#------------------------------------------------------------------------------
#$Date: 2021-05-05 11:39:17 +0300 (Wed, 05 May 2021) $
#$Revision: 264900 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/69/7706996.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_7706996
loop_
_publ_author_name
'Hamilton, Elizabeth A.'
'Kilpatrick, Alexander F. R.'
'Turner, Zoë R'
'Fraser, Duncan A. X.'
'Buffet, Jean-Charles'
'O'Hare, Dermot'
_publ_section_title
;
 CO₂ activation by permethylpentalene amido zirconium
 complexes.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4494
_journal_page_last               4498
_journal_paper_doi               10.1039/d1dt00770j
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C40 H38 N2 O4 Zr'
_chemical_formula_sum            'C40 H38 N2 O4 Zr'
_chemical_formula_weight         701.94
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-05-20
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2021-03-05 deposited with the CCDC.	2021-03-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.045(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.02400(19)
_cell_length_b                   21.6398(5)
_cell_length_c                   18.9459(5)
_cell_measurement_reflns_used    5678
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      76.0980
_cell_measurement_theta_min      4.6600
_cell_volume                     3679.14(15)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43b (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    "'Superflip (Palatinus and Chapuis, 2007)"
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5035
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -120.00  -6.00   1.00   20.00    --  -41.90 -19.00-120.00  114
  2  ω    -49.00  30.00   1.00   20.00    --  -41.90  37.00  60.00   79
  3  ω     89.00 178.00   1.00   97.50    --  111.00  45.00-180.00   89
  4  ω     41.00  99.00   1.00   97.50    --  111.00 -45.00  90.00   58
  5  ω     40.00  84.00   1.00   97.50    --  111.00 -45.00-150.00   44
  6  ω     87.00 178.00   1.00   97.50    --  111.00  30.00-120.00   91
  7  ω    100.00 177.00   1.00   97.50    --  111.00 111.00  60.00   77
  8  ω     40.00  84.00   1.00   97.50    --  111.00 -45.00   0.00   44
  9  ω     44.00  98.00   1.00   97.50    --  111.00 -45.00  30.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0369068000
_diffrn_orient_matrix_UB_12      -0.0136398000
_diffrn_orient_matrix_UB_13      -0.0797283000
_diffrn_orient_matrix_UB_21      -0.1226933000
_diffrn_orient_matrix_UB_22      -0.0453960000
_diffrn_orient_matrix_UB_23      0.0172545000
_diffrn_orient_matrix_UB_31      -0.1141916000
_diffrn_orient_matrix_UB_32      0.0531362000
_diffrn_orient_matrix_UB_33      -0.0055784000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_unetI/netI     0.0597
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            14982
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.490
_diffrn_reflns_theta_min         6.408
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.771
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74808
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.081
_exptl_crystal_size_min          0.034
_refine_diff_density_max         2.321
_refine_diff_density_min         -2.195
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         7386
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0838
_refine_ls_R_factor_gt           0.0747
_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)+(0.0680P)²+24.9216P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1949
_refine_ls_wR_factor_ref         0.1992
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6272
_reflns_number_total             7386
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt00770j2.cif
_cod_data_source_block           eh-082
_cod_depositor_comments
'Adding full bibliography for 7706993--7706996.cif.'
_cod_original_cell_volume        3679.13(16)
_cod_database_code               7706996
_chemical_oxdiff_formula         'C48 H50 N2 O4 Zr1'
_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   0.912
_shelx_estimated_absorpt_t_min   0.732
_exptl_absorpt_special_details   multi-scan
_reflns_odcompleteness_completeness 98.08
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Me refined with riding coordinates:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,
 H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C)
2.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24), C25(H25),
 C26(H26), C27(H27), C28(H28), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35),
  C37(H37), C38(H38), C39(H39), C40(H40), C41(H41)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.426
_oxdiff_exptl_absorpt_empirical_full_min 0.796
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
C0AA C 0.0434(6) 0.0639(3) 0.0933(3) 0.0193(10) Uani 1 1 d . . . . .
C1AA C 0.1422(6) 0.1149(3) 0.1006(3) 0.0219(11) Uani 1 1 d . . . . .
C3 C 0.2866(6) 0.0959(3) 0.0890(3) 0.0233(11) Uani 1 1 d . . . . .
C4 C 0.2799(6) 0.0315(3) 0.0704(3) 0.0198(11) Uani 1 1 d . . . . .
C2AA C 0.3749(6) -0.0200(3) 0.0915(3) 0.0227(11) Uani 1 1 d . . . . .
C6 C 0.2779(7) -0.0707(3) 0.1000(3) 0.0242(11) Uani 1 1 d . . . . .
C7 C 0.1282(7) -0.0523(3) 0.0902(3) 0.0230(11) Uani 1 1 d . . . . .
C8 C 0.1262(6) 0.0124(3) 0.0710(2) 0.0180(10) Uani 1 1 d . . . . .
