236 -0.1995 0.062 Uiso 0.5 1 calc R U P A -1
H45C H 0.7485 1.0462 -0.0824 0.062 Uiso 0.5 1 calc R U P A -1
C46 C 0.6814(5) 0.8433(8) -0.1903(11) 0.0384(19) Uani 0.5 1 d D . P A -1
H46A H 0.6422 0.7863 -0.1958 0.058 Uiso 0.5 1 calc R U P A -1
H46B H 0.6973 0.8345 -0.2830 0.058 Uiso 0.5 1 calc R U P A -1
H46C H 0.7277 0.8347 -0.0887 0.058 Uiso 0.5 1 calc R U P A -1
C47 C 0.5742(3) 0.982(2) -0.3549(6) 0.0319(16) Uani 0.5 1 d D . P A -1
H47A H 0.5333 0.9266 -0.3676 0.048 Uiso 0.5 1 calc R U P A -1
H47B H 0.5530 1.0571 -0.3522 0.048 Uiso 0.5 1 calc R U P A -1
H47C H 0.5911 0.9773 -0.4467 0.048 Uiso 0.5 1 calc R U P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr O3 2.089(3) . ?
Zr O4 2.154(3) . ?
Zr O1 2.221(12) . ?
Zr O2 2.280(12) . ?
Zr N3 2.298(8) . ?
Zr N1 2.307(11) . ?
Zr N2 2.334(11) . ?
Zr N4 2.378(9) . ?
Zr C3 2.585(11) . ?
Zr C4 2.685(9) . ?
Zr C1 2.696(19) . ?
Zr C2 2.73(2) . ?
N1 C1 1.20(3) . ?
N1 C14 1.53(2) . ?
N2 C2 1.38(2) . ?
N2 C24 1.46(2) . ?
N3 C3 1.285(9) . ?
N3 C34 1.482(8) . ?
N4 C4 1.300(9) . ?
N4 C44 1.518(11) . ?
O1 C1 1.32(2) . ?
O2 C2 1.31(2) . ?
O3 C3 1.298(12) . ?
O4 C4 1.298(10) . ?
C1 C11 1.52(3) . ?
C2 C21 1.51(3) . ?
C3 C31 1.517(12) . ?
C4 C41 1.529(10) . ?
C11 C13 1.45(3) . ?
C11 C12 1.64(3) . ?
C11 H11 1.0000 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C16 1.46(3) . ?
C14 C17 1.52(3) . ?
C14 C15 1.58(3) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C21 C22 1.42(3) . ?
C21 C23 1.64(3) . ?
C21 H21 1.0000 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C27 1.48(2) . ?
C24 C25 1.55(3) . ?
C24 C26 1.63(2) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C31 C32 1.510(18) . ?
C31 C33 1.567(18) . ?
C31 H31 1.0000 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C37 1.53(2) . ?
C34 C35 1.533(8) . ?
C34 C36 1.550(19) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C41 C43 1.532(19) . ?
C41 C42 1.544(15) . ?
C41 H41 1.0000 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 C45 1.501(13) . ?
C44 C47 1.533(10) . ?
C44 C46 1.557(15) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Zr O4 82.18(11) . . ?
O3 Zr O1 128.0(6) . . ?
O4 Zr O1 122.5(5) . . ?
O3 Zr O2 126.5(5) . . ?
O4 Zr O2 126.5(5) . . ?
O1 Zr O2 77.87(13) . . ?
O3 Zr N3 59.6(2) . . ?
O4 Zr N3 141.7(2) . . ?
O1 Zr N3 84.1(6) . . ?
O2 Zr N3 82.8(6) . . ?
O3 Zr N1 89.4(7) . . ?
O4 Zr N1 82.5(6) . . ?
O1 Zr N1 55.3(5) . . ?
O2 Zr N1 133.0(5) . . ?
N3 Zr N1 94.4(9) . . ?
