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#$Date: 2023-02-20 12:16:19 +0200 (Mon, 20 Feb 2023) $
#$Revision: 281005 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/23/7712324.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7712324
loop_
_publ_author_name
'Chuprin, Alexander S.'
'Pavlov, Alexander A.'
'Vologzhanina, Anna V. V.'
'Dorovatovskii, Pavel'
'Makarenkov, Anton V.'
'Ol'shevskaya, Valentina Antonovna'
'Dudkin, Semyon V.'
'Voloshin, Yan Z.'
_publ_section_title
;
 Multistep synthesis and X-ray structure of the carboxyl-terminated hybrid
 iron(II) phthalocyaninatoclathrochelates and their postsynthetic
 transformation into polytopic carboranyl-containing derivatives
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00076A
_journal_year                    2023
_chemical_formula_moiety         'C57 H45 B Fe N14 O8 Zr, 2.5(C6 H6)'
_chemical_formula_sum            'C72 H60 B Fe N14 O8 Zr'
_chemical_formula_weight         1407.22
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-04-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-09-07 deposited with the CCDC.	2023-02-16 downloaded from the CCDC.
;
_cell_angle_alpha                90.70(3)
_cell_angle_beta                 93.99(3)
_cell_angle_gamma                106.72(3)
_cell_formula_units_Z            2
_cell_length_a                   12.236(3)
_cell_length_b                   12.862(3)
_cell_length_c                   23.178(5)
_cell_measurement_reflns_used    942
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.092
_cell_measurement_theta_min      1.846
_cell_volume                     3483.1(15)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rayonix CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.745
_diffrn_reflns_av_R_equivalents  0.0659
_diffrn_reflns_av_unetI/netI     0.0721
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            52706
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.551
_diffrn_reflns_theta_max         31.012
_diffrn_reflns_theta_min         1.734
_exptl_absorpt_coefficient_mu    0.478
_exptl_absorpt_correction_T_max  0.093
_exptl_absorpt_correction_T_min  0.041
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 2010)'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_description       plate
_exptl_crystal_F_000             1450
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: benzene -- iso-octane'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.317
_refine_diff_density_min         -1.677
_refine_diff_density_rms         0.112
_refine_ls_extinction_coef       0.0046(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     903
_refine_ls_number_reflns         19204
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0950
_refine_ls_R_factor_gt           0.0595
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0400P)²+8.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1306
_refine_ls_wR_factor_ref         0.1470
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13159
_reflns_number_total             19204
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt00076a2.cif
_cod_data_source_block           ac68
_cod_original_cell_volume        3483.1(13)
_cod_database_code               7712324
_shelxl_version_number           2014-3
_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.
;
_shelx_estimated_absorpt_t_max   0.995
_shelx_estimated_absorpt_t_min   0.945
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C16S) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
3. Rigid body (RIGU) restrains
 C18S, C13S, C17S, C16S, C14S, C15S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: C14S(0.5) H14S(0.5) C15S(0.5) H15S(0.5) C18S(0.5) H18S(0.5)
 C13S(0.5) H13S(0.5) C17S(0.5) H17S(0.5) C16S(0.5) H16S(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C9(H9A,H9B), C12(H12A,H12B), C15(H15A,H15B), C3(H3A,H3B),
 C16(H16A,H16B), C11(H11A,H11B), C10(H10A,H10B), C18(H18A,H18B), C4(H4A,H4B),
 C17(H17A,H17B), C5(H5A,H5B)
5.b Aromatic/amide H refined with riding coordinates:
 C23(H23), C5S(H5S), C22(H22), C45(H45), C32(H32), C12S(H12S), C47(H47),
 C21(H21), C2S(H2S), C56(H56), C10S(H10S), C38(H38), C55(H55), C48(H48),
 C40(H40), C52(H52), C37(H37), C1S(H1S), C24(H24), C7S(H7S), C29(H29), C39(H39),
  C8S(H8S), C30(H30), C9S(H9S), C53(H53), C46(H46), C31(H31), C11S(H11S),
 C3S(H3S), C6S(H6S), C4S(H4S), C14S(H14S), C15S(H15S), C18S(H18S), C13S(H13S),
 C17S(H17S), C16S(H16S)
5.c Idealised tetrahedral OH refined as rotating group:
 O8(H8)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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 0.48422(3) 0.09668(2) 0.85799(2) 0.01810(8) Uani 1 1 d . . . . .
Fe1 Fe 0.59708(4) 0.32629(3) 0.75668(2) 0.01806(10) Uani 1 1 d . . . . .
O4 O 0.5844(2) 0.25582(17) 0.87631(10) 0.0222(5) Uani 1 1 d . . . . .
O2 O 0.5903(2) 0.10494(17) 0.78976(10) 0.0216(5) Uani 1 1 d . . . . .
O3 O 0.78631(19) 0.49499(18) 0.71700(11) 0.0233(5) Uani 1 1 d . . . . .