C9 C -0.1222(6) 0.0665(3) 0.0981(3) 0.0261(12) Uani 1 1 d . . . . .
H9A H -0.1646 0.0250 0.0911 0.039 Uiso 1 1 calc R . . . .
H9B H -0.1408 0.0820 0.1449 0.039 Uiso 1 1 calc R . . . .
H9C H -0.1687 0.0943 0.0613 0.039 Uiso 1 1 calc R . . . .
C10 C 0.0999(7) 0.1792(3) 0.1205(4) 0.0307(13) Uani 1 1 d . . . . .
H10A H -0.0070 0.1806 0.1256 0.046 Uiso 1 1 calc R . . . .
H10B H 0.1563 0.1907 0.1656 0.046 Uiso 1 1 calc R . . . .
H10C H 0.1227 0.2081 0.0834 0.046 Uiso 1 1 calc R . . . .
C11 C 0.4226(7) 0.1375(3) 0.0915(4) 0.0307(13) Uani 1 1 d . . . . .
H11A H 0.5094 0.1130 0.0816 0.046 Uiso 1 1 calc R . . . .
H11B H 0.4048 0.1702 0.0558 0.046 Uiso 1 1 calc R . . . .
H11C H 0.4413 0.1561 0.1388 0.046 Uiso 1 1 calc R . . . .
C12 C 0.5409(6) -0.0223(3) 0.0959(3) 0.0304(13) Uani 1 1 d . . . . .
H12A H 0.5796 0.0191 0.0880 0.046 Uiso 1 1 calc R . . . .
H12B H 0.5809 -0.0370 0.1431 0.046 Uiso 1 1 calc R . . . .
H12C H 0.5711 -0.0506 0.0596 0.046 Uiso 1 1 calc R . . . .
C13 C 0.3295(7) -0.1355(3) 0.1184(4) 0.0315(13) Uani 1 1 d . . . . .
H13A H 0.4386 -0.1370 0.1225 0.047 Uiso 1 1 calc R . . . .
H13B H 0.2946 -0.1477 0.1636 0.047 Uiso 1 1 calc R . . . .
H13C H 0.2887 -0.1639 0.0810 0.047 Uiso 1 1 calc R . . . .
C15 C -0.0054(7) -0.0940(3) 0.0935(3) 0.0289(13) Uani 1 1 d . . . . .
H15A H -0.0970 -0.0695 0.0847 0.043 Uiso 1 1 calc R . . . .
H15B H -0.0048 -0.1262 0.0572 0.043 Uiso 1 1 calc R . . . .
H15C H -0.0011 -0.1131 0.1405 0.043 Uiso 1 1 calc R . . . .
C16 C 0.3895(6) 0.0960(3) 0.2679(3) 0.0224(11) Uani 1 1 d . . . . .
C17 C 0.3872(6) 0.1823(3) 0.3469(3) 0.0215(11) Uani 1 1 d . . . . .
C18 C 0.3438(7) 0.2380(3) 0.3154(4) 0.0315(13) Uani 1 1 d . . . . .
H18 H 0.3645 0.2469 0.2684 0.038 Uiso 1 1 calc R . . . .
C19 C 0.2697(7) 0.2808(3) 0.3536(4) 0.0387(16) Uani 1 1 d . . . . .
H19 H 0.2377 0.3188 0.3322 0.046 Uiso 1 1 calc R . . . .
C20 C 0.2423(7) 0.2682(4) 0.4223(4) 0.0429(18) Uani 1 1 d . . . . .
H20 H 0.1936 0.2980 0.4486 0.051 Uiso 1 1 calc R . . . .
C21 C 0.2855(8) 0.2124(4) 0.4528(4) 0.0442(18) Uani 1 1 d . . . . .
H21 H 0.2636 0.2033 0.4996 0.053 Uiso 1 1 calc R . . . .
C22 C 0.3608(7) 0.1696(3) 0.4158(3) 0.0330(14) Uani 1 1 d . . . . .
H22 H 0.3938 0.1318 0.4375 0.040 Uiso 1 1 calc R . . . .
C23 C 0.6321(6) 0.1462(3) 0.3137(3) 0.0247(12) Uani 1 1 d . . . . .
C24 C 0.6942(7) 0.1954(3) 0.3534(4) 0.0322(14) Uani 1 1 d . . . . .
H24 H 0.6324 0.2229 0.3762 0.039 Uiso 1 1 calc R . . . .
C25 C 0.8480(7) 0.2040(3) 0.3595(4) 0.0350(15) Uani 1 1 d . . . . .
H25 H 0.8895 0.2377 0.3870 0.042 Uiso 1 1 calc R . . . .
C26 C 0.9404(7) 0.1664(4) 0.3280(4) 0.0372(15) Uani 1 1 d . . . . .
H26 H 1.0453 0.1721 0.3345 0.045 Uiso 1 1 calc R . . . .
