 
data_cmmm_a_sq
 
_audit_creation_method            'SHELXL-2019/2'
_shelx_SHELXL_version_number      '2019/2'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C188 H126 Fe2 N12 O32 Zr6' 
_chemical_formula_weight          3724.02

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0030   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'   0.0059   0.0032
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0105   0.0059
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Fe'  'Fe'   0.3456   0.8265
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Zr'  'Zr'  -3.5084   0.5477
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       orthorhombic
_space_group_IT_number            65
_space_group_name_H-M_alt         'C m m m'
_space_group_name_Hall            '-C 2 2'
 
_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, y, -z'
 'x, -y, -z'
 'x+1/2, y+1/2, z'
 '-x+1/2, -y+1/2, z'
 '-x+1/2, y+1/2, -z'
 'x+1/2, -y+1/2, -z'
 '-x, -y, -z'
 'x, y, -z'
 'x, -y, z'
 '-x, y, z'
 '-x+1/2, -y+1/2, -z'
 'x+1/2, y+1/2, -z'
 'x+1/2, -y+1/2, z'
 '-x+1/2, y+1/2, z'
 
_cell_length_a                    26.924(5)
_cell_length_b                    41.374(8)
_cell_length_c                    26.072(5)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      29043(10)
_cell_formula_units_Z             2
_cell_measurement_temperature     298(2)
_cell_measurement_reflns_used     314658
_cell_measurement_theta_min       1.777
_cell_measurement_theta_max       29.858
 
_exptl_crystal_description        'Rhombus'
_exptl_crystal_colour             'Reddish purple'
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     0.426          
_exptl_crystal_F_000              3772
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.200
_exptl_crystal_size_mid           0.150
_exptl_crystal_size_min           0.010
_exptl_absorpt_coefficient_mu     0.166
_exptl_absorpt_correction_type    'None'
_exptl_absorpt_correction_T_min   0.968
_exptl_absorpt_correction_T_max   0.998
_exptl_absorpt_process_details    ?
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       298(2)
_diffrn_radiation_wavelength      0.700
_diffrn_radiation_type            'synchrotron'
_diffrn_source                    'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             160348
_diffrn_reflns_av_unetI/netI      0.0370
_diffrn_reflns_av_R_equivalents   0.0822
_diffrn_reflns_limit_h_min        -38
_diffrn_reflns_limit_h_max        38
_diffrn_reflns_limit_k_min        -58
_diffrn_reflns_limit_k_max        58
_diffrn_reflns_limit_l_min        -37
_diffrn_reflns_limit_l_max        37
_diffrn_reflns_theta_min          1.777
_diffrn_reflns_theta_max          29.858
_diffrn_reflns_theta_full         24.835
_diffrn_measured_fraction_theta_max   0.997
_diffrn_measured_fraction_theta_full  0.996
_diffrn_reflns_Laue_measured_fraction_max    0.997
_diffrn_reflns_Laue_measured_fraction_full   0.996
_diffrn_reflns_point_group_measured_fraction_max   0.997
_diffrn_reflns_point_group_measured_fraction_full  0.996
_reflns_number_total              22997
_reflns_number_gt                 19264
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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      'Bruker APEX2'
_computing_cell_refinement      'Bruker SAINT'
_computing_data_reduction       'Bruker SAINT, SADABS and XPREP'
_computing_structure_solution   'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics   'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
_refine_special_details           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0936P)²+33.2995P] 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_number_reflns          22997
_refine_ls_number_parameters      318
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0643
_refine_ls_R_factor_gt            0.0564
_refine_ls_wR_factor_ref          0.1738
_refine_ls_wR_factor_gt           0.1659
_refine_ls_goodness_of_fit_ref    0.967
_refine_ls_restrained_S_all       0.967
_refine_ls_shift/su_max           0.005
_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
C1 C 0.42081(9) 0.44576(5) 0.87622(7) 0.0554(5) Uani 1 1 d . . . . .
C2 C 0.39982(11) 0.42520(6) 0.83414(7) 0.0691(7) Uani 1 1 d . . . . .
C3 C 0.42097(13) 0.42593(8) 0.78627(9) 0.0962(12) Uani 1 1 d . . . . .
H3 H 0.447064 0.440064 0.779686 0.115 Uiso 1 1 calc R U . . .
C4 C 0.40377(14) 0.40577(9) 0.74756(9) 0.1053(13) Uani 1 1 d . . . . .
H4 H 0.419824 0.405674 0.715983 0.126 Uiso 1 1 calc R U . . .