N1 N 0.6125(2) 0.3162(2) 0.67554(12) 0.0217(5) Uani 1 1 d . . . . .
O1 O 0.6376(2) 0.40558(18) 0.64096(10) 0.0242(5) Uani 1 1 d . . . . .
O5 O 0.6003(2) 0.53475(17) 0.71024(11) 0.0226(5) Uani 1 1 d . . . . .
N3 N 0.7465(2) 0.4257(2) 0.76092(12) 0.0212(5) Uani 1 1 d . . . . .
N4 N 0.6429(2) 0.3232(2) 0.83708(12) 0.0209(5) Uani 1 1 d . . . . .
N11 N 0.3313(2) 0.0985(2) 0.90620(12) 0.0209(5) Uani 1 1 d . . . . .
N6 N 0.4414(2) 0.2692(2) 0.77487(12) 0.0199(5) Uani 1 1 d . . . . .
N8 N 0.7085(2) 0.0319(2) 0.94390(13) 0.0222(5) Uani 1 1 d . . . . .
N9 N 0.5456(2) 0.1021(2) 0.95252(12) 0.0206(5) Uani 1 1 d . . . . .
C27 C 0.6516(3) 0.0906(2) 0.96985(14) 0.0211(6) Uani 1 1 d . . . . .
O8 O 0.9807(3) 0.8572(2) 0.49851(13) 0.0382(7) Uani 1 1 d . . . . .
H8 H 1.0076 0.9148 0.4811 0.057 Uiso 1 1 calc GR . . . .
N2 N 0.6032(2) 0.1788(2) 0.74744(12) 0.0204(5) Uani 1 1 d . . . . .
N14 N 0.4575(2) -0.1596(2) 0.78564(12) 0.0211(5) Uani 1 1 d . . . . .
N7 N 0.5601(2) -0.0426(2) 0.86712(12) 0.0205(5) Uani 1 1 d . . . . .
N12 N 0.1746(2) 0.0076(2) 0.83608(12) 0.0219(5) Uani 1 1 d . . . . .
O6 O 0.39486(19) 0.17089(17) 0.79714(10) 0.0207(5) Uani 1 1 d . . . . .
C2 C 0.6055(3) 0.1416(3) 0.69478(14) 0.0212(6) Uani 1 1 d . . . . .
O7 O 0.9251(3) 0.9698(2) 0.55668(13) 0.0365(6) Uani 1 1 d . . . . .
N13 N 0.3449(2) -0.0467(2) 0.81896(12) 0.0209(5) Uani 1 1 d . . . . .
C20 C 0.6441(3) -0.1633(3) 0.82751(15) 0.0219(6) Uani 1 1 d . . . . .
C23 C 0.8529(3) -0.2011(3) 0.85157(17) 0.0307(8) Uani 1 1 d . . . . .
H23 H 0.9254 -0.2137 0.8586 0.037 Uiso 1 1 calc R . . . .
C5S C 0.8836(5) 0.1810(6) 0.7445(3) 0.0693(19) Uani 1 1 d . . . . .
H5S H 0.8375 0.1832 0.7756 0.083 Uiso 1 1 calc R . . . .
C25 C 0.7199(3) -0.1044(3) 0.87204(15) 0.0217(6) Uani 1 1 d . . . . .
C6 C 0.6435(3) 0.2085(3) 0.59184(16) 0.0301(8) Uani 1 1 d . . . . .
H6A H 0.7267 0.2376 0.5878 0.036 Uiso 1 1 calc R . . . .
H6B H 0.6034 0.2480 0.5655 0.036 Uiso 1 1 calc R . . . .
C26 C 0.6635(3) -0.0316(2) 0.89762(15) 0.0210(6) Uani 1 1 d . . . . .
C13 C 0.4338(3) 0.4376(3) 0.74714(15) 0.0223(6) Uani 1 1 d . . . . .
C19 C 0.5457(3) -0.1219(2) 0.82441(14) 0.0205(6) Uani 1 1 d . . . . .
C9 C 0.8037(3) 0.3662(3) 0.91256(17) 0.0299(8) Uani 1 1 d . . . . .
H9A H 0.8167 0.2940 0.9156 0.036 Uiso 1 1 calc R . . . .
H9B H 0.7512 0.3727 0.9422 0.036 Uiso 1 1 calc R . . . .
C22 C 0.7756(3) -0.2623(3) 0.80812(17) 0.0301(8) Uani 1 1 d . . . . .
H22 H 0.7959 -0.3166 0.7868 0.036 Uiso 1 1 calc R . . . .
C44 C 0.1769(3) -0.1317(3) 0.76445(15) 0.0228(6) Uani 1 1 d . . . . .
C45 C 0.0644(3) -0.1697(3) 0.74049(16) 0.0253(7) Uani 1 1 d . . . . .
H45 H 0.0071 -0.1388 0.7518 0.030 Uiso 1 1 calc R . . . .
C12 C 0.9299(3) 0.5118(3) 0.82014(18) 0.0296(8) Uani 1 1 d . . . . .