C27 C 0.8769(7) 0.1192(4) 0.2857(5) 0.050(2) Uani 1 1 d . . . . .
H27 H 0.9388 0.0937 0.2605 0.060 Uiso 1 1 calc R . . . .
C28 C 0.7238(8) 0.1083(4) 0.2795(5) 0.049(2) Uani 1 1 d . . . . .
H28 H 0.6828 0.0747 0.2517 0.059 Uiso 1 1 calc R . . . .
C29 C 0.1053(6) -0.0540(3) 0.2663(3) 0.0197(10) Uani 1 1 d . . . . .
C30 C 0.1403(6) -0.1429(3) 0.3405(3) 0.0235(11) Uani 1 1 d . . . . .
C31 C 0.1903(8) -0.1315(4) 0.4101(4) 0.0405(16) Uani 1 1 d . . . . .
H31 H 0.1635 -0.0946 0.4328 0.049 Uiso 1 1 calc R . . . .
C32 C 0.2821(10) -0.1758(5) 0.4472(5) 0.057(2) Uani 1 1 d . . . . .
H32 H 0.3192 -0.1685 0.4952 0.069 Uiso 1 1 calc R . . . .
C33 C 0.3185(9) -0.2291(4) 0.4146(5) 0.057(3) Uani 1 1 d . . . . .
H33 H 0.3780 -0.2593 0.4407 0.069 Uiso 1 1 calc R . . . .
C34 C 0.2700(9) -0.2394(4) 0.3451(5) 0.050(2) Uani 1 1 d . . . . .
H34 H 0.2991 -0.2759 0.3222 0.060 Uiso 1 1 calc R . . . .
C35 C 0.1774(7) -0.1963(3) 0.3074(4) 0.0326(14) Uani 1 1 d . . . . .
H35 H 0.1404 -0.2039 0.2594 0.039 Uiso 1 1 calc R . . . .
C36 C -0.1170(6) -0.1072(3) 0.3059(3) 0.0211(11) Uani 1 1 d . . . . .
C37 C -0.1645(6) -0.1581(3) 0.3409(3) 0.0272(12) Uani 1 1 d . . . . .
H37 H -0.0936 -0.1870 0.3617 0.033 Uiso 1 1 calc R . . . .
C38 C -0.3153(7) -0.1676(3) 0.3461(4) 0.0323(14) Uani 1 1 d . . . . .
H38 H -0.3460 -0.2032 0.3701 0.039 Uiso 1 1 calc R . . . .
C39 C -0.4214(6) -0.1262(3) 0.3171(4) 0.0338(14) Uani 1 1 d . . . . .
H39 H -0.5242 -0.1322 0.3217 0.041 Uiso 1 1 calc R . . . .
C40 C -0.3735(8) -0.0764(4) 0.2816(5) 0.046(2) Uani 1 1 d . . . . .
H40 H -0.4449 -0.0478 0.2607 0.056 Uiso 1 1 calc R . . . .
C41 C -0.2232(8) -0.0662(3) 0.2750(4) 0.0395(16) Uani 1 1 d . . . . .
H41 H -0.1934 -0.0314 0.2494 0.047 Uiso 1 1 calc R . . . .
N1 N 0.4720(5) 0.1390(2) 0.3086(3) 0.0230(10) Uani 1 1 d . . . . .
N2 N 0.0393(5) -0.0992(2) 0.3024(2) 0.0203(9) Uani 1 1 d . . . . .
O1 O 0.2486(4) 0.09639(19) 0.2673(2) 0.0224(8) Uani 1 1 d . . . . .
O2 O 0.4503(4) 0.05623(18) 0.2307(2) 0.0192(8) Uani 1 1 d . . . . .
O3 O 0.2468(4) -0.05383(18) 0.2656(2) 0.0199(8) Uani 1 1 d . . . . .
O4 O 0.0294(4) -0.01230(17) 0.2306(2) 0.0199(8) Uani 1 1 d . . . . .
Zr1 Zr 0.22974(4) 0.02173(2) 0.18357(2) 0.01588(15) Uani 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -0.1862 2.2449 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-6 -1 1 0.0525
6 1 -1 0.0525
0 -14 0 0.0151
-1 14 0 0.0164
4 -10 -2 0.0434
-4 10 2 0.0434
0 9 9 0.0183
0 -9 -9 0.0161
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
C1AA C0AA C8 107.0(5) . . ?
C1AA C0AA C9 125.7(5) . . ?
C1AA C0AA Zr1 80.9(3) . . ?
C8 C0AA C9 126.8(5) . . ?
C8 C0AA Zr1 64.7(3) . . ?
C9 C0AA Zr1 125.8(4) . . ?
C0AA C1AA C10 124.9(5) . . ?
C0AA C1AA Zr1 66.9(3) . . ?
C3 C1AA C0AA 110.0(5) . . ?
