# Supplementary Information (SI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2024

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

data_FeTiMo6_3p22_104K_a
_database_code_depnum_ccdc_archive 'CCDC 2372554'
loop_
_audit_author_name
_audit_author_address
'Ryoji Mitsuhashi'
;Kanazawa University
Japan
;
_audit_update_record             
;
2024-07-22 deposited with the CCDC.	2024-09-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H90 Fe Mo6 N18 O18 Ti, H12 O6, 6(Cl O4)'
_chemical_formula_sum            'C36 H102 Cl6 Fe Mo6 N18 O48 Ti'
_chemical_formula_weight         2447.44

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'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 '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'

_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_H-M_alt        'R 3 :H'
_space_group_name_Hall           'R 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.
;

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'

_cell_length_a                   21.6648(4)
_cell_length_b                   21.6648(4)
_cell_length_c                   14.6787(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     5966.6(3)
_cell_formula_units_Z            3
_cell_measurement_temperature    104(2)
_cell_measurement_reflns_used    8629
_cell_measurement_theta_min      2.9640
_cell_measurement_theta_max      30.1460

_exptl_crystal_description       rhombohedral
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.043
_exptl_crystal_F_000             3690
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.141
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.085
_exptl_absorpt_coefficient_mu    1.499
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.17458
_exptl_absorpt_correction_T_max  1.00000
_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_absorpt_special_details   ?
_diffrn_ambient_temperature      104(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10783
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_av_R_equivalents  0.0210
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.577
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.737
_diffrn_reflns_point_group_measured_fraction_full 0.765
_reflns_number_total             4493
_reflns_number_gt                4392
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.478
_reflns_Friedel_fraction_max     0.476
_reflns_Friedel_fraction_full    0.534