C5 C 0.36379(12) 0.38614(7) 0.75503(9) 0.0805(9) Uani 1 1 d . . . . .
C6 C 0.34370(16) 0.38516(10) 0.80313(11) 0.1312(18) Uani 1 1 d . . . . .
H6 H 0.317272 0.371270 0.809552 0.157 Uiso 1 1 calc R U . . .
C7 C 0.36173(16) 0.40440(10) 0.84277(10) 0.1250(17) Uani 1 1 d . . . . .
H7 H 0.347633 0.402998 0.875259 0.150 Uiso 1 1 calc R U . . .
C8 C 0.34532(11) 0.36455(7) 0.71302(9) 0.0774(8) Uani 1 1 d . . . . .
C9 C 0.37736(13) 0.34866(9) 0.68192(13) 0.1101(13) Uani 1 1 d . . . . .
H9 H 0.411332 0.351300 0.686799 0.132 Uiso 1 1 calc R U . . .
C10 C 0.36070(12) 0.32845(9) 0.64284(12) 0.0983(11) Uani 1 1 d . . . . .
H10 H 0.383773 0.317842 0.622315 0.118 Uiso 1 1 calc R U . . .
C11 C 0.31155(9) 0.32393(5) 0.63407(7) 0.0547(5) Uani 1 1 d . . . . .
C12 C 0.27936(13) 0.34060(10) 0.66450(14) 0.1151(14) Uani 1 1 d . . . . .
H12 H 0.245370 0.338519 0.659059 0.138 Uiso 1 1 calc R U . . .
C13 C 0.29638(14) 0.36070(11) 0.70362(15) 0.1277(17) Uani 1 1 d . . . . .
H13 H 0.273449 0.371730 0.723753 0.153 Uiso 1 1 calc R U . . .
C14 C 0.29329(7) 0.30135(4) 0.59297(6) 0.0422(4) Uani 1 1 d . . . . .
C15 C 0.26937(7) 0.27325(4) 0.60829(6) 0.0434(4) Uani 1 1 d . . . . .
C16 C 0.26219(12) 0.26407(6) 0.66102(7) 0.0776(9) Uani 1 1 d . . . . .
H16 H 0.272575 0.275574 0.689731 0.093 Uiso 1 1 calc R U . . .
C17 C 0.30095(7) 0.30995(4) 0.54196(6) 0.0385(3) Uani 1 1 d . . . . .
C18 C 0.32439(10) 0.33940(5) 0.52571(8) 0.0651(7) Uani 1 1 d . . . . .
H18 H 0.337174 0.355463 0.546884 0.078 Uiso 1 1 calc R U . . .
C19 C 0.14445(15) 0.26430(9) 0.47467(16) 0.0496(9) Uani 0.5 1 d . . P A -1
H19 H 0.147299 0.245232 0.456002 0.060 Uiso 0.5 1 calc R U P A -1
C20 C 0.09945(16) 0.27988(10) 0.47384(19) 0.0586(11) Uani 0.5 1 d . . P A -1
H20 H 0.073165 0.271057 0.455420 0.070 Uiso 0.5 1 calc R U P A -1
C22 C 0.13394(17) 0.31924(11) 0.5280(2) 0.0669(13) Uani 0.5 1 d . . P A -1
H22 H 0.131873 0.338121 0.547225 0.080 Uiso 0.5 1 calc R U P A -1
C31 C 0.17781(15) 0.30165(10) 0.52694(17) 0.0535(9) Uani 0.5 1 d . . P A -1
H31 H 0.204519 0.309247 0.546068 0.064 Uiso 0.5 1 calc R U P A -1
C21 C 0.09288(11) 0.30845(7) 0.500000 0.0530(7) Uani 1 2 d S T P . .
C23 C 0.04503(12) 0.32647(7) 0.500000 0.0605(8) Uani 1 2 d S T P A .
C24 C 0.000000 0.30991(10) 0.500000 0.0591(11) Uani 1 4 d S T P . .
H24 H -0.000001 0.287436 0.500000 0.071 Uiso 1 4 calc R U P A .
C25 C 0.04434(14) 0.36014(8) 0.500000 0.0804(13) Uani 1 2 d S T P . .
H25 H 0.074272 0.371359 0.500000 0.096 Uiso 1 2 calc R U P A .
C26 C 0.000000 0.37738(11) 0.500000 0.0826(19) Uani 1 4 d S T P A .
C27 C 0.000000 0.41328(12) 0.500000 0.104(3) Uani 1 4 d S T P . .