C3 C1AA C10 125.1(5) . . ?
C3 C1AA Zr1 69.2(3) . . ?
C10 C1AA Zr1 129.0(4) . . ?
C1AA C3 C4 107.8(5) . . ?
C1AA C3 C11 125.6(5) . . ?
C1AA C3 Zr1 79.1(3) . . ?
C4 C3 C11 126.5(5) . . ?
C4 C3 Zr1 63.0(3) . . ?
C11 C3 Zr1 125.7(4) . . ?
C3 C4 C8 106.8(5) . . ?
C3 C4 Zr1 82.2(3) . . ?
C2AA C4 C3 132.5(5) . . ?
C2AA C4 C8 108.6(5) . . ?
C2AA C4 Zr1 80.5(3) . . ?
C8 C4 Zr1 71.1(3) . . ?
C4 C2AA C12 127.4(6) . . ?
C4 C2AA Zr1 64.3(3) . . ?
C6 C2AA C4 105.9(5) . . ?
C6 C2AA C12 126.4(6) . . ?
C6 C2AA Zr1 79.8(3) . . ?
C12 C2AA Zr1 125.4(4) . . ?
C2AA C6 C13 124.4(5) . . ?
C2AA C6 Zr1 67.8(3) . . ?
C7 C6 C2AA 111.3(5) . . ?
C7 C6 C13 124.4(5) . . ?
C7 C6 Zr1 69.1(3) . . ?
C13 C6 Zr1 129.7(4) . . ?
C6 C7 C8 107.1(5) . . ?
C6 C7 C15 126.0(5) . . ?
C6 C7 Zr1 79.1(3) . . ?
C8 C7 C15 126.8(5) . . ?
C8 C7 Zr1 63.2(3) . . ?
C15 C7 Zr1 126.2(4) . . ?
C0AA C8 C4 108.1(5) . . ?
C0AA C8 C7 132.3(5) . . ?
C0AA C8 Zr1 80.1(3) . . ?
C4 C8 Zr1 71.3(3) . . ?
C7 C8 C4 107.0(5) . . ?
C7 C8 Zr1 81.6(3) . . ?
C0AA C9 H9A 109.5 . . ?
C0AA C9 H9B 109.5 . . ?
C0AA C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C1AA C10 H10A 109.5 . . ?
C1AA C10 H10B 109.5 . . ?
C1AA C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C3 C11 H11A 109.5 . . ?
C3 C11 H11B 109.5 . . ?
C3 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C2AA C12 H12A 109.5 . . ?
C2AA C12 H12B 109.5 . . ?
C2AA C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C6 C13 H13A 109.5 . . ?
C6 C13 H13B 109.5 . . ?
C6 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C7 C15 H15A 109.5 . . ?
C7 C15 H15B 109.5 . . ?
C7 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N1 C16 Zr1 175.4(4) . . ?
O1 C16 N1 118.9(5) . . ?
O1 C16 O2 119.2(5) . . ?
O1 C16 Zr1 60.5(3) . . ?
O2 C16 N1 121.9(5) . . ?
O2 C16 Zr1 58.9(3) . . ?
C18 C17 N1 119.1(5) . . ?
C22 C17 C18 120.9(6) . . ?
C22 C17 N1 119.8(5) . . ?
C17 C18 H18 120.5 . . ?
C17 C18 C19 119.1(7) . . ?
C19 C18 H18 120.5 . . ?
C18 C19 H19 119.8 . . ?
C20 C19 C18 120.3(7) . . ?
C20 C19 H19 119.8 . . ?
C19 C20 H20 120.1 . . ?
C21 C20 C19 119.8(6) . . ?
C21 C20 H20 120.1 . . ?
C20 C21 H21 119.7 . . ?
C20 C21 C22 120.5(7) . . ?
C22 C21 H21 119.7 . . ?
C17 C22 C21 119.3(7) . . ?
C17 C22 H22 120.4 . . ?
C21 C22 H22 120.4 . . ?
C24 C23 N1 117.5(5) . . ?
C28 C23 C24 119.0(6) . . ?
C28 C23 N1 123.5(5) . . ?
C23 C24 H24 120.4 . . ?
C23 C24 C25 119.3(6) . . ?
C25 C24 H24 120.4 . . ?
C24 C25 H25 118.7 . . ?
C26 C25 C24 122.7(6) . . ?
C26 C25 H25 118.7 . . ?
C25 C26 H26 121.2 . . ?
C25 C26 C27 117.6(6) . . ?
C27 C26 H26 121.2 . . ?
C26 C27 H27 119.4 . . ?
C26 C27 C28 121.3(7) . . ?
C28 C27 H27 119.4 . . ?
C23 C28 C27 120.0(6) . . ?
C23 C28 H28 120.0 . . ?
C27 C28 H28 120.0 . . ?
N2 C29 Zr1 172.4(4) . . ?