O3 Zr N2 84.4(6) . . ?
O4 Zr N2 85.4(6) . . ?
O1 Zr N2 136.7(4) . . ?
O2 Zr N2 58.9(4) . . ?
N3 Zr N2 92.3(9) . . ?
N1 Zr N2 167.03(16) . . ?
O3 Zr N4 139.6(2) . . ?
O4 Zr N4 57.4(2) . . ?
O1 Zr N4 80.7(6) . . ?
O2 Zr N4 82.7(6) . . ?
N3 Zr N4 160.8(2) . . ?
N1 Zr N4 86.5(8) . . ?
N2 Zr N4 90.8(8) . . ?
O3 Zr C3 29.9(2) . . ?
O4 Zr C3 112.1(2) . . ?
O1 Zr C3 108.1(6) . . ?
O2 Zr C3 104.7(5) . . ?
N3 Zr C3 29.8(2) . . ?
N1 Zr C3 93.7(7) . . ?
N2 Zr C3 86.6(7) . . ?
N4 Zr C3 169.4(3) . . ?
O3 Zr C4 110.6(2) . . ?
O4 Zr C4 28.5(2) . . ?
O1 Zr C4 103.2(6) . . ?
O2 Zr C4 105.0(6) . . ?
N3 Zr C4 170.2(3) . . ?
N1 Zr C4 84.7(8) . . ?
N2 Zr C4 86.8(8) . . ?
N4 Zr C4 29.0(2) . . ?
C3 Zr C4 140.5(3) . . ?
O3 Zr C1 107.9(7) . . ?
O4 Zr C1 103.2(6) . . ?
O1 Zr C1 29.1(5) . . ?
O2 Zr C1 107.0(5) . . ?
N3 Zr C1 87.9(9) . . ?
N1 Zr C1 26.2(6) . . ?
N2 Zr C1 165.7(5) . . ?
N4 Zr C1 84.4(8) . . ?
C3 Zr C1 100.4(7) . . ?
C4 Zr C1 95.3(8) . . ?
O3 Zr C2 107.0(7) . . ?
O4 Zr C2 108.1(6) . . ?
O1 Zr C2 106.4(5) . . ?
O2 Zr C2 28.6(5) . . ?
N3 Zr C2 86.6(9) . . ?
N1 Zr C2 161.3(6) . . ?
N2 Zr C2 30.4(5) . . ?
N4 Zr C2 86.6(8) . . ?
C3 Zr C2 96.2(7) . . ?
C4 Zr C2 97.4(8) . . ?
C1 Zr C2 135.5(2) . . ?
C1 N1 C14 126.8(14) . . ?
C1 N1 Zr 95.4(11) . . ?
C14 N1 Zr 137.4(11) . . ?
C2 N2 C24 124.8(14) . . ?
C2 N2 Zr 90.8(10) . . ?
C24 N2 Zr 144.4(10) . . ?
C3 N3 C34 127.2(10) . . ?
C3 N3 Zr 87.6(8) . . ?
C34 N3 Zr 144.9(6) . . ?
C4 N4 C44 127.4(9) . . ?
C4 N4 Zr 88.7(6) . . ?
C44 N4 Zr 142.8(7) . . ?
C1 O1 Zr 95.8(11) . . ?
C2 O2 Zr 95.1(11) . . ?
C3 O3 Zr 96.7(4) . . ?
C4 O4 Zr 99.1(5) . . ?
N1 C1 O1 113.2(16) . . ?
N1 C1 C11 131.2(17) . . ?
O1 C1 C11 115.4(17) . . ?
N1 C1 Zr 58.4(9) . . ?
O1 C1 Zr 55.0(8) . . ?
C11 C1 Zr 170.4(13) . . ?
O2 C2 N2 115.2(16) . . ?
O2 C2 C21 115.7(16) . . ?
N2 C2 C21 129.1(17) . . ?