H12A H 0.9299 0.5874 0.8286 0.036 Uiso 1 1 calc R . . . .
H12B H 0.9722 0.5112 0.7853 0.036 Uiso 1 1 calc R . . . .
C50 C 0.3640(3) -0.1258(3) 0.78461(15) 0.0217(6) Uani 1 1 d . . . . .
C36 C 0.2286(3) 0.1872(3) 0.95922(15) 0.0235(6) Uani 1 1 d . . . . .
C32 C 0.6314(3) 0.2754(3) 1.08534(15) 0.0238(6) Uani 1 1 d . . . . .
H32 H 0.5749 0.3085 1.0953 0.029 Uiso 1 1 calc R . . . .
C42 C 0.2212(3) 0.0742(3) 0.88104(15) 0.0213(6) Uani 1 1 d . . . . .
C12S C 0.2556(4) 0.0070(4) 0.5618(2) 0.0386(9) Uani 1 1 d . . . . .
H12S H 0.2256 -0.0591 0.5397 0.046 Uiso 1 1 calc R . . . .
C47 C 0.1243(3) -0.2990(3) 0.68192(16) 0.0291(7) Uani 1 1 d . . . . .
H47 H 0.1049 -0.3554 0.6529 0.035 Uiso 1 1 calc R . . . .
C51 C 0.7433(3) 0.6048(3) 0.63602(15) 0.0237(7) Uani 1 1 d . . . . .
C21 C 0.6693(3) -0.2452(3) 0.79534(15) 0.0251(7) Uani 1 1 d . . . . .
H21 H 0.6162 -0.2873 0.7661 0.030 Uiso 1 1 calc R . . . .
C2S C 1.0201(4) 0.1763(4) 0.6546(2) 0.0458(11) Uani 1 1 d . . . . .
H2S H 1.0672 0.1741 0.6240 0.055 Uiso 1 1 calc R . . . .
C56 C 0.7393(3) 0.7101(3) 0.64826(17) 0.0270(7) Uani 1 1 d . . . . .
H56 H 0.6951 0.7221 0.6784 0.032 Uiso 1 1 calc R . . . .
C10S C 0.2973(4) 0.1033(4) 0.6539(2) 0.0434(10) Uani 1 1 d . . . . .
H10S H 0.2972 0.1034 0.6949 0.052 Uiso 1 1 calc R . . . .
C38 C 0.0780(3) 0.2504(3) 0.99151(18) 0.0322(8) Uani 1 1 d . . . . .
H38 H 0.0499 0.2916 1.0180 0.039 Uiso 1 1 calc R . . . .
C43 C 0.2319(3) -0.0494(2) 0.80873(15) 0.0213(6) Uani 1 1 d . . . . .
C55 C 0.7987(3) 0.7979(3) 0.61737(16) 0.0262(7) Uani 1 1 d . . . . .
H55 H 0.7953 0.8689 0.6268 0.031 Uiso 1 1 calc R . . . .
C8 C 0.7495(3) 0.3751(3) 0.85396(15) 0.0227(6) Uani 1 1 d . . . . .
C41 C 0.1547(3) 0.1293(3) 0.91315(15) 0.0228(6) Uani 1 1 d . . . . .
C48 C 0.2365(3) -0.2622(3) 0.70622(16) 0.0263(7) Uani 1 1 d . . . . .
H48 H 0.2939 -0.2929 0.6948 0.032 Uiso 1 1 calc R . . . .
C40 C 0.0418(3) 0.1311(3) 0.90571(16) 0.0258(7) Uani 1 1 d . . . . .
H40 H -0.0079 0.0924 0.8743 0.031 Uiso 1 1 calc R . . . .
C52 C 0.8065(3) 0.5901(3) 0.59028(16) 0.0293(8) Uani 1 1 d . . . . .
H52 H 0.8096 0.5190 0.5806 0.035 Uiso 1 1 calc R . . . .
C15 C 0.2564(3) 0.3062(3) 0.78870(18) 0.0292(8) Uani 1 1 d . . . . .
H15A H 0.2546 0.2852 0.8296 0.035 Uiso 1 1 calc R . . . .
H15B H 0.2090 0.2432 0.7646 0.035 Uiso 1 1 calc R . . . .
C37 C 0.1917(3) 0.2498(3) 0.99876(16) 0.0275(7) Uani 1 1 d . . . . .
H37 H 0.2421 0.2904 1.0294 0.033 Uiso 1 1 calc R . . . .
C1S C 0.9984(4) 0.0942(4) 0.6939(2) 0.0495(11) Uani 1 1 d . . . . .
H1S H 1.0306 0.0357 0.6901 0.059 Uiso 1 1 calc R . . . .
C24 C 0.8265(3) -0.1223(3) 0.88487(16) 0.0261(7) Uani 1 1 d . . . . .
H24 H 0.8785 -0.0822 0.9151 0.031 Uiso 1 1 calc R . . . .