O3 C29 N2 119.7(5) . . ?
O3 C29 O4 118.2(5) . . ?
O3 C29 Zr1 59.9(3) . . ?
O4 C29 N2 122.1(5) . . ?
O4 C29 Zr1 58.7(3) . . ?
C31 C30 C35 121.3(6) . . ?
C31 C30 N2 119.2(6) . . ?
C35 C30 N2 119.5(6) . . ?
C30 C31 H31 120.8 . . ?
C30 C31 C32 118.3(8) . . ?
C32 C31 H31 120.8 . . ?
C31 C32 H32 119.7 . . ?
C33 C32 C31 120.6(8) . . ?
C33 C32 H32 119.7 . . ?
C32 C33 H33 119.8 . . ?
C34 C33 C32 120.5(7) . . ?
C34 C33 H33 119.8 . . ?
C33 C34 H34 120.0 . . ?
C33 C34 C35 119.9(8) . . ?
C35 C34 H34 120.0 . . ?
C30 C35 C34 119.4(7) . . ?
C30 C35 H35 120.3 . . ?
C34 C35 H35 120.3 . . ?
C37 C36 C41 118.5(5) . . ?
C37 C36 N2 118.5(5) . . ?
C41 C36 N2 122.9(5) . . ?
C36 C37 H37 119.7 . . ?
C36 C37 C38 120.6(5) . . ?
C38 C37 H37 119.7 . . ?
C37 C38 H38 119.4 . . ?
C39 C38 C37 121.2(6) . . ?
C39 C38 H38 119.4 . . ?
C38 C39 H39 121.1 . . ?
C40 C39 C38 117.7(6) . . ?
C40 C39 H39 121.1 . . ?
C39 C40 H40 119.0 . . ?
C39 C40 C41 122.1(6) . . ?
C41 C40 H40 119.0 . . ?
C36 C41 C40 119.8(6) . . ?
C36 C41 H41 120.1 . . ?
C40 C41 H41 120.1 . . ?
C16 N1 C17 115.7(4) . . ?
C16 N1 C23 126.0(5) . . ?
C23 N1 C17 118.2(4) . . ?
C29 N2 C30 115.6(4) . . ?
C29 N2 C36 126.5(5) . . ?
C36 N2 C30 118.0(5) . . ?
C16 O1 Zr1 90.2(3) . . ?
C16 O2 Zr1 91.7(3) . . ?
C29 O3 Zr1 90.7(3) . . ?
C29 O4 Zr1 91.9(3) . . ?
C0AA Zr1 C3 55.69(17) . . ?
C0AA Zr1 C2AA 91.10(18) . . ?
C0AA Zr1 C7 64.44(19) . . ?
C0AA Zr1 C16 119.73(18) . . ?
C0AA Zr1 C29 110.36(17) . . ?
C3 Zr1 C16 84.30(18) . . ?
C3 Zr1 C29 166.04(17) . . ?
C4 Zr1 C0AA 59.35(18) . . ?
C4 Zr1 C3 34.7(2) . . ?
C4 Zr1 C2AA 35.2(2) . . ?
C4 Zr1 C7 58.58(19) . . ?
C4 Zr1 C16 111.99(19) . . ?
C4 Zr1 C29 140.96(19) . . ?
C4 Zr1 O1 126.52(18) . . ?
C4 Zr1 O3 136.17(18) . . ?
C2AA Zr1 C3 64.1(2) . . ?
C2AA Zr1 C7 56.19(19) . . ?
C2AA Zr1 C16 111.18(18) . . ?
C2AA Zr1 C29 119.42(19) . . ?
C7 Zr1 C3 89.54(19) . . ?
C7 Zr1 C16 167.36(18) . . ?
C7 Zr1 C29 82.68(17) . . ?
C8 Zr1 C0AA 35.17(19) . . ?
C8 Zr1 C3 58.19(19) . . ?
C8 Zr1 C4 37.61(19) . . ?
C8 Zr1 C2AA 59.54(18) . . ?
C8 Zr1 C7 35.11(19) . . ?
C8 Zr1 C16 142.10(19) . . ?
C8 Zr1 C29 110.65(18) . . ?
C8 Zr1 O1 136.43(18) . . ?
C8 Zr1 O3 125.61(17) . . ?
C16 Zr1 C29 105.46(17) . . ?
O1 Zr1 C0AA 102.70(17) . . ?
O1 Zr1 C3 92.19(18) . . ?
O1 Zr1 C2AA 138.96(17) . . ?
O1 Zr1 C7 162.70(17) . . ?
O1 Zr1 C16 29.32(16) . . ?
O1 Zr1 C29 91.89(16) . . ?
O2 Zr1 C0AA 132.54(16) . . ?
O2 Zr1 C3 80.20(16) . . ?
O2 Zr1 C4 95.16(17) . . ?
O2 Zr1 C2AA 83.53(16) . . ?