O2 C2 Zr 56.4(9) . . ?
N2 C2 Zr 58.8(8) . . ?
C21 C2 Zr 171.6(13) . . ?
N3 C3 O3 115.8(10) . . ?
N3 C3 C31 127.9(12) . . ?
O3 C3 C31 115.9(7) . . ?
N3 C3 Zr 62.6(6) . . ?
O3 C3 Zr 53.4(4) . . ?
C31 C3 Zr 169.2(7) . . ?
O4 C4 N4 114.6(8) . . ?
O4 C4 C41 116.0(8) . . ?
N4 C4 C41 128.6(9) . . ?
O4 C4 Zr 52.4(3) . . ?
N4 C4 Zr 62.3(5) . . ?
C41 C4 Zr 167.4(11) . . ?
C13 C11 C1 114.5(15) . . ?
C13 C11 C12 108.6(18) . . ?
C1 C11 C12 105.7(16) . . ?
C13 C11 H11 109.3 . . ?
C1 C11 H11 109.3 . . ?
C12 C11 H11 109.3 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C16 C14 C17 110.1(16) . . ?
C16 C14 N1 113.1(14) . . ?
C17 C14 N1 109.7(14) . . ?
C16 C14 C15 110.1(16) . . ?
C17 C14 C15 106.0(14) . . ?
N1 C14 C15 107.6(14) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C22 C21 C2 114.1(17) . . ?
C22 C21 C23 111.8(19) . . ?
C2 C21 C23 106.7(15) . . ?
C22 C21 H21 108.0 . . ?
C2 C21 H21 108.0 . . ?
C23 C21 H21 108.0 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N2 C24 C27 116.4(15) . . ?
N2 C24 C25 105.5(15) . . ?
C27 C24 C25 108.9(15) . . ?
N2 C24 C26 107.0(14) . . ?
C27 C24 C26 113.2(16) . . ?
C25 C24 C26 105.0(14) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C24 C27 H27A 109.5 . . ?
C24 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C24 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C32 C31 C3 108.2(15) . . ?
C32 C31 C33 109.2(7) . . ?
C3 C31 C33 112.5(16) . . ?
C32 C31 H31 109.0 . . ?
C3 C31 H31 109.0 . . ?
C33 C31 H31 109.0 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
N3 C34 C37 107.6(18) . . ?
N3 C34 C35 107.5(6) . . ?
C37 C34 C35 109.2(17) . . ?
N3 C34 C36 113.7(18) . . ?
C37 C34 C36 112.9(8) . . ?
C35 C34 C36 105.8(16) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C4 C41 C43 104.4(17) . . ?
C4 C41 C42 113.2(12) . . ?
C43 C41 C42 110.4(9) . . ?
C4 C41 H41 109.6 . . ?
C43 C41 H41 109.6 . . ?
C42 C41 H41 109.6 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C45 C44 N4 109.2(12) . . ?
C45 C44 C47 105.4(12) . . ?
N4 C44 C47 106.3(7) . . ?
C45 C44 C46 110.6(8) . . ?
N4 C44 C46 112.5(14) . . ?
C47 C44 C46 112.4(13) . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C44 C46 H46A 109.5 . . ?
C44 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C44 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C44 C47 H47A 109.5 . . ?
C44 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C44 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C14 N1 C1 O1 178.7(13) . . . . ?
Zr N1 C1 O1 5.1(16) . . . . ?
C14 N1 C1 C11 -7(3) . . . . ?
Zr N1 C1 C11 179.8(18) . . . . ?
C14 N1 C1 Zr 173.6(16) . . . . ?
Zr O1 C1 N1 -5.3(16) . . . . ?
Zr O1 C1 C11 179.1(13) . . . . ?
Zr O2 C2 N2 1.5(16) . . . . ?
Zr O2 C2 C21 -177.0(13) . . . . ?
C24 N2 C2 O2 179.6(14) . . . . ?
