#------------------------------------------------------------------------------
#$Date: 2024-12-06 20:35:58 +0200 (Fri, 06 Dec 2024) $
#$Revision: 296544 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/70/7717046.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_7717046
loop_
_publ_author_name
'Mitsuhashi, Ryoji'
'Imai, Yuya'
'Sugiarto, ?'
'Sakiyama, Hiroshi'
'Kikukawa, Yuji'
'Hayashi, Yoshihito'
_publ_section_title
;
 Controlling the symmetry of hexamonodentate 3d-transition metal complexes
 through symmetry propagation from high-symmetry Ti-Mo and Zr-Mo clusters
 via hydrogen-bonding interactions.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16186
_journal_page_last               16194
_journal_paper_doi               10.1039/d4dt02120g
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C36 H90 Mo6 N18 O18 Zr, H12 Ni O6, 6(Cl O4)'
_chemical_formula_sum            'C36 H102 Cl6 Mo6 N18 Ni O48 Zr'
_chemical_formula_weight         2493.62
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3 :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-07-22 deposited with the CCDC.	2024-09-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   21.7869(4)
_cell_length_b                   21.7869(4)
_cell_length_c                   14.6803(3)
_cell_measurement_reflns_used    6994
_cell_measurement_temperature    102(2)
_cell_measurement_theta_max      30.0500
_cell_measurement_theta_min      2.5660
_cell_volume                     6034.7(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      102(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0194
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8842
_diffrn_reflns_point_group_measured_fraction_full 0.892
_diffrn_reflns_point_group_measured_fraction_max 0.869
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_min         2.566
_exptl_absorpt_coefficient_mu    1.566
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97140
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.43a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale green'
_exptl_crystal_density_diffrn    2.058
_exptl_crystal_description       plate
_exptl_crystal_F_000             3750
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.759
_refine_diff_density_min         -2.051
_refine_diff_density_rms         0.126
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.00(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         5351
_refine_ls_number_restraints     202
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0337
_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)+(0.0499P)²+39.1925P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0897
_refine_ls_wR_factor_ref         0.0902
_reflns_Friedel_coverage         0.746
_reflns_Friedel_fraction_full    0.785
_reflns_Friedel_fraction_max     0.742
_reflns_number_gt                5241
_reflns_number_total             5351
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt02120g2.cif
_cod_data_source_block           NiZrMo6
_cod_depositor_comments
'Adding full bibliography for 7717042--7717049.cif.'
_cod_original_cell_volume        6034.7(3)
_cod_database_code               7717046
_shelx_shelxl_version_number     2018/3
_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_min   0.885
_shelx_estimated_absorpt_t_max   0.940
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
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 0.333333 0.666667 0.67934(8) 0.0115(2) Uani 1 3 d S T P . .
Mo1 Mo 0.48004(3) 0.74110(3) 0.52295(4) 0.01326(13) Uani 1 1 d . . . . .
O1 O 0.4140(3) 0.7409(3) 0.5986(4) 0.0176(10) Uani 1 1 d . . . . .
O2 O 0.4357(3) 0.6880(3) 0.4317(4) 0.0207(11) Uani 1 1 d D . . . .
O3 O 0.5164(3) 0.6995(3) 0.5812(4) 0.0198(11) Uani 1 1 d . . . . .
N1 N 0.4762(3) 0.8338(3) 0.4505(4) 0.0174(12) Uani 1 1 d . . . . .
H1 H 0.427448 0.814517 0.424744 0.021 Uiso 1 1 calc R U . . .
C1 C 0.5272(4) 0.8657(4) 0.3741(6) 0.0254(16) Uani 1 1 d . . . . .
H1A H 0.565458 0.913555 0.391797 0.030 Uiso 1 1 calc R U . . .
H1B H 0.502557 0.870812 0.320379 0.030 Uiso 1 1 calc R U . . .
C2 C 0.5588(4) 0.8202(4) 0.3495(5) 0.0240(16) Uani 1 1 d . . . . .
H2 H 0.524365 0.778856 0.313236 0.029 Uiso 1 1 calc R U . . .
H2A H 0.601975 0.847803 0.312298 0.029 Uiso 1 1 calc R U . . .