C7S C 0.3018(4) 0.1029(4) 0.53436(19) 0.0404(9) Uani 1 1 d . . . . .
H7S H 0.3038 0.1028 0.4935 0.048 Uiso 1 1 calc R . . . .
C29 C 0.8000(3) 0.1739(3) 1.05657(15) 0.0245(7) Uani 1 1 d . . . . .
H29 H 0.8556 0.1390 1.0475 0.029 Uiso 1 1 calc R . . . .
C3 C 0.5980(3) 0.0270(3) 0.67860(16) 0.0269(7) Uani 1 1 d . . . . .
H3A H 0.5174 -0.0183 0.6782 0.032 Uiso 1 1 calc R . . . .
H3B H 0.6439 -0.0015 0.7078 0.032 Uiso 1 1 calc R . . . .
C33 C 0.6139(3) 0.2049(3) 1.03701(14) 0.0219(6) Uani 1 1 d . . . . .
C39 C 0.0043(3) 0.1914(3) 0.94579(18) 0.0320(8) Uani 1 1 d . . . . .
H39 H -0.0731 0.1927 0.9422 0.038 Uiso 1 1 calc R . . . .
C16 C 0.2065(3) 0.4018(3) 0.7810(2) 0.0402(10) Uani 1 1 d . . . . .
H16A H 0.1219 0.3748 0.7797 0.048 Uiso 1 1 calc R . . . .
H16B H 0.2333 0.4532 0.8146 0.048 Uiso 1 1 calc R . . . .
C8S C 0.3451(4) 0.1990(4) 0.5666(2) 0.0412(10) Uani 1 1 d . . . . .
H8S H 0.3773 0.2650 0.5479 0.049 Uiso 1 1 calc R . . . .
C14 C 0.3769(3) 0.3354(3) 0.77178(15) 0.0218(6) Uani 1 1 d . . . . .
C28 C 0.6974(3) 0.1557(3) 1.02264(14) 0.0214(6) Uani 1 1 d . . . . .
C11 C 0.9885(3) 0.4690(3) 0.87201(19) 0.0352(9) Uani 1 1 d . . . . .
H11A H 0.9996 0.3984 0.8608 0.042 Uiso 1 1 calc R . . . .
H11B H 1.0648 0.5207 0.8825 0.042 Uiso 1 1 calc R . . . .
C35 C 0.3372(3) 0.1641(3) 0.95460(16) 0.0228(6) Uani 1 1 d . . . . .
C7 C 0.8088(3) 0.4396(3) 0.80950(15) 0.0235(6) Uani 1 1 d . . . . .
C10 C 0.9175(3) 0.4545(3) 0.92424(19) 0.0376(9) Uani 1 1 d . . . . .
H10A H 0.9026 0.5240 0.9341 0.045 Uiso 1 1 calc R . . . .
H10B H 0.9612 0.4349 0.9578 0.045 Uiso 1 1 calc R . . . .
N10 N 0.4254(2) 0.2000(2) 0.99406(12) 0.0218(5) Uani 1 1 d . . . . .
C1 C 0.6188(3) 0.2259(3) 0.65271(15) 0.0233(6) Uani 1 1 d . . . . .
C30 C 0.8178(3) 0.2448(3) 1.10400(16) 0.0258(7) Uani 1 1 d . . . . .
H30 H 0.8878 0.2601 1.1275 0.031 Uiso 1 1 calc R . . . .
C9S C 0.3413(4) 0.1987(4) 0.6262(2) 0.0425(10) Uani 1 1 d . . . . .
H9S H 0.3694 0.2651 0.6481 0.051 Uiso 1 1 calc R . . . .
C18 C 0.3702(3) 0.5170(3) 0.72883(19) 0.0317(8) Uani 1 1 d . . . . .
H18A H 0.3925 0.5447 0.6904 0.038 Uiso 1 1 calc R . . . .
H18B H 0.3899 0.5794 0.7569 0.038 Uiso 1 1 calc R . . . .
C53 C 0.8652(3) 0.6771(3) 0.55848(17) 0.0316(8) Uani 1 1 d . . . . .
H53 H 0.9067 0.6651 0.5271 0.038 Uiso 1 1 calc R . . . .
C57 C 0.9260(3) 0.8769(3) 0.54144(16) 0.0299(8) Uani 1 1 d . . . . .
C46 C 0.0394(3) -0.2547(3) 0.69943(17) 0.0302(8) Uani 1 1 d . . . . .
H46 H -0.0369 -0.2832 0.6829 0.036 Uiso 1 1 calc R . . . .
C4 C 0.6421(5) 0.0200(3) 0.61917(19) 0.0465(11) Uani 1 1 d . . . . .
H4A H 0.7268 0.0427 0.6233 0.056 Uiso 1 1 calc R . . . .
H4B H 0.6164 -0.0568 0.6050 0.056 Uiso 1 1 calc R . . . .
N5 N 0.5403(2) 0.4467(2) 0.74027(12) 0.0212(5) Uani 1 1 d . . . . .