O2 Zr1 C7 138.50(17) . . ?
O2 Zr1 C8 132.62(17) . . ?
O2 Zr1 C16 29.36(16) . . ?
O2 Zr1 C29 113.22(15) . . ?
O2 Zr1 O1 58.62(13) . . ?
O2 Zr1 O3 88.46(14) . . ?
O3 Zr1 C0AA 138.29(16) . . ?
O3 Zr1 C3 163.32(16) . . ?
O3 Zr1 C2AA 102.71(17) . . ?
O3 Zr1 C7 90.95(17) . . ?
O3 Zr1 C16 91.82(16) . . ?
O3 Zr1 C29 29.42(15) . . ?
O3 Zr1 O1 92.29(15) . . ?
O4 Zr1 C0AA 82.87(15) . . ?
O4 Zr1 C3 137.47(16) . . ?
O4 Zr1 C4 131.85(17) . . ?
O4 Zr1 C2AA 132.70(17) . . ?
O4 Zr1 C7 79.46(17) . . ?
O4 Zr1 C8 94.36(17) . . ?
O4 Zr1 C16 112.42(16) . . ?
O4 Zr1 C29 29.49(15) . . ?
O4 Zr1 O1 87.71(14) . . ?
O4 Zr1 O2 132.98(14) . . ?
O4 Zr1 O3 58.80(13) . . ?
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
C0AA C1AA 1.415(8) . ?
C0AA C8 1.430(8) . ?
C0AA C9 1.508(7) . ?
C0AA Zr1 2.446(5) . ?
C1AA C3 1.405(8) . ?
C1AA C10 1.502(8) . ?
C1AA Zr1 2.626(6) . ?
C3 C4 1.438(8) . ?
C3 C11 1.519(7) . ?
C3 Zr1 2.499(6) . ?
C4 C2AA 1.437(8) . ?
C4 C8 1.449(7) . ?
C4 Zr1 2.248(5) . ?
C2AA C6 1.422(8) . ?
C2AA C12 1.492(7) . ?
C2AA Zr1 2.460(5) . ?
C6 C7 1.402(8) . ?
C6 C13 1.507(8) . ?
C6 Zr1 2.614(6) . ?
C7 C8 1.446(8) . ?
C7 C15 1.512(8) . ?
C7 Zr1 2.488(5) . ?
C8 Zr1 2.246(5) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 N1 1.376(8) . ?
C16 O1 1.270(7) . ?
C16 O2 1.273(7) . ?
C16 Zr1 2.594(6) . ?
C17 C18 1.382(9) . ?
C17 C22 1.378(9) . ?
C17 N1 1.452(7) . ?
C18 H18 0.9500 . ?
C18 C19 1.389(9) . ?
C19 H19 0.9500 . ?
C19 C20 1.377(12) . ?
C20 H20 0.9500 . ?
C20 C21 1.377(12) . ?
C21 H21 0.9500 . ?
C21 C22 1.383(10) . ?
C22 H22 0.9500 . ?
C23 C24 1.388(8) . ?
C23 C28 1.374(9) . ?
C23 N1 1.446(7) . ?
C24 H24 0.9500 . ?
C24 C25 1.393(8) . ?
C25 H25 0.9500 . ?
C25 C26 1.349(10) . ?
C26 H26 0.9500 . ?
C26 C27 1.385(10) . ?
C27 H27 0.9500 . ?
C27 C28 1.394(9) . ?
C28 H28 0.9500 . ?
C29 N2 1.366(8) . ?
C29 O3 1.278(6) . ?
C29 O4 1.281(7) . ?
C29 Zr1 2.601(6) . ?
C30 C31 1.372(9) . ?
C30 C35 1.372(9) . ?
C30 N2 1.451(7) . ?
C31 H31 0.9500 . ?
C31 C32 1.405(10) . ?
C32 H32 0.9500 . ?
C32 C33 1.366(14) . ?
C33 H33 0.9500 . ?
C33 C34 1.362(14) . ?
C34 H34 0.9500 . ?
C34 C35 1.398(10) . ?
C35 H35 0.9500 . ?
C36 C37 1.378(8) . ?
C36 C41 1.388(9) . ?
C36 N2 1.430(7) . ?
C37 H37 0.9500 . ?
C37 C38 1.389(8) . ?
C38 H38 0.9500 . ?
C38 C39 1.383(9) . ?
C39 H39 0.9500 . ?
C39 C40 1.364(10) . ?
C40 H40 0.9500 . ?
C40 C41 1.393(10) . ?
C41 H41 0.9500 . ?
O1 Zr1 2.258(4) . ?
O2 Zr1 2.223(3) . ?
O3 Zr1 2.251(4) . ?
O4 Zr1 2.223(4) . ?
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
C0AA C1AA C3 C4 2.7(6) . . . . ?
C0AA C1AA C3 C11 179.4(5) . . . . ?