N2 N 0.5769(3) 0.7954(3) 0.4353(4) 0.0199(13) Uani 1 1 d . . . . .
H2B H 0.588672 0.758286 0.416873 0.024 Uiso 1 1 calc R U . . .
C3 C 0.6410(4) 0.8524(5) 0.4799(6) 0.0278(17) Uani 1 1 d . . . . .
H3 H 0.652640 0.898625 0.452747 0.033 Uiso 1 1 calc R U . . .
H3A H 0.681448 0.844724 0.468740 0.033 Uiso 1 1 calc R U . . .
C4 C 0.6303(4) 0.8545(5) 0.5807(6) 0.0252(17) Uani 1 1 d . . . . .
H4 H 0.634856 0.816424 0.611333 0.030 Uiso 1 1 calc R U . . .
H4A H 0.666829 0.900592 0.605957 0.030 Uiso 1 1 calc R U . . .
N3 N 0.5582(3) 0.8444(3) 0.5971(4) 0.0174(12) Uani 1 1 d . . . . .
H3B H 0.548489 0.835137 0.663809 0.021 Uiso 1 1 calc R U . . .
C5 C 0.5527(4) 0.9078(4) 0.5758(5) 0.0247(16) Uani 1 1 d . . . . .
H5 H 0.594755 0.941882 0.540449 0.030 Uiso 1 1 calc R U . . .
H5A H 0.551539 0.931174 0.633063 0.030 Uiso 1 1 calc R U . . .
C6 C 0.4860(4) 0.8872(4) 0.5211(6) 0.0234(16) Uani 1 1 d . . . . .
H6 H 0.444477 0.867082 0.562271 0.028 Uiso 1 1 calc R U . . .
H6A H 0.489803 0.929729 0.491448 0.028 Uiso 1 1 calc R U . . .
Mo2 Mo 0.47932(3) 0.71103(3) 0.84027(4) 0.01518(14) Uani 1 1 d . . . . .
O4 O 0.4082(3) 0.6616(3) 0.7617(4) 0.0193(11) Uani 1 1 d . . . . .
O5 O 0.4434(3) 0.7316(3) 0.9323(4) 0.0232(12) Uani 1 1 d . . . . .
O6 O 0.5355(3) 0.7894(3) 0.7866(4) 0.0216(11) Uani 1 1 d . . . . .
N4 N 0.4448(3) 0.6030(3) 0.9111(4) 0.0206(13) Uani 1 1 d . . . . .
H4B H 0.392328 0.579245 0.920222 0.025 Uiso 1 1 calc R U . . .
C7 C 0.4772(5) 0.6187(5) 1.0021(6) 0.0315(19) Uani 1 1 d . . . . .
H7A H 0.469776 0.574297 1.030775 0.038 Uiso 1 1 calc R U . . .
H7B H 0.454233 0.638530 1.040973 0.038 Uiso 1 1 calc R U . . .
C8 C 0.5538(5) 0.6698(5) 0.9958(6) 0.0317(19) Uani 1 1 d . . . . .
H8A H 0.578967 0.644066 0.979141 0.038 Uiso 1 1 calc R U . . .
H8B H 0.571360 0.691685 1.056310 0.038 Uiso 1 1 calc R U . . .
N5 N 0.5710(4) 0.7266(3) 0.9277(5) 0.0215(13) Uani 1 1 d . . . . .
H5B H 0.587763 0.771879 0.962126 0.026 Uiso 1 1 calc R U . . .
C9 C 0.6294(4) 0.7369(5) 0.8657(7) 0.0316(19) Uani 1 1 d . . . . .
H9A H 0.669219 0.740034 0.901919 0.038 Uiso 1 1 calc R U . . .
H9B H 0.646971 0.781810 0.831608 0.038 Uiso 1 1 calc R U . . .
C10 C 0.6034(4) 0.6754(5) 0.7990(6) 0.0281(18) Uani 1 1 d . . . . .
H10A H 0.637048 0.688579 0.747514 0.034 Uiso 1 1 calc R U . . .
H10B H 0.600470 0.633608 0.829813 0.034 Uiso 1 1 calc R U . . .
N6 N 0.5333(4) 0.6580(3) 0.7648(5) 0.0211(13) Uani 1 1 d . . . . .