C49 C 0.2611(3) -0.1784(3) 0.74799(15) 0.0232(6) Uani 1 1 d . . . . .
C17 C 0.2415(3) 0.4607(3) 0.7259(2) 0.0438(11) Uani 1 1 d . . . . .
H17A H 0.1996 0.5155 0.7196 0.053 Uiso 1 1 calc R . . . .
H17B H 0.2202 0.4080 0.6926 0.053 Uiso 1 1 calc R . . . .
C31 C 0.7347(3) 0.2947(3) 1.11819(15) 0.0252(7) Uani 1 1 d . . . . .
H31 H 0.7497 0.3429 1.1511 0.030 Uiso 1 1 calc R . . . .
C11S C 0.2532(4) 0.0072(4) 0.6215(2) 0.0411(10) Uani 1 1 d . . . . .
H11S H 0.2213 -0.0587 0.6403 0.049 Uiso 1 1 calc R . . . .
C3S C 0.9734(4) 0.2619(4) 0.6598(3) 0.0567(14) Uani 1 1 d . . . . .
H3S H 0.9882 0.3189 0.6332 0.068 Uiso 1 1 calc R . . . .
C6S C 0.9300(4) 0.0969(5) 0.7387(2) 0.0595(14) Uani 1 1 d . . . . .
H6S H 0.9152 0.0401 0.7655 0.071 Uiso 1 1 calc R . . . .
B1 B 0.6889(3) 0.5068(3) 0.67659(17) 0.0234(7) Uani 1 1 d . . . . .
C54 C 0.8624(3) 0.7816(3) 0.57306(16) 0.0272(7) Uani 1 1 d . . . . .
C4S C 0.9039(5) 0.2623(6) 0.7054(3) 0.071(2) Uani 1 1 d . . . . .
H4S H 0.8702 0.3198 0.7092 0.085 Uiso 1 1 calc R . . . .
C34 C 0.5201(3) 0.1698(2) 0.99278(15) 0.0216(6) Uani 1 1 d . . . . .
C14S C 0.2345(7) 0.5670(7) 0.5535(3) 0.0335(16) Uani 0.5 1 d . U P . .
H14S H 0.1551 0.5295 0.5484 0.040 Uiso 0.5 1 calc R . P . .
C15S C 0.2692(6) 0.6786(6) 0.5542(3) 0.0275(13) Uani 0.5 1 d . U P . .
H15S H 0.2145 0.7178 0.5489 0.033 Uiso 0.5 1 calc R . P . .
C18S C 0.4297(8) 0.5705(10) 0.5670(3) 0.052(2) Uani 0.5 1 d . U P . .
H18S H 0.4874 0.5345 0.5704 0.062 Uiso 0.5 1 calc R . P . .
C13S C 0.3127(8) 0.5080(8) 0.5601(4) 0.045(2) Uani 0.5 1 d . U P . .
H13S H 0.2898 0.4309 0.5600 0.054 Uiso 0.5 1 calc R . P . .
C17S C 0.4591(8) 0.6770(9) 0.5688(3) 0.0478(19) Uani 0.5 1 d . U P . .
H17S H 0.5380 0.7159 0.5748 0.057 Uiso 0.5 1 calc R . P . .
C16S C 0.3835(7) 0.7326(8) 0.5627(3) 0.0400(17) Uani 0.5 1 d . U P . .
H16S H 0.4085 0.8097 0.5641 0.048 Uiso 0.5 1 calc R . P . .
C5 C 0.6038(5) 0.0874(4) 0.5751(2) 0.0511(12) Uani 1 1 d . . . . .
H5A H 0.5192 0.0632 0.5697 0.061 Uiso 1 1 calc R . . . .
H5B H 0.6339 0.0760 0.5377 0.061 Uiso 1 1 calc R . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0018 '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'
B B 0.0017 0.0008 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3647 0.9262 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0074 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0129 0.0068 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.1574 0.6341 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
O4 Zr1 O2 83.81(9) . . ?
O4 Zr1 N11 99.16(10) . . ?
O4 Zr1 N9 74.45(10) . . ?
O4 Zr1 N7 120.77(10) . . ?
O4 Zr1 O6 83.46(9) . . ?
O4 Zr1 N13 161.23(9) . . ?
O2 Zr1 N11 160.46(10) . . ?
O2 Zr1 N9 123.93(10) . . ?
O2 Zr1 N7 73.14(10) . . ?
O2 Zr1 O6 82.06(9) . . ?
O2 Zr1 N13 94.60(10) . . ?
N11 Zr1 N9 75.16(10) . . ?
N7 Zr1 N11 120.04(10) . . ?
N7 Zr1 N9 75.17(10) . . ?
N7 Zr1 N13 76.14(10) . . ?
O6 Zr1 N11 79.13(10) . . ?
O6 Zr1 N9 142.58(10) . . ?
O6 Zr1 N7 142.07(10) . . ?
O6 Zr1 N13 77.80(9) . . ?