C28 C 0.0400(2) 0.43070(12) 0.500000 0.277(8) Uani 1 2 d S T P A .
H28 H 0.070486 0.420160 0.500000 0.333 Uiso 1 2 calc R U P . .
C29 C 0.0397(2) 0.46495(12) 0.500000 0.306(10) Uani 1 2 d S T P . .
H29 H 0.070074 0.475664 0.500000 0.367 Uiso 1 2 calc R U P A .
C30 C 0.000000 0.48194(13) 0.500000 0.141(4) Uani 1 4 d S T P A .
Fe1 Fe 0.250000 0.250000 0.500000 0.02279(8) Uani 1 4 d S T P A .
N1 N 0.28640(7) 0.29216(4) 0.500000 0.0281(3) Uani 1 2 d S T P . .
N2 N 0.250000 0.250000 0.57646(6) 0.0310(4) Uani 1 2 d S T P . .
N3 N 0.18397(7) 0.27437(4) 0.500000 0.0348(4) Uani 1 2 d S T P . .
O1 O 0.56447(11) 0.500000 0.95402(8) 0.0705(8) Uani 1 2 d S T P . .
O2 O 0.500000 0.54270(7) 0.95414(9) 0.0818(9) Uani 1 2 d S T P . .
O3 O 0.55866(14) 0.59520(5) 1.000000 0.0898(10) Uani 1 2 d S T P . .
O4 O 0.64638(10) 0.53527(11) 1.000000 0.1067(13) Uani 1 2 d S T P . .
O5 O 0.45086(5) 0.46771(3) 0.86200(4) 0.0452(3) Uani 1 1 d . . . . .
O6 O 0.40748(7) 0.43958(4) 0.92177(5) 0.0675(5) Uani 1 1 d . . . . .
Zr01 Zr 0.500000 0.500000 0.90545(2) 0.02359(7) Uani 1 4 d S T P . .
Zr02 Zr 0.56557(2) 0.54254(2) 1.000000 0.03255(7) Uani 1 2 d S T P . .
 
 
_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
C1 O5 1.271(2) . ?
C1 O6 1.267(2) . ?
C1 C2 1.499(2) . ?
C2 C7 1.358(4) . ?
C2 C3 1.372(3) . ?
C3 C4 1.389(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.362(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.366(4) . ?
C5 C8 1.498(3) . ?
C6 C7 1.392(3) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 C13 1.350(5) . ?
C8 C9 1.354(4) . ?
C9 C10 1.392(3) . ?
C9 H9 0.9300 . ?
C10 C11 1.356(4) . ?
C10 H10 0.9300 . ?
C11 C12 1.363(4) . ?
C11 C14 1.504(2) . ?
C12 C13 1.394(3) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 C15 1.388(2) . ?
C14 C17 1.392(2) . ?
C15 N2 1.3733(17) . ?
C15 C16 1.439(2) . ?
C16 C16 1.337(5) 6 ?
C16 H16 0.9300 . ?
C17 N1 1.3755(17) . ?
C17 C18 1.436(2) . ?
C18 C18 1.341(4) 10_556 ?
C18 H18 0.9300 . ?
C19 N3 1.320(4) . ?
C19 C20 1.373(6) . ?
C19 H19 0.9300 . ?
C20 C21 1.376(5) . ?
C20 H20 0.9300 . ?
C22 C31 1.388(6) . ?
C22 C21 1.398(5) . ?
C22 H22 0.9300 . ?
C31 N3 1.340(4) . ?
C31 H31 0.9300 . ?
C21 C23 1.488(4) . ?
C23 C24 1.392(4) . ?
C23 C25 1.393(4) . ?
C24 H24 0.9300 . ?
C25 C26 1.391(4) . ?
C25 H25 0.9300 . ?
C26 C27 1.485(7) . ?
C27 C28 1.295(6) . ?
C27 C28 1.295(6) 3_556 ?
C28 C29 1.417(7) . ?
C28 H28 0.9300 . ?
C29 C30 1.280(6) . ?
C29 H29 0.9300 . ?
C30 C30 1.494(11) 9_566 ?
Fe1 N2 1.9934(16) 13_556 ?
Fe1 N2 1.9935(16) . ?
Fe1 N1 2.0007(16) 13_556 ?
Fe1 N1 2.0008(16) . ?
Fe1 N3 2.044(2) 13_556 ?
Fe1 N3 2.044(2) . ?
O1 Zr02 2.1298(11) 11_565 ?