C0AA C1AA C3 Zr1 -54.2(4) . . . . ?
C1AA C0AA C8 C4 4.5(6) . . . . ?
C1AA C0AA C8 C7 139.9(6) . . . . ?
C1AA C0AA C8 Zr1 70.9(4) . . . . ?
C1AA C3 C4 C2AA -136.7(6) . . . . ?
C1AA C3 C4 C8 0.2(6) . . . . ?
C1AA C3 C4 Zr1 -67.3(4) . . . . ?
C3 C4 C2AA C6 140.2(6) . . . . ?
C3 C4 C2AA C12 -46.0(9) . . . . ?
C3 C4 C2AA Zr1 70.2(6) . . . . ?
C3 C4 C8 C0AA -2.9(6) . . . . ?
C3 C4 C8 C7 -150.1(5) . . . . ?
C3 C4 C8 Zr1 -75.3(4) . . . . ?
C4 C2AA C6 C7 -4.2(6) . . . . ?
C4 C2AA C6 C13 176.7(5) . . . . ?
C4 C2AA C6 Zr1 -59.4(3) . . . . ?
C2AA C4 C8 C0AA 145.0(5) . . . . ?
C2AA C4 C8 C7 -2.2(6) . . . . ?
C2AA C4 C8 Zr1 72.6(4) . . . . ?
C2AA C6 C7 C8 2.9(6) . . . . ?
C2AA C6 C7 C15 178.4(5) . . . . ?
C2AA C6 C7 Zr1 -54.5(4) . . . . ?
C6 C7 C8 C0AA -136.2(6) . . . . ?
C6 C7 C8 C4 -0.4(6) . . . . ?
C6 C7 C8 Zr1 -67.9(4) . . . . ?
C8 C0AA C1AA C3 -4.5(6) . . . . ?
C8 C0AA C1AA C10 177.6(5) . . . . ?
C8 C0AA C1AA Zr1 -60.0(3) . . . . ?
C8 C4 C2AA C6 3.8(6) . . . . ?
C8 C4 C2AA C12 177.6(5) . . . . ?
C8 C4 C2AA Zr1 -66.2(3) . . . . ?
C9 C0AA C1AA C3 -176.6(5) . . . . ?
C9 C0AA C1AA C10 5.5(9) . . . . ?
C9 C0AA C1AA Zr1 127.9(6) . . . . ?
C9 C0AA C8 C4 176.6(5) . . . . ?
C9 C0AA C8 C7 -48.0(9) . . . . ?
C9 C0AA C8 Zr1 -117.0(5) . . . . ?
C10 C1AA C3 C4 -179.4(5) . . . . ?
C10 C1AA C3 C11 -2.7(9) . . . . ?
C10 C1AA C3 Zr1 123.7(6) . . . . ?
C11 C3 C4 C2AA 46.6(9) . . . . ?
C11 C3 C4 C8 -176.5(5) . . . . ?
C11 C3 C4 Zr1 116.0(6) . . . . ?
C12 C2AA C6 C7 -178.1(5) . . . . ?
C12 C2AA C6 C13 2.8(9) . . . . ?
C12 C2AA C6 Zr1 126.7(6) . . . . ?
C13 C6 C7 C8 -178.0(5) . . . . ?
C13 C6 C7 C15 -2.5(9) . . . . ?
C13 C6 C7 Zr1 124.6(6) . . . . ?
C15 C7 C8 C0AA 48.3(9) . . . . ?
C15 C7 C8 C4 -175.9(5) . . . . ?
C15 C7 C8 Zr1 116.7(5) . . . . ?
C17 C18 C19 C20 1.2(10) . . . . ?
C18 C17 C22 C21 2.1(9) . . . . ?
C18 C17 N1 C16 -91.8(7) . . . . ?
C18 C17 N1 C23 85.6(7) . . . . ?
C18 C19 C20 C21 -1.5(11) . . . . ?
C19 C20 C21 C22 2.1(11) . . . . ?
C20 C21 C22 C17 -2.4(11) . . . . ?
C22 C17 C18 C19 -1.5(9) . . . . ?
C22 C17 N1 C16 93.0(6) . . . . ?
C22 C17 N1 C23 -89.5(7) . . . . ?
C23 C24 C25 C26 0.3(12) . . . . ?
C24 C23 C28 C27 0.7(13) . . . . ?
C24 C23 N1 C16 175.2(6) . . . . ?
C24 C23 N1 C17 -2.0(8) . . . . ?
C24 C25 C26 C27 2.7(12) . . . . ?
C25 C26 C27 C28 -4.0(14) . . . . ?
C26 C27 C28 C23 2.4(15) . . . . ?
C28 C23 C24 C25 -2.0(11) . . . . ?
C28 C23 N1 C16 -2.5(10) . . . . ?
C28 C23 N1 C17 -179.7(7) . . . . ?
C30 C31 C32 C33 -1.0(13) . . . . ?