N13 Zr1 N11 76.35(10) . . ?
N13 Zr1 N9 120.75(10) . . ?
N1 Fe1 N4 155.33(12) . . ?
N1 Fe1 N6 111.86(13) . . ?
N1 Fe1 N2 78.47(12) . . ?
N3 Fe1 N1 85.86(13) . . ?
N3 Fe1 N4 78.87(12) . . ?
N3 Fe1 N6 156.66(12) . . ?
N3 Fe1 N2 110.88(12) . . ?
N3 Fe1 N5 87.28(12) . . ?
N4 Fe1 N6 88.58(12) . . ?
N4 Fe1 N2 88.94(12) . . ?
N6 Fe1 N2 88.24(12) . . ?
N5 Fe1 N1 86.50(12) . . ?
N5 Fe1 N4 111.75(12) . . ?
N5 Fe1 N6 79.13(12) . . ?
N5 Fe1 N2 155.21(12) . . ?
N4 O4 Zr1 124.78(19) . . ?
N2 O2 Zr1 124.63(18) . . ?
N3 O3 B1 111.2(2) . . ?
O1 N1 Fe1 123.1(2) . . ?
C1 N1 Fe1 119.4(2) . . ?
C1 N1 O1 116.5(3) . . ?
N1 O1 B1 110.6(2) . . ?
N5 O5 B1 111.3(2) . . ?
O3 N3 Fe1 122.8(2) . . ?
C7 N3 Fe1 118.9(2) . . ?
C7 N3 O3 117.7(3) . . ?
O4 N4 Fe1 126.3(2) . . ?
C8 N4 Fe1 117.1(2) . . ?
C8 N4 O4 115.3(3) . . ?
C42 N11 Zr1 124.1(2) . . ?
C42 N11 C35 107.2(3) . . ?
C35 N11 Zr1 123.6(2) . . ?
O6 N6 Fe1 125.8(2) . . ?
C14 N6 Fe1 117.3(2) . . ?
C14 N6 O6 116.4(3) . . ?
C26 N8 C27 122.0(3) . . ?
C27 N9 Zr1 121.6(2) . . ?
C27 N9 C34 107.6(3) . . ?
C34 N9 Zr1 122.2(2) . . ?
N8 C27 N9 127.7(3) . . ?
N8 C27 C28 122.5(3) . . ?
N9 C27 C28 109.7(3) . . ?
O2 N2 Fe1 125.6(2) . . ?
C2 N2 Fe1 117.7(2) . . ?
C2 N2 O2 116.1(3) . . ?
C19 N14 C50 122.5(3) . . ?
C26 N7 Zr1 121.9(2) . . ?
C26 N7 C19 107.9(3) . . ?
C19 N7 Zr1 122.9(2) . . ?
C42 N12 C43 122.6(3) . . ?
N6 O6 Zr1 123.77(18) . . ?
N2 C2 C3 125.3(3) . . ?
N2 C2 C1 112.1(3) . . ?
C1 C2 C3 122.6(3) . . ?
C50 N13 Zr1 123.9(2) . . ?
C50 N13 C43 107.9(3) . . ?
C43 N13 Zr1 124.7(2) . . ?
C25 C20 C19 106.8(3) . . ?
C25 C20 C21 121.5(3) . . ?
C21 C20 C19 131.7(3) . . ?
C24 C23 C22 121.7(3) . . ?
C6S C5S C4S 119.9(6) . . ?
C20 C25 C26 106.4(3) . . ?
C20 C25 C24 121.1(3) . . ?
C24 C25 C26 132.5(3) . . ?
C1 C6 C5 110.2(3) . . ?
N8 C26 N7 127.9(3) . . ?
N8 C26 C25 122.7(3) . . ?
N7 C26 C25 109.3(3) . . ?
C14 C13 C18 121.7(3) . . ?
N5 C13 C14 111.9(3) . . ?
N5 C13 C18 126.3(3) . . ?
N14 C19 N7 128.2(3) . . ?
N14 C19 C20 122.4(3) . . ?
N7 C19 C20 109.4(3) . . ?
C8 C9 C10 111.3(3) . . ?
C21 C22 C23 121.3(3) . . ?
C45 C44 C43 132.5(3) . . ?
C45 C44 C49 121.0(3) . . ?
C49 C44 C43 106.5(3) . . ?
C46 C45 C44 117.4(3) . . ?
C7 C12 C11 108.6(3) . . ?
N14 C50 N13 127.6(3) . . ?
N14 C50 C49 122.3(3) . . ?
N13 C50 C49 109.9(3) . . ?
C41 C36 C35 106.3(3) . . ?
C37 C36 C41 121.2(3) . . ?
C37 C36 C35 132.5(3) . . ?
C31 C32 C33 117.1(3) . . ?
N11 C42 C41 110.0(3) . . ?
N12 C42 N11 128.2(3) . . ?
N12 C42 C41 121.8(3) . . ?
C7S C12S C11S 120.0(4) . . ?