O1 Zr02 2.1298(11) . ?
O1 Zr01 2.149(2) . ?
O2 Zr02 2.1322(14) 3_657 ?
O2 Zr02 2.1322(14) . ?
O2 Zr01 2.175(2) . ?
O3 Zr02 2.187(2) . ?
O4 Zr02 2.196(3) . ?
O5 Zr01 2.1952(12) . ?
O6 Zr02 2.2878(13) 9_667 ?
Zr01 Zr02 3.5058(5) 11_565 ?
Zr01 Zr02 3.5058(5) 3_657 ?
Zr01 Zr02 3.5058(5) 9_667 ?
Zr01 Zr02 3.5059(5) . ?
Zr02 Zr02 3.5202(8) 11_565 ?
Zr02 Zr02 3.5308(9) 3_657 ?
 
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
O5 C1 O6 126.73(15) . . ?
O5 C1 C2 115.58(16) . . ?
O6 C1 C2 117.69(19) . . ?
C7 C2 C3 118.57(19) . . ?
C7 C2 C1 121.6(2) . . ?
C3 C2 C1 119.8(2) . . ?
C2 C3 C4 120.6(2) . . ?
C2 C3 H3 119.7 . . ?
C4 C3 H3 119.7 . . ?
C5 C4 C3 121.2(2) . . ?
C5 C4 H4 119.4 . . ?
C3 C4 H4 119.4 . . ?
C4 C5 C6 117.5(2) . . ?
C4 C5 C8 120.9(2) . . ?
C6 C5 C8 121.5(2) . . ?
C5 C6 C7 121.8(3) . . ?
C5 C6 H6 119.1 . . ?
C7 C6 H6 119.1 . . ?
C2 C7 C6 120.2(3) . . ?
C2 C7 H7 119.9 . . ?
C6 C7 H7 119.9 . . ?
C13 C8 C9 117.1(2) . . ?
C13 C8 C5 121.8(3) . . ?
C9 C8 C5 121.1(3) . . ?
C8 C9 C10 121.7(3) . . ?
C8 C9 H9 119.2 . . ?
C10 C9 H9 119.2 . . ?
C11 C10 C9 121.4(3) . . ?
C11 C10 H10 119.3 . . ?
C9 C10 H10 119.3 . . ?
C10 C11 C12 116.9(2) . . ?
C10 C11 C14 121.7(2) . . ?
C12 C11 C14 121.4(2) . . ?
C11 C12 C13 121.3(3) . . ?
C11 C12 H12 119.4 . . ?
C13 C12 H12 119.4 . . ?
C8 C13 C12 121.6(3) . . ?
C8 C13 H13 119.2 . . ?
C12 C13 H13 119.2 . . ?
C15 C14 C17 123.90(13) . . ?
C15 C14 C11 117.84(15) . . ?
C17 C14 C11 118.25(15) . . ?
N2 C15 C14 126.10(13) . . ?
N2 C15 C16 109.96(16) . . ?
C14 C15 C16 123.93(15) . . ?
C16 C16 C15 107.20(11) 6 . ?
C16 C16 H16 126.4 6 . ?
C15 C16 H16 126.4 . . ?
N1 C17 C14 125.52(14) . . ?
N1 C17 C18 110.14(14) . . ?
C14 C17 C18 124.32(15) . . ?
C18 C18 C17 107.16(10) 10_556 . ?
C18 C18 H18 126.4 10_556 . ?
C17 C18 H18 126.4 . . ?
N3 C19 C20 124.8(3) . . ?
N3 C19 H19 117.6 . . ?
C20 C19 H19 117.6 . . ?
C19 C20 C21 120.6(4) . . ?
C19 C20 H20 119.7 . . ?
C21 C20 H20 119.7 . . ?
C31 C22 C21 119.7(3) . . ?
C31 C22 H22 120.2 . . ?
C21 C22 H22 120.2 . . ?
N3 C31 C22 123.9(3) . . ?
N3 C31 H31 118.0 . . ?
C22 C31 H31 118.0 . . ?
C20 C21 C22 115.6(3) . . ?
C20 C21 C23 122.8(3) . . ?
C22 C21 C23 121.6(3) . . ?
C24 C23 C25 118.7(3) . . ?
C24 C23 C21 120.5(3) . . ?
C25 C23 C21 120.8(3) . . ?
C23 C24 C23 121.1(4) 3_556 . ?
C23 C24 H24 119.5 3_556 . ?
C23 C24 H24 119.5 . . ?