Zr N2 C2 O2 -1.5(16) . . . . ?
C24 N2 C2 C21 -2(3) . . . . ?
Zr N2 C2 C21 176.8(18) . . . . ?
C24 N2 C2 Zr -178.9(17) . . . . ?
C34 N3 C3 O3 180(3) . . . . ?
Zr N3 C3 O3 -5(3) . . . . ?
C34 N3 C3 C31 7(6) . . . . ?
Zr N3 C3 C31 -177(3) . . . . ?
C34 N3 C3 Zr -175(4) . . . . ?
Zr O3 C3 N3 5(3) . . . . ?
Zr O3 C3 C31 178.7(19) . . . . ?
Zr O4 C4 N4 -4(3) . . . . ?
Zr O4 C4 C41 -174(2) . . . . ?
C44 N4 C4 O4 -167(2) . . . . ?
Zr N4 C4 O4 3(3) . . . . ?
C44 N4 C4 C41 2(5) . . . . ?
Zr N4 C4 C41 173(3) . . . . ?
C44 N4 C4 Zr -171(3) . . . . ?
N1 C1 C11 C13 -123(2) . . . . ?
O1 C1 C11 C13 52(2) . . . . ?
N1 C1 C11 C12 117(2) . . . . ?
O1 C1 C11 C12 -68(2) . . . . ?
C1 N1 C14 C16 63(2) . . . . ?
Zr N1 C14 C16 -126.0(14) . . . . ?
C1 N1 C14 C17 -173.1(16) . . . . ?
Zr N1 C14 C17 -3(2) . . . . ?
C1 N1 C14 C15 -58(2) . . . . ?
Zr N1 C14 C15 112.3(14) . . . . ?
O2 C2 C21 C22 61(2) . . . . ?
N2 C2 C21 C22 -117(2) . . . . ?
O2 C2 C21 C23 -63(2) . . . . ?
N2 C2 C21 C23 119(2) . . . . ?
C2 N2 C24 C27 60(2) . . . . ?
Zr N2 C24 C27 -117.8(19) . . . . ?
C2 N2 C24 C25 -178.8(15) . . . . ?
Zr N2 C24 C25 3(2) . . . . ?
C2 N2 C24 C26 -67(2) . . . . ?
Zr N2 C24 C26 114.6(18) . . . . ?
N3 C3 C31 C32 -125(3) . . . . ?
O3 C3 C31 C32 62(3) . . . . ?
Zr C3 C31 C32 68(11) . . . . ?
N3 C3 C31 C33 114(3) . . . . ?
O3 C3 C31 C33 -58(3) . . . . ?
Zr C3 C31 C33 -53(11) . . . . ?
C3 N3 C34 C37 55(4) . . . . ?
Zr N3 C34 C37 -117(3) . . . . ?
C3 N3 C34 C35 173(3) . . . . ?
Zr N3 C34 C35 1(5) . . . . ?
C3 N3 C34 C36 -70(4) . . . . ?
Zr N3 C34 C36 118(3) . . . . ?
O4 C4 C41 C43 -86(3) . . . . ?
N4 C4 C41 C43 105(3) . . . . ?
Zr C4 C41 C43 -107(9) . . . . ?
O4 C4 C41 C42 34(3) . . . . ?
N4 C4 C41 C42 -135(3) . . . . ?
Zr C4 C41 C42 13(9) . . . . ?
C4 N4 C44 C45 -59(3) . . . . ?
Zr N4 C44 C45 137(3) . . . . ?
C4 N4 C44 C47 -172(3) . . . . ?
Zr N4 C44 C47 23(3) . . . . ?
C4 N4 C44 C46 64(3) . . . . ?
Zr N4 C44 C46 -100(3) . . . . ?

_refine_diff_density_max         0.248
_refine_diff_density_min         -0.701
_refine_diff_density_rms         0.055