C31 C30 C35 C34 -1.2(10) . . . . ?
C31 C30 N2 C29 91.9(7) . . . . ?
C31 C30 N2 C36 -88.1(7) . . . . ?
C31 C32 C33 C34 2.0(14) . . . . ?
C32 C33 C34 C35 -2.6(12) . . . . ?
C33 C34 C35 C30 2.2(11) . . . . ?
C35 C30 C31 C32 0.6(11) . . . . ?
C35 C30 N2 C29 -91.7(7) . . . . ?
C35 C30 N2 C36 88.4(7) . . . . ?
C36 C37 C38 C39 -0.6(11) . . . . ?
C37 C36 C41 C40 1.8(11) . . . . ?
C37 C36 N2 C29 175.5(6) . . . . ?
C37 C36 N2 C30 -4.5(8) . . . . ?
C37 C38 C39 C40 1.6(12) . . . . ?
C38 C39 C40 C41 -0.9(13) . . . . ?
C39 C40 C41 C36 -0.8(14) . . . . ?
C41 C36 C37 C38 -1.1(10) . . . . ?
C41 C36 N2 C29 -3.7(10) . . . . ?
C41 C36 N2 C30 176.2(6) . . . . ?
N1 C16 O1 Zr1 174.8(5) . . . . ?
N1 C16 O2 Zr1 -174.7(5) . . . . ?
N1 C17 C18 C19 -176.6(5) . . . . ?
N1 C17 C22 C21 177.2(6) . . . . ?
N1 C23 C24 C25 -179.8(6) . . . . ?
N1 C23 C28 C27 178.4(8) . . . . ?
N2 C29 O3 Zr1 171.2(5) . . . . ?
N2 C29 O4 Zr1 -171.1(5) . . . . ?
N2 C30 C31 C32 176.9(7) . . . . ?
N2 C30 C35 C34 -177.5(6) . . . . ?
N2 C36 C37 C38 179.6(6) . . . . ?
N2 C36 C41 C40 -179.0(7) . . . . ?
O1 C16 N1 C17 -0.9(8) . . . . ?
O1 C16 N1 C23 -178.1(5) . . . . ?
O1 C16 O2 Zr1 4.9(5) . . . . ?
O2 C16 N1 C17 178.7(5) . . . . ?
O2 C16 N1 C23 1.5(9) . . . . ?
O2 C16 O1 Zr1 -4.9(5) . . . . ?
O3 C29 N2 C30 2.6(7) . . . . ?
O3 C29 N2 C36 -177.4(5) . . . . ?
O3 C29 O4 Zr1 6.6(5) . . . . ?
O4 C29 N2 C30 -179.8(5) . . . . ?
O4 C29 N2 C36 0.2(9) . . . . ?
O4 C29 O3 Zr1 -6.5(5) . . . . ?
Zr1 C0AA C1AA C3 55.5(4) . . . . ?
Zr1 C0AA C1AA C10 -122.4(6) . . . . ?
Zr1 C0AA C8 C4 -66.4(3) . . . . ?
Zr1 C0AA C8 C7 69.0(5) . . . . ?
Zr1 C1AA C3 C4 56.9(4) . . . . ?
Zr1 C1AA C3 C11 -126.4(6) . . . . ?
Zr1 C3 C4 C2AA -69.4(6) . . . . ?
Zr1 C3 C4 C8 67.5(3) . . . . ?
Zr1 C4 C2AA C6 70.1(4) . . . . ?
Zr1 C4 C2AA C12 -116.2(6) . . . . ?
Zr1 C4 C8 C0AA 72.4(4) . . . . ?
Zr1 C4 C8 C7 -74.7(3) . . . . ?
Zr1 C2AA C6 C7 55.2(4) . . . . ?
Zr1 C2AA C6 C13 -123.9(6) . . . . ?
Zr1 C6 C7 C8 57.4(3) . . . . ?
Zr1 C6 C7 C15 -127.1(6) . . . . ?
Zr1 C7 C8 C0AA -68.4(5) . . . . ?
Zr1 C7 C8 C4 67.4(3) . . . . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-6.0000 -1.0000 1.0003 0.1553 0.7988 0.6264
6.0000 1.0000 -1.0003 -0.1553 -0.7988 -0.6264
-0.0000 -14.0000 -0.0000 0.1910 0.6355 -0.7439
-1.0000 14.0000 0.0001 -0.1541 -0.5129 0.8581
4.0000 -10.0000 -2.0002 0.1482 -0.0713 -0.9770
-4.0000 10.0000 2.0002 -0.1482 0.0713 0.9770
0.0000 9.0000 9.0000 -0.8403 -0.2533 0.4280
-0.0000 -9.0000 -9.0000 0.8403 0.2533 -0.4280
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 -0.698 0.000 0.500 252.0 68.9 ?
2 -0.102 0.500 0.000 252.0 68.9 ?