C26 C25 C23 121.6(3) . . ?
C26 C25 H25 119.2 . . ?
C23 C25 H25 119.2 . . ?
C25 C26 C25 118.3(4) . 3_556 ?
C25 C26 C27 120.9(2) . . ?
C25 C26 C27 120.9(2) 3_556 . ?
C28 C27 C28 112.4(6) . 3_556 ?
C28 C27 C26 123.8(3) . . ?
C28 C27 C26 123.8(3) 3_556 . ?
C27 C28 C29 123.5(6) . . ?
C27 C28 H28 118.2 . . ?
C29 C28 H28 118.2 . . ?
C30 C29 C28 123.6(6) . . ?
C30 C29 H29 118.2 . . ?
C28 C29 H29 118.2 . . ?
C29 C30 C29 113.3(6) 3_556 . ?
C29 C30 C30 123.3(3) 3_556 9_566 ?
C29 C30 C30 123.3(3) . 9_566 ?
N2 Fe1 N2 180.0 13_556 . ?
N2 Fe1 N1 90.0 13_556 13_556 ?
N2 Fe1 N1 90.0 . 13_556 ?
N2 Fe1 N1 90.0 13_556 . ?
N2 Fe1 N1 90.0 . . ?
N1 Fe1 N1 180.0 13_556 . ?
N2 Fe1 N3 90.0 13_556 13_556 ?
N2 Fe1 N3 90.0 . 13_556 ?
N1 Fe1 N3 89.77(7) 13_556 13_556 ?
N1 Fe1 N3 90.23(7) . 13_556 ?
N2 Fe1 N3 90.0 13_556 . ?
N2 Fe1 N3 90.0 . . ?
N1 Fe1 N3 90.23(7) 13_556 . ?
N1 Fe1 N3 89.77(7) . . ?
N3 Fe1 N3 180.0 13_556 . ?
C17 N1 C17 105.39(17) 10_556 . ?
C17 N1 Fe1 127.29(8) 10_556 . ?
C17 N1 Fe1 127.30(8) . . ?
C15 N2 C15 105.65(17) . 6 ?
C15 N2 Fe1 127.17(9) . . ?
C15 N2 Fe1 127.17(9) 6 . ?
C19 N3 C31 115.4(3) . . ?
C19 N3 Fe1 123.1(2) . . ?
C31 N3 Fe1 121.6(2) . . ?
Zr02 O1 Zr02 111.47(9) 11_565 . ?
Zr02 O1 Zr01 110.06(9) 11_565 . ?
Zr02 O1 Zr01 110.06(9) . . ?
Zr02 O2 Zr02 111.78(11) 3_657 . ?
Zr02 O2 Zr01 108.95(9) 3_657 . ?
Zr02 O2 Zr01 108.95(9) . . ?
C1 O5 Zr01 131.89(10) . . ?
C1 O6 Zr02 132.89(13) . 9_667 ?
O1 Zr01 O1 107.78(15) 2_665 . ?
O1 Zr01 O2 69.89(6) 2_665 2_665 ?
O1 Zr01 O2 69.89(6) . 2_665 ?
O1 Zr01 O2 69.89(6) 2_665 . ?
O1 Zr01 O2 69.88(6) . . ?
O2 Zr01 O2 108.60(18) 2_665 . ?
O1 Zr01 O5 142.28(4) 2_665 2_665 ?
O1 Zr01 O5 79.47(7) . 2_665 ?
O2 Zr01 O5 142.69(4) 2_665 2_665 ?
O2 Zr01 O5 78.87(8) . 2_665 ?
O1 Zr01 O5 142.28(4) 2_665 12_655 ?
O1 Zr01 O5 79.47(7) . 12_655 ?
O2 Zr01 O5 78.86(8) 2_665 12_655 ?
O2 Zr01 O5 142.69(4) . 12_655 ?
O5 Zr01 O5 74.98(8) 2_665 12_655 ?
O1 Zr01 O5 79.47(7) 2_665 11_565 ?
O1 Zr01 O5 142.28(4) . 11_565 ?
O2 Zr01 O5 142.69(4) 2_665 11_565 ?
O2 Zr01 O5 78.87(8) . 11_565 ?
O5 Zr01 O5 74.13(8) 2_665 11_565 ?
O5 Zr01 O5 117.86(7) 12_655 11_565 ?
O1 Zr01 O5 79.47(7) 2_665 . ?
O1 Zr01 O5 142.28(4) . . ?