H6B H 0.539775 0.674633 0.700208 0.025 Uiso 1 1 calc R U . . .
C11 C 0.4816(5) 0.5794(4) 0.7636(6) 0.0323(19) Uani 1 1 d . . . . .
H11A H 0.439774 0.569550 0.726327 0.039 Uiso 1 1 calc R U . . .
H11B H 0.504302 0.554333 0.735713 0.039 Uiso 1 1 calc R U . . .
C12 C 0.4589(4) 0.5533(4) 0.8573(7) 0.0314(19) Uani 1 1 d . . . . .
H12A H 0.496357 0.547770 0.887877 0.038 Uiso 1 1 calc R U . . .
H12B H 0.415389 0.506246 0.855153 0.038 Uiso 1 1 calc R U . . .
Cl1 Cl 0.30011(11) 0.41026(11) 0.07732(15) 0.0320(5) Uani 1 1 d . U . . .
O9 O 0.3320(5) 0.4650(5) 0.1456(5) 0.054(2) Uani 1 1 d . U . . .
O10 O 0.3400(5) 0.4370(6) -0.0048(6) 0.068(3) Uani 1 1 d . U . . .
O11 O 0.2300(4) 0.3906(5) 0.0593(6) 0.063(3) Uani 1 1 d . U . . .
O12 O 0.3017(5) 0.3490(4) 0.1082(7) 0.064(3) Uani 1 1 d . U . . .
Cl2 Cl 0.55776(9) 0.64264(10) 0.27700(12) 0.0211(4) Uani 1 1 d . U . . .
O13 O 0.6018(9) 0.6130(10) 0.2522(13) 0.032(4) Uani 0.67(4) 1 d . U P A 1
O14 O 0.5124(8) 0.5951(10) 0.3466(13) 0.045(4) Uani 0.67(4) 1 d . U P A 1
O15 O 0.6075(6) 0.7069(7) 0.3157(13) 0.041(4) Uani 0.67(4) 1 d . U P A 1
O16 O 0.5075(8) 0.6292(14) 0.2116(8) 0.054(5) Uani 0.67(4) 1 d D U P A 1
O13B O 0.588(2) 0.6147(19) 0.218(3) 0.039(8) Uani 0.33(4) 1 d . U P A 2
O14B O 0.534(2) 0.631(3) 0.3671(18) 0.051(9) Uani 0.33(4) 1 d . U P A 2
O15B O 0.5978(14) 0.7194(11) 0.265(3) 0.045(7) Uani 0.33(4) 1 d . U P A 2
O16B O 0.5146(15) 0.6664(14) 0.222(2) 0.044(7) Uani 0.33(4) 1 d . U P A 2
Ni1 Ni 0.333333 0.666667 0.18710(14) 0.0302(4) Uani 1 3 d S T P . .
O7 O 0.3851(4) 0.6308(4) 0.2672(5) 0.0387(15) Uani 1 1 d D . . . .
H7W H 0.423(4) 0.629(7) 0.255(8) 0.058 Uiso 1 1 d D U . . .
H7WA H 0.391(5) 0.643(2) 0.3236(19) 0.058 Uiso 1 1 d D U . . .
O8 O 0.3074(4) 0.5795(4) 0.1105(5) 0.0420(17) Uani 1 1 d D . . . .
H8W H 0.317(7) 0.586(6) 0.054(2) 0.19(13) Uiso 1 1 d D . . . .
H8WA H 0.318(6) 0.548(5) 0.128(7) 0.04(3) Uiso 1 1 d D . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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'
Mo Mo -1.6832 0.6857 '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
O1 Zr1 O1 90.3(2) 2_665 3_565 ?
O1 Zr1 O1 90.3(2) 2_665 . ?
O1 Zr1 O1 90.3(2) 3_565 . ?
O1 Zr1 O4 179.1(2) 2_665 . ?
O1 Zr1 O4 90.5(2) 3_565 . ?
O1 Zr1 O4 89.5(2) . . ?
O1 Zr1 O4 89.5(2) 2_665 2_665 ?
O1 Zr1 O4 179.1(2) 3_565 2_665 ?
O1 Zr1 O4 90.5(2) . 2_665 ?