C48 C47 C46 121.4(3) . . ?
C56 C51 C52 117.5(3) . . ?
C56 C51 B1 121.4(3) . . ?
C52 C51 B1 120.8(3) . . ?
C22 C21 C20 117.1(3) . . ?
C1S C2S C3S 120.1(5) . . ?
C55 C56 C51 121.5(3) . . ?
C9S C10S C11S 119.4(4) . . ?
C37 C38 C39 121.2(3) . . ?
N12 C43 N13 128.0(3) . . ?
N12 C43 C44 122.3(3) . . ?
N13 C43 C44 109.6(3) . . ?
C54 C55 C56 120.0(3) . . ?
N4 C8 C9 123.6(3) . . ?
N4 C8 C7 112.7(3) . . ?
C7 C8 C9 123.7(3) . . ?
C36 C41 C42 106.3(3) . . ?
C40 C41 C36 121.3(3) . . ?
C40 C41 C42 132.4(3) . . ?
C49 C48 C47 117.2(3) . . ?
C41 C40 C39 117.5(3) . . ?
C53 C52 C51 121.6(3) . . ?
C14 C15 C16 111.0(3) . . ?
C38 C37 C36 117.3(3) . . ?
C2S C1S C6S 120.3(5) . . ?
C23 C24 C25 117.2(3) . . ?
C12S C7S C8S 119.9(4) . . ?
C30 C29 C28 117.4(3) . . ?
C2 C3 C4 110.8(3) . . ?
C32 C33 C28 121.3(3) . . ?
C32 C33 C34 132.0(3) . . ?
C28 C33 C34 106.7(3) . . ?
C40 C39 C38 121.4(3) . . ?
C17 C16 C15 111.5(4) . . ?
C7S C8S C9S 119.7(4) . . ?
N6 C14 C13 112.2(3) . . ?
N6 C14 C15 124.1(3) . . ?
C13 C14 C15 123.7(3) . . ?
C29 C28 C27 132.6(3) . . ?
C29 C28 C33 121.2(3) . . ?
C33 C28 C27 106.2(3) . . ?
C10 C11 C12 111.5(3) . . ?
N11 C35 C36 110.1(3) . . ?
N10 C35 N11 127.4(3) . . ?
N10 C35 C36 122.5(3) . . ?
N3 C7 C12 126.1(3) . . ?
N3 C7 C8 111.8(3) . . ?
C8 C7 C12 122.1(3) . . ?
C11 C10 C9 111.5(3) . . ?
C34 N10 C35 122.2(3) . . ?
N1 C1 C2 111.8(3) . . ?
N1 C1 C6 125.9(3) . . ?
C2 C1 C6 122.2(3) . . ?
C29 C30 C31 121.4(3) . . ?
C10S C9S C8S 120.8(4) . . ?
C13 C18 C17 109.4(3) . . ?
C52 C53 C54 119.4(3) . . ?
O8 C57 C54 116.6(3) . . ?
O7 C57 O8 123.5(3) . . ?
O7 C57 C54 119.9(4) . . ?
C45 C46 C47 121.4(3) . . ?
C5 C4 C3 114.4(4) . . ?
O5 N5 Fe1 122.4(2) . . ?
C13 N5 Fe1 118.8(2) . . ?
C13 N5 O5 117.4(3) . . ?
C44 C49 C50 106.1(3) . . ?
C48 C49 C44 121.6(3) . . ?
C48 C49 C50 132.3(3) . . ?
C16 C17 C18 111.6(4) . . ?
C32 C31 C30 121.5(3) . . ?
C10S C11S C12S 120.2(4) . . ?
C2S C3S C4S 118.5(6) . . ?
C5S C6S C1S 120.2(6) . . ?
O3 B1 C51 106.0(3) . . ?
O1 B1 O3 110.4(3) . . ?
O1 B1 O5 110.6(3) . . ?
O1 B1 C51 110.0(3) . . ?
O5 B1 O3 110.3(3) . . ?
O5 B1 C51 109.3(3) . . ?
C55 C54 C53 120.0(3) . . ?
C55 C54 C57 118.8(3) . . ?
C53 C54 C57 121.3(3) . . ?
C5S C4S C3S 121.0(5) . . ?
N9 C34 C33 109.8(3) . . ?
N10 C34 N9 127.9(3) . . ?
N10 C34 C33 122.3(3) . . ?
C15S C14S C13S 121.4(8) . . ?
C16S C15S C14S 119.3(8) . . ?
C17S C18S C13S 121.1(9) . . ?
C14S C13S C18S 115.6(9) . . ?
C18S C17S C16S 122.7(9) . . ?
C17S C16S C15S 119.8(9) . . ?
C4 C5 C6 112.8(4) . . ?
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 O4 2.082(2) . ?
Zr1 O2 2.100(2) . ?
Zr1 N11 2.251(3) . ?
Zr1 N9 2.260(3) . ?
Zr1 N7 2.248(3) . ?
Zr1 O6 2.125(2) . ?