O2 Zr01 O5 78.86(8) 2_665 . ?
O2 Zr01 O5 142.69(4) . . ?
O5 Zr01 O5 117.86(7) 2_665 . ?
O5 Zr01 O5 74.13(8) 12_655 . ?
O5 Zr01 O5 74.98(8) 11_565 . ?
O1 Zr01 Zr02 89.57(7) 2_665 11_565 ?
O1 Zr01 Zr02 34.79(4) . 11_565 ?
O2 Zr01 Zr02 35.12(4) 2_665 11_565 ?
O2 Zr01 Zr02 89.85(8) . 11_565 ?
O5 Zr01 Zr02 111.40(4) 2_665 11_565 ?
O5 Zr01 Zr02 75.75(4) 12_655 11_565 ?
O5 Zr01 Zr02 166.39(3) 11_565 11_565 ?
O5 Zr01 Zr02 111.15(4) . 11_565 ?
O1 Zr01 Zr02 34.80(4) 2_665 3_657 ?
O1 Zr01 Zr02 89.56(7) . 3_657 ?
O2 Zr01 Zr02 89.85(8) 2_665 3_657 ?
O2 Zr01 Zr02 35.11(4) . 3_657 ?
O5 Zr01 Zr02 111.15(4) 2_665 3_657 ?
O5 Zr01 Zr02 166.39(3) 12_655 3_657 ?
O5 Zr01 Zr02 75.75(4) 11_565 3_657 ?
O5 Zr01 Zr02 111.40(4) . 3_657 ?
Zr02 Zr01 Zr02 90.642(16) 11_565 3_657 ?
O1 Zr01 Zr02 34.80(4) 2_665 9_667 ?
O1 Zr01 Zr02 89.56(7) . 9_667 ?
O2 Zr01 Zr02 35.12(4) 2_665 9_667 ?
O2 Zr01 Zr02 89.85(8) . 9_667 ?
O5 Zr01 Zr02 166.39(3) 2_665 9_667 ?
O5 Zr01 Zr02 111.15(4) 12_655 9_667 ?
O5 Zr01 Zr02 111.40(4) 11_565 9_667 ?
O5 Zr01 Zr02 75.75(4) . 9_667 ?
Zr02 Zr01 Zr02 60.470(14) 11_565 9_667 ?
Zr02 Zr01 Zr02 60.270(14) 3_657 9_667 ?
O1 Zr01 Zr02 89.57(7) 2_665 . ?
O1 Zr01 Zr02 34.79(4) . . ?
O2 Zr01 Zr02 89.85(8) 2_665 . ?
O2 Zr01 Zr02 35.11(4) . . ?
O5 Zr01 Zr02 75.75(4) 2_665 . ?
O5 Zr01 Zr02 111.40(4) 12_655 . ?
O5 Zr01 Zr02 111.15(4) 11_565 . ?
O5 Zr01 Zr02 166.39(3) . . ?
Zr02 Zr01 Zr02 60.270(14) 11_565 . ?
Zr02 Zr01 Zr02 60.470(15) 3_657 . ?
Zr02 Zr01 Zr02 90.643(16) 9_667 . ?
O1 Zr02 O1 68.51(9) . 10_557 ?
O1 Zr02 O2 71.05(9) . . ?
O1 Zr02 O2 107.86(12) 10_557 . ?
O1 Zr02 O2 107.86(12) . 10_557 ?
O1 Zr02 O2 71.06(9) 10_557 10_557 ?
O2 Zr02 O2 68.22(11) . 10_557 ?
O1 Zr02 O3 145.31(4) . . ?
O1 Zr02 O3 145.31(4) 10_557 . ?
O2 Zr02 O3 85.78(12) . . ?
O2 Zr02 O3 85.78(12) 10_557 . ?
O1 Zr02 O4 84.30(12) . . ?
O1 Zr02 O4 84.30(12) 10_557 . ?
O2 Zr02 O4 145.14(5) . . ?
O2 Zr02 O4 145.14(5) 10_557 . ?
O3 Zr02 O4 102.75(15) . . ?
O1 Zr02 O6 140.67(6) . 9_667 ?
O1 Zr02 O6 76.69(7) 10_557 9_667 ?
O2 Zr02 O6 139.60(7) . 9_667 ?
O2 Zr02 O6 76.21(8) 10_557 9_667 ?
O3 Zr02 O6 72.83(6) . 9_667 ?
O4 Zr02 O6 74.34(7) . 9_667 ?
O1 Zr02 O6 76.70(7) . 2_665 ?