O4 Zr1 O4 89.6(2) . 2_665 ?
O1 Zr1 O4 90.5(2) 2_665 3_565 ?
O1 Zr1 O4 89.5(2) 3_565 3_565 ?
O1 Zr1 O4 179.1(2) . 3_565 ?
O4 Zr1 O4 89.6(2) . 3_565 ?
O4 Zr1 O4 89.6(2) 2_665 3_565 ?
O3 Mo1 O2 106.8(3) . . ?
O3 Mo1 O1 105.7(2) . . ?
O2 Mo1 O1 107.3(3) . . ?
O3 Mo1 N2 90.2(2) . . ?
O2 Mo1 N2 88.4(3) . . ?
O1 Mo1 N2 152.8(2) . . ?
O3 Mo1 N3 88.2(2) . . ?
O2 Mo1 N3 156.6(2) . . ?
O1 Mo1 N3 84.9(2) . . ?
N2 Mo1 N3 73.4(2) . . ?
O3 Mo1 N1 157.3(2) . . ?
O2 Mo1 N1 88.6(2) . . ?
O1 Mo1 N1 84.8(2) . . ?
N2 Mo1 N1 73.2(2) . . ?
N3 Mo1 N1 72.4(2) . . ?
Mo1 O1 Zr1 135.7(3) . . ?
C1 N1 C6 112.2(6) . . ?
C1 N1 Mo1 114.2(4) . . ?
C6 N1 Mo1 107.8(4) . . ?
N1 C1 C2 110.7(6) . . ?
N2 C2 C1 109.0(6) . . ?
C3 N2 C2 112.2(6) . . ?
C3 N2 Mo1 115.8(5) . . ?
C2 N2 Mo1 108.9(5) . . ?
N2 C3 C4 111.4(6) . . ?
N3 C4 C3 108.7(6) . . ?
C5 N3 C4 113.5(6) . . ?
C5 N3 Mo1 116.5(5) . . ?
C4 N3 Mo1 106.1(4) . . ?
N3 C5 C6 110.4(6) . . ?
N1 C6 C5 110.0(6) . . ?
O6 Mo2 O5 106.9(3) . . ?
O6 Mo2 O4 105.9(3) . . ?
O5 Mo2 O4 106.9(3) . . ?
O6 Mo2 N5 88.5(3) . . ?
O5 Mo2 N5 89.9(3) . . ?
O4 Mo2 N5 153.0(2) . . ?
O6 Mo2 N6 89.4(2) . . ?
O5 Mo2 N6 156.5(2) . . ?
O4 Mo2 N6 83.9(2) . . ?
N5 Mo2 N6 73.3(2) . . ?
O6 Mo2 N4 157.0(2) . . ?
O5 Mo2 N4 87.3(2) . . ?
O4 Mo2 N4 86.3(2) . . ?
N5 Mo2 N4 73.3(2) . . ?
N6 Mo2 N4 72.3(2) . . ?
Mo2 O4 Zr1 143.8(3) . . ?
C7 N4 C12 113.6(7) . . ?
C7 N4 Mo2 107.3(5) . . ?
C12 N4 Mo2 114.7(5) . . ?
N4 C7 C8 110.4(7) . . ?
C7 C8 N5 112.9(7) . . ?
C8 N5 C9 112.0(7) . . ?
C8 N5 Mo2 115.0(5) . . ?
C9 N5 Mo2 107.5(5) . . ?
N5 C9 C10 110.3(7) . . ?
N6 C10 C9 109.2(7) . . ?
C10 N6 C11 112.8(6) . . ?
C10 N6 Mo2 115.7(5) . . ?
C11 N6 Mo2 107.3(5) . . ?
C12 C11 N6 110.0(7) . . ?
C11 C12 N4 111.4(7) . . ?
O11 Cl1 O12 108.0(5) . . ?
O11 Cl1 O10 108.4(6) . . ?
O12 Cl1 O10 110.9(6) . . ?
O11 Cl1 O9 112.8(6) . . ?
O12 Cl1 O9 109.0(5) . . ?
O10 Cl1 O9 107.8(6) . . ?
O16 Cl2 O15 129.5(18) . . ?
O14B Cl2 O13B 136(3) . . ?