Zr1 N13 2.250(3) . ?
Fe1 N1 1.910(3) . ?
Fe1 N3 1.902(3) . ?
Fe1 N4 1.913(3) . ?
Fe1 N6 1.913(3) . ?
Fe1 N2 1.929(3) . ?
Fe1 N5 1.903(3) . ?
O4 N4 1.357(3) . ?
O2 N2 1.360(3) . ?
O3 N3 1.381(3) . ?
O3 B1 1.508(5) . ?
N1 O1 1.383(3) . ?
N1 C1 1.295(4) . ?
O1 B1 1.484(5) . ?
O5 N5 1.385(3) . ?
O5 B1 1.499(5) . ?
N3 C7 1.295(4) . ?
N4 C8 1.312(4) . ?
N11 C42 1.378(4) . ?
N11 C35 1.381(4) . ?
N6 O6 1.354(3) . ?
N6 C14 1.316(4) . ?
N8 C27 1.329(4) . ?
N8 C26 1.327(4) . ?
N9 C27 1.380(4) . ?
N9 C34 1.380(4) . ?
C27 C28 1.457(5) . ?
O8 C57 1.299(5) . ?
N2 C2 1.311(4) . ?
N14 C19 1.326(4) . ?
N14 C50 1.335(4) . ?
N7 C26 1.375(4) . ?
N7 C19 1.378(4) . ?
N12 C42 1.326(4) . ?
N12 C43 1.332(4) . ?
C2 C3 1.492(4) . ?
C2 C1 1.449(5) . ?
O7 C57 1.246(4) . ?
N13 C50 1.367(4) . ?
N13 C43 1.377(4) . ?
C20 C25 1.394(5) . ?
C20 C19 1.448(4) . ?
C20 C21 1.400(5) . ?
C23 C22 1.395(5) . ?
C23 C24 1.390(5) . ?
C5S C6S 1.368(9) . ?
C5S C4S 1.372(10) . ?
C25 C26 1.457(4) . ?
C25 C24 1.400(5) . ?
C6 C1 1.490(5) . ?
C6 C5 1.529(6) . ?
C13 C14 1.444(4) . ?
C13 C18 1.500(5) . ?
C13 N5 1.296(4) . ?
C9 C8 1.490(5) . ?
C9 C10 1.527(5) . ?
C22 C21 1.393(5) . ?
C44 C45 1.394(5) . ?
C44 C43 1.447(5) . ?
C44 C49 1.405(5) . ?
C45 C46 1.391(5) . ?
C12 C11 1.544(5) . ?
C12 C7 1.507(5) . ?
C50 C49 1.452(5) . ?
C36 C41 1.403(5) . ?
C36 C37 1.393(5) . ?
C36 C35 1.453(5) . ?
C32 C33 1.397(5) . ?
C32 C31 1.385(5) . ?
C42 C41 1.456(5) . ?
C12S C7S 1.384(6) . ?
C12S C11S 1.388(6) . ?
C47 C48 1.393(5) . ?
C47 C46 1.402(5) . ?
C51 C56 1.395(5) . ?
C51 C52 1.397(5) . ?
C51 B1 1.596(5) . ?
C2S C1S 1.382(7) . ?
C2S C3S 1.386(7) . ?
C56 C55 1.391(5) . ?
C10S C9S 1.378(7) . ?
C10S C11S 1.386(6) . ?
C38 C37 1.392(5) . ?
C38 C39 1.402(6) . ?
C55 C54 1.381(5) . ?
C8 C7 1.433(5) . ?
C41 C40 1.387(5) . ?
C48 C49 1.391(5) . ?
C40 C39 1.387(5) . ?
C52 C53 1.394(5) . ?
C15 C16 1.529(5) . ?
C15 C14 1.495(5) . ?
C1S C6S 1.385(7) . ?
C7S C8S 1.382(6) . ?
C29 C28 1.393(5) . ?
C29 C30 1.384(5) . ?
C3 C4 1.525(5) . ?
C33 C28 1.403(5) . ?
C33 C34 1.449(5) . ?
C16 C17 1.517(6) . ?
C8S C9S 1.385(7) . ?
C11 C10 1.521(6) . ?
C35 N10 1.334(4) . ?
N10 C34 1.326(4) . ?
C30 C31 1.404(5) . ?
C18 C17 1.528(5) . ?
C53 C54 1.393(5) . ?
C57 C54 1.482(5) . ?
C4 C5 1.485(6) . ?
C3S C4S 1.402(9) . ?
C14S C15S 1.374(11) . ?
C14S C13S 1.383(11) . ?
C15S C16S 1.370(11) . ?
C18S C13S 1.423(14) . ?
C18S C17S 1.311(15) . ?
C17S C16S 1.323(13) . ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.500 0.500 53.2 0.0 ?
2 0.500 0.500 1.000 215.6 49.5 ?
3 0.458 0.208 0.319 7.2 0.0 ?
4 0.542 0.792 0.681 7.2 0.0 ?