O1 Zr02 O6 140.67(6) 10_557 2_665 ?
O2 Zr02 O6 76.21(8) . 2_665 ?
O2 Zr02 O6 139.60(7) 10_557 2_665 ?
O3 Zr02 O6 72.83(6) . 2_665 ?
O4 Zr02 O6 74.34(7) . 2_665 ?
O6 Zr02 O6 126.13(8) 9_667 2_665 ?
O1 Zr02 Zr01 88.50(7) . 9_667 ?
O1 Zr02 Zr01 35.15(6) 10_557 9_667 ?
O2 Zr02 Zr01 88.79(8) . 9_667 ?
O2 Zr02 Zr01 35.94(6) 10_557 9_667 ?
O3 Zr02 Zr01 117.22(6) . 9_667 ?
O4 Zr02 Zr01 115.47(7) . 9_667 ?
O6 Zr02 Zr01 72.25(4) 9_667 9_667 ?
O6 Zr02 Zr01 161.61(4) 2_665 9_667 ?
O1 Zr02 Zr01 35.15(6) . . ?
O1 Zr02 Zr01 88.50(7) 10_557 . ?
O2 Zr02 Zr01 35.93(6) . . ?
O2 Zr02 Zr01 88.79(8) 10_557 . ?
O3 Zr02 Zr01 117.22(6) . . ?
O4 Zr02 Zr01 115.47(7) . . ?
O6 Zr02 Zr01 161.61(4) 9_667 . ?
O6 Zr02 Zr01 72.25(4) 2_665 . ?
Zr01 Zr02 Zr01 89.356(16) 9_667 . ?
O1 Zr02 Zr02 34.27(4) . 11_565 ?
O1 Zr02 Zr02 34.27(4) 10_557 11_565 ?
O2 Zr02 Zr02 90.17(8) . 11_565 ?
O2 Zr02 Zr02 90.18(8) 10_557 11_565 ?
O3 Zr02 Zr02 175.12(10) . 11_565 ?
O4 Zr02 Zr02 82.13(11) . 11_565 ?
O6 Zr02 Zr02 108.87(5) 9_667 11_565 ?
O6 Zr02 Zr02 108.87(5) 2_665 11_565 ?
Zr01 Zr02 Zr02 59.864(7) 9_667 11_565 ?
Zr01 Zr02 Zr02 59.864(8) . 11_565 ?
O1 Zr02 Zr02 89.20(8) . 3_657 ?
O1 Zr02 Zr02 89.20(8) 10_557 3_657 ?
O2 Zr02 Zr02 34.11(5) . 3_657 ?
O2 Zr02 Zr02 34.11(5) 10_557 3_657 ?
O3 Zr02 Zr02 85.12(10) . 3_657 ?
O4 Zr02 Zr02 172.13(11) . 3_657 ?
O6 Zr02 Zr02 108.49(5) 9_667 3_657 ?
O6 Zr02 Zr02 108.49(5) 2_665 3_657 ?
Zr01 Zr02 Zr02 59.764(8) 9_667 3_657 ?
Zr01 Zr02 Zr02 59.764(8) . 3_657 ?
Zr02 Zr02 Zr02 89.998(1) 11_565 3_657 ?
 
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
O5 C1 C2 C7 -169.5(3) . . . . ?
O6 C1 C2 C7 11.0(5) . . . . ?
O5 C1 C2 C3 14.0(4) . . . . ?
O6 C1 C2 C3 -165.5(3) . . . . ?
C7 C2 C3 C4 -0.1(6) . . . . ?
C1 C2 C3 C4 176.5(3) . . . . ?
C2 C3 C4 C5 3.8(7) . . . . ?
C3 C4 C5 C6 -5.0(6) . . . . ?
C3 C4 C5 C8 179.8(4) . . . . ?
C4 C5 C6 C7 2.7(7) . . . . ?
C8 C5 C6 C7 177.9(4) . . . . ?
C3 C2 C7 C6 -2.2(7) . . . . ?
C1 C2 C7 C6 -178.7(4) . . . . ?
C5 C6 C7 C2 0.9(8) . . . . ?
C4 C5 C8 C13 -138.4(4) . . . . ?
C6 C5 C8 C13 46.6(6) . . . . ?
C4 C5 C8 C9 39.9(5) . . . . ?
C6 C5 C8 C9 -135.1(4) . . . . ?
C13 C8 C9 C10 -1.8(6) . . . . ?
C5 C8 C9 C10 179.8(3) . . . . ?