O16 Cl2 O14 98.9(13) . . ?
O15 Cl2 O14 110.1(9) . . ?
O16 Cl2 O13 111.4(8) . . ?
O15 Cl2 O13 101.3(11) . . ?
O14 Cl2 O13 103.2(11) . . ?
O14B Cl2 O15B 106.4(19) . . ?
O13B Cl2 O15B 106(2) . . ?
O14B Cl2 O16B 109.4(19) . . ?
O13B Cl2 O16B 109.1(18) . . ?
O15B Cl2 O16B 70(2) . . ?
Cl2 O15B O16B 56.4(14) . . ?
Cl2 O16B O15B 53.3(13) . . ?
O8 Ni1 O8 92.3(3) 3_565 2_665 ?
O8 Ni1 O8 92.3(3) 3_565 . ?
O8 Ni1 O8 92.3(3) 2_665 . ?
O8 Ni1 O7 93.2(3) 3_565 2_665 ?
O8 Ni1 O7 84.8(3) 2_665 2_665 ?
O8 Ni1 O7 173.9(3) . 2_665 ?
O8 Ni1 O7 84.8(3) 3_565 3_565 ?
O8 Ni1 O7 173.9(3) 2_665 3_565 ?
O8 Ni1 O7 93.2(3) . 3_565 ?
O7 Ni1 O7 90.0(3) 2_665 3_565 ?
O8 Ni1 O7 173.9(3) 3_565 . ?
O8 Ni1 O7 93.2(3) 2_665 . ?
O8 Ni1 O7 84.8(3) . . ?
O7 Ni1 O7 90.0(3) 2_665 . ?
O7 Ni1 O7 90.0(3) 3_565 . ?
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 2.066(5) 2_665 ?
Zr1 O1 2.066(5) 3_565 ?
Zr1 O1 2.066(5) . ?
Zr1 O4 2.077(5) . ?
Zr1 O4 2.077(5) 2_665 ?
Zr1 O4 2.077(5) 3_565 ?
Mo1 O3 1.703(5) . ?
Mo1 O2 1.717(5) . ?
Mo1 O1 1.816(5) . ?
Mo1 N2 2.239(6) . ?
Mo1 N3 2.305(6) . ?
Mo1 N1 2.322(6) . ?
N1 C1 1.484(10) . ?
N1 C6 1.491(10) . ?
C1 C2 1.508(11) . ?
C2 N2 1.500(10) . ?
N2 C3 1.478(10) . ?
C3 C4 1.503(12) . ?
C4 N3 1.495(9) . ?
N3 C5 1.479(10) . ?
C5 C6 1.517(11) . ?
Mo2 O6 1.716(5) . ?
Mo2 O5 1.730(5) . ?
Mo2 O4 1.795(5) . ?
Mo2 N5 2.252(6) . ?
Mo2 N6 2.302(6) . ?
Mo2 N4 2.327(6) . ?
N4 C7 1.469(11) . ?
N4 C12 1.491(11) . ?
C7 C8 1.475(13) . ?
C8 N5 1.487(10) . ?
N5 C9 1.489(10) . ?
C9 C10 1.522(13) . ?
C10 N6 1.466(10) . ?
N6 C11 1.508(10) . ?
C11 C12 1.477(13) . ?
Cl1 O11 1.390(8) . ?
Cl1 O12 1.426(8) . ?
Cl1 O10 1.428(9) . ?
Cl1 O9 1.442(8) . ?
Cl2 O16 1.373(11) . ?
Cl2 O15 1.394(10) . ?
Cl2 O14B 1.40(3) . ?
Cl2 O13B 1.41(3) . ?
Cl2 O14 1.439(12) . ?
Cl2 O13 1.445(14) . ?
Cl2 O15B 1.46(2) . ?
Cl2 O16B 1.52(2) . ?
O15B O16B 1.71(4) . ?
Ni1 O8 2.030(7) 3_565 ?
Ni1 O8 2.030(7) 2_665 ?
Ni1 O8 2.030(7) . ?
Ni1 O7 2.037(7) 2_665 ?
Ni1 O7 2.037(7) 3_565 ?