C8 C9 C10 C11 0.3(6) . . . . ?
C9 C10 C11 C12 1.4(6) . . . . ?
C9 C10 C11 C14 -178.1(3) . . . . ?
C10 C11 C12 C13 -1.6(6) . . . . ?
C14 C11 C12 C13 177.9(4) . . . . ?
C9 C8 C13 C12 1.6(7) . . . . ?
C5 C8 C13 C12 180.0(4) . . . . ?
C11 C12 C13 C8 0.1(7) . . . . ?
C10 C11 C14 C15 111.4(3) . . . . ?
C12 C11 C14 C15 -68.0(4) . . . . ?
C10 C11 C14 C17 -69.1(3) . . . . ?
C12 C11 C14 C17 111.4(3) . . . . ?
C17 C14 C15 N2 0.1(3) . . . . ?
C11 C14 C15 N2 179.54(18) . . . . ?
C17 C14 C15 C16 178.9(2) . . . . ?
C11 C14 C15 C16 -1.7(4) . . . . ?
N2 C15 C16 C16 -1.3(4) . . . 6 ?
C14 C15 C16 C16 179.8(3) . . . 6 ?
C15 C14 C17 N1 -0.3(3) . . . . ?
C11 C14 C17 N1 -179.7(2) . . . . ?
C15 C14 C17 C18 178.1(2) . . . . ?
C11 C14 C17 C18 -1.3(3) . . . . ?
N1 C17 C18 C18 -0.43(18) . . . 10_556 ?
C14 C17 C18 C18 -179.03(17) . . . 10_556 ?
N3 C19 C20 C21 0.9(7) . . . . ?
C21 C22 C31 N3 0.4(8) . . . . ?
C19 C20 C21 C22 -2.1(6) . . . . ?
C19 C20 C21 C23 179.5(3) . . . . ?
C31 C22 C21 C20 1.5(6) . . . . ?
C31 C22 C21 C23 179.9(4) . . . . ?
C20 C21 C23 C24 36.1(3) . . . . ?
C22 C21 C23 C24 -142.2(3) . . . . ?
C20 C21 C23 C25 -143.9(3) . . . . ?
C22 C21 C23 C25 37.8(3) . . . . ?
C25 C23 C24 C23 0.0 . . . 3_556 ?
C21 C23 C24 C23 180.0 . . . 3_556 ?
C24 C23 C25 C26 0.0 . . . . ?
C21 C23 C25 C26 180.0 . . . . ?
C23 C25 C26 C25 0.0 . . . 3_556 ?
C23 C25 C26 C27 180.0 . . . . ?
C25 C26 C27 C28 0.0 . . . . ?
C25 C26 C27 C28 180.0 3_556 . . . ?
C25 C26 C27 C28 180.0 . . . 3_556 ?
C25 C26 C27 C28 0.0 3_556 . . 3_556 ?
C28 C27 C28 C29 0.0 3_556 . . . ?
C26 C27 C28 C29 180.0 . . . . ?
C27 C28 C29 C30 0.0 . . . . ?
C28 C29 C30 C29 0.0 . . . 3_556 ?
C28 C29 C30 C30 180.0 . . . 9_566 ?
C14 C17 N1 C17 179.26(13) . . . 10_556 ?
C18 C17 N1 C17 0.7(3) . . . 10_556 ?
C14 C17 N1 Fe1 0.9(3) . . . . ?
C18 C17 N1 Fe1 -177.71(17) . . . . ?
C14 C15 N2 C15 179.4(3) . . . 6 ?
C16 C15 N2 C15 0.46(16) . . . 6 ?
C14 C15 N2 Fe1 -0.6(3) . . . . ?
C16 C15 N2 Fe1 -179.53(16) . . . . ?
C20 C19 N3 C31 1.0(6) . . . . ?
C20 C19 N3 Fe1 179.8(4) . . . . ?
C22 C31 N3 C19 -1.7(6) . . . . ?
C22 C31 N3 Fe1 179.5(4) . . . . ?
O6 C1 O5 Zr01 9.0(4) . . . . ?
C2 C1 O5 Zr01 -170.41(17) . . . . ?
O5 C1 O6 Zr02 -9.1(4) . . . 9_667 ?
C2 C1 O6 Zr02 170.26(19) . . . 9_667 ?
 
_refine_diff_density_max    1.711
_refine_diff_density_min   -1.068
_refine_diff_density_rms    0.066




loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1 -0.023 -0.004  0.276     22968      4432 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                           ?