Ni1 O7 2.037(7) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1 O2 1.00 2.19 3.112(8) 152.5 2_665 yes
N1 H1 O7 1.00 2.65 3.411(10) 133.1 2_665 yes
N2 H2B O15^a 1.00 2.02 2.920(13) 148.4 . yes
N2 H2B O14B^b 1.00 2.53 3.38(5) 142.8 . yes
N2 H2B O15B^b 1.00 2.43 3.15(4) 129.1 . yes
N3 H3B O6 1.00 2.01 2.971(8) 160.1 . yes
N4 H4B O5 1.00 2.07 3.050(8) 164.8 3_565 yes
N5 H5B O11 1.00 1.93 2.900(11) 162.6 2_666 yes
N6 H6B O3 1.00 1.97 2.924(8) 158.7 . yes
O7 H7W O16^a 0.86(2) 1.95(2) 2.805(13) 172(12) . yes
O7 H7W O16B^b 0.86(2) 1.81(7) 2.61(3) 154(13) . yes
O7 H7WA O2 0.86(2) 1.86(3) 2.687(9) 160(9) . yes
O8 H8WA O9 0.87(3) 1.99(4) 2.846(11) 169(11) . yes
O8 H8W O5 0.86(3) 1.89(5) 2.657(9) 148(10) 3_564 yes
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
O3 Mo1 O1 Zr1 -47.0(5) . . . . ?
O2 Mo1 O1 Zr1 66.7(4) . . . . ?
N2 Mo1 O1 Zr1 -170.6(4) . . . . ?
N3 Mo1 O1 Zr1 -133.7(4) . . . . ?
N1 Mo1 O1 Zr1 153.6(4) . . . . ?
C6 N1 C1 C2 134.9(7) . . . . ?
Mo1 N1 C1 C2 11.8(8) . . . . ?
N1 C1 C2 N2 -42.9(9) . . . . ?
C1 C2 N2 C3 -74.6(8) . . . . ?
C1 C2 N2 Mo1 54.8(7) . . . . ?
C2 N2 C3 C4 134.8(7) . . . . ?
Mo1 N2 C3 C4 8.9(9) . . . . ?
N2 C3 C4 N3 -42.3(9) . . . . ?
C3 C4 N3 C5 -75.1(8) . . . . ?
C3 C4 N3 Mo1 54.1(7) . . . . ?
C4 N3 C5 C6 134.3(7) . . . . ?
Mo1 N3 C5 C6 10.7(8) . . . . ?
C1 N1 C6 C5 -73.3(8) . . . . ?
Mo1 N1 C6 C5 53.3(7) . . . . ?
N3 C5 C6 N1 -42.2(8) . . . . ?
O6 Mo2 O4 Zr1 -51.6(5) . . . . ?
O5 Mo2 O4 Zr1 62.2(5) . . . . ?
N5 Mo2 O4 Zr1 -171.6(4) . . . . ?
N6 Mo2 O4 Zr1 -139.2(5) . . . . ?
N4 Mo2 O4 Zr1 148.2(5) . . . . ?
C12 N4 C7 C8 77.1(9) . . . . ?
Mo2 N4 C7 C8 -50.7(8) . . . . ?
N4 C7 C8 N5 39.8(11) . . . . ?
C7 C8 N5 C9 -131.5(8) . . . . ?
C7 C8 N5 Mo2 -8.3(10) . . . . ?
C8 N5 C9 C10 72.7(9) . . . . ?
Mo2 N5 C9 C10 -54.7(8) . . . . ?
N5 C9 C10 N6 43.1(9) . . . . ?
C9 C10 N6 C11 -135.3(8) . . . . ?
C9 C10 N6 Mo2 -11.2(8) . . . . ?
C10 N6 C11 C12 73.5(9) . . . . ?
Mo2 N6 C11 C12 -55.1(8) . . . . ?
N6 C11 C12 N4 42.2(9) . . . . ?
C7 N4 C12 C11 -133.1(8) . . . . ?
Mo2 N4 C12 C11 -9.2(8) . . . . ?
O14B Cl2 O15B O16B -105(2) . . . . ?
O13B Cl2 O15B O16B 105(2) . . . . ?
O14B Cl2 O16B O15B 101(2) . . . . ?
O13B Cl2 O16B O15B -101(2) . . . . ?