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0814P)²+42.1115P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.44(5)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         4493
_refine_ls_number_parameters     399
_refine_ls_number_restraints     148
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0317
_refine_ls_wR_factor_ref         0.0877
_refine_ls_wR_factor_gt          0.0868
_refine_ls_goodness_of_fit_ref   0.822
_refine_ls_restrained_S_all      0.810
_refine_ls_shift/su_max          0.001
_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
Ti1 Ti 0.333333 0.666667 0.31960(14) 0.0117(3) Uani 1 3 d S T P . .
Mo1 Mo 0.40584(2) 0.80882(2) 0.47345(4) 0.01425(12) Uani 1 1 d . . . . .
O1 O 0.4038(2) 0.7431(2) 0.3951(3) 0.0175(9) Uani 1 1 d . . . . .
O2 O 0.3532(2) 0.7635(2) 0.5656(3) 0.0202(9) Uani 1 1 d D . . . .
O3 O 0.3631(2) 0.8468(2) 0.4191(3) 0.0213(9) Uani 1 1 d . . . . .
N1 N 0.5002(3) 0.8068(3) 0.5442(4) 0.0208(11) Uani 1 1 d . . . . .
H1 H 0.481587 0.757611 0.569031 0.025 Uiso 1 1 calc R U . . .
C1 C 0.5321(4) 0.8569(4) 0.6214(5) 0.0266(15) Uani 1 1 d . . . . .
H1A H 0.579671 0.896433 0.603886 0.032 Uiso 1 1 calc R U . . .
H1B H 0.538057 0.831861 0.674169 0.032 Uiso 1 1 calc R U . . .
C2 C 0.4841(4) 0.8864(4) 0.6476(5) 0.0250(14) Uani 1 1 d . . . . .
H2A H 0.442738 0.850248 0.682677 0.030 Uiso 1 1 calc R U . . .
H2B H 0.510691 0.929112 0.686378 0.030 Uiso 1 1 calc R U . . .
N2 N 0.4590(3) 0.9055(3) 0.5636(4) 0.0211(12) Uani 1 1 d . . . . .
H2 H 0.421057 0.916189 0.583004 0.025 Uiso 1 1 calc R U . . .
C3 C 0.5160(4) 0.9714(3) 0.5199(6) 0.0297(16) Uani 1 1 d . . . . .
H3A H 0.562766 0.983502 0.546496 0.036 Uiso 1 1 calc R U . . .
H3B H 0.507529 1.011459 0.532114 0.036 Uiso 1 1 calc R U . . .
C4 C 0.5175(4) 0.9612(3) 0.4190(6) 0.0271(15) Uani 1 1 d . . . . .
H4A H 0.478691 0.965359 0.389338 0.033 Uiso 1 1 calc R U . . .
H4B H 0.563484 0.998516 0.393527 0.033 Uiso 1 1 calc R U . . .
N3 N 0.5083(3) 0.8898(3) 0.4009(4) 0.0202(11) Uani 1 1 d . . . . .
H3 H 0.499320 0.880961 0.334077 0.024 Uiso 1 1 calc R U . . .
C5 C 0.5735(3) 0.8855(4) 0.4215(6) 0.0256(14) Uani 1 1 d . . . . .
H5A H 0.607064 0.927441 0.457949 0.031 Uiso 1 1 calc R U . . .
H5B H 0.597474 0.885845 0.363982 0.031 Uiso 1 1 calc R U . . .
C6 C 0.5537(3) 0.8180(4) 0.4740(6) 0.0250(15) Uani 1 1 d . . . . .
H6A H 0.534009 0.776854 0.431781 0.030 Uiso 1 1 calc R U . . .
H6B H 0.596727 0.821948 0.503240 0.030 Uiso 1 1 calc R U . . .
Mo2 Mo 0.37528(2) 0.80827(2) 0.16322(3) 0.01332(12) Uani 1 1 d . . . . .
O4 O 0.3278(2) 0.7365(2) 0.2431(3) 0.0165(8) Uani 1 1 d . . . . .
O5 O 0.3958(2) 0.7731(2) 0.0699(3) 0.0200(9) Uani 1 1 d . . . . .
O6 O 0.4547(2) 0.8653(2) 0.2149(4) 0.0209(9) Uani 1 1 d . . . . .
N4 N 0.2678(3) 0.7755(3) 0.0916(4) 0.0179(11) Uani 1 1 d . . . . .
H4 H 0.243792 0.722720 0.082380 0.021 Uiso 1 1 calc R U . . .
C7 C 0.2843(4) 0.8076(4) -0.0002(6) 0.0310(16) Uani 1 1 d . . . . .
H7A H 0.239969 0.800281 -0.029651 0.037 Uiso 1 1 calc R U . . .
H7B H 0.304495 0.784333 -0.038228 0.037 Uiso 1 1 calc R U . . .
C8 C 0.3371(4) 0.8865(4) 0.0070(6) 0.0302(16) Uani 1 1 d . . . . .
H8A H 0.360152 0.904350 -0.052924 0.036 Uiso 1 1 calc R U . . .
H8B H 0.311377 0.912032 0.023018 0.036 Uiso 1 1 calc R U . . .
N5 N 0.3925(3) 0.9020(3) 0.0763(4) 0.0212(12) Uani 1 1 d . . . . .
H5 H 0.438455 0.919056 0.043048 0.025 Uiso 1 1 calc R U . . .
C9 C 0.4025(4) 0.9598(3) 0.1393(6) 0.0324(18) Uani 1 1 d . . . . .
H9A H 0.406426 1.000421 0.103794 0.039 Uiso 1 1 calc R U . . .
H9B H 0.447367 0.976613 0.173888 0.039 Uiso 1 1 calc R U . . .
C10 C 0.3405(4) 0.9335(4) 0.2051(6) 0.0293(16) Uani 1 1 d . . . . .
H10A H 0.353532 0.966835 0.257050 0.035 Uiso 1 1 calc R U . . .
H10B H 0.298783 0.931103 0.173947 0.035 Uiso 1 1 calc R U . . .
N6 N 0.3226(3) 0.8631(3) 0.2377(4) 0.0197(11) Uani 1 1 d . . . . .
H6 H 0.339256 0.869253 0.302371 0.024 Uiso 1 1 calc R U . . .
C11 C 0.2433(4) 0.8106(4) 0.2393(6) 0.0307(16) Uani 1 1 d . . . . .
H11A H 0.233504 0.768312 0.275968 0.037 Uiso 1 1 calc R U . . .
H11B H 0.217824 0.833073 0.267493 0.037 Uiso 1 1 calc R U . . .
C12 C 0.2180(3) 0.7888(4) 0.1445(6) 0.0300(16) Uani 1 1 d . . . . .
H12A H 0.170651 0.744988 0.145568 0.036 Uiso 1 1 calc R U . . .
H12B H 0.212664 0.826790 0.114457 0.036 Uiso 1 1 calc R U . . .
Fe1 Fe 0.333333 0.666667 0.81489(15) 0.0295(4) Uani 1 3 d S T P . .
O7 O 0.2981(3) 0.7222(3) 0.7321(4) 0.0378(14) Uani 1 1 d D . . . .
H7W H 0.301(5) 0.761(3) 0.749(6) 0.057 Uiso 1 1 d D U . . .
H7WA H 0.310(2) 0.728(4) 0.6767(11) 0.057 Uiso 1 1 d D U . . .
O8 O 0.4035(4) 0.7552(4) 0.8923(5) 0.0451(15) Uani 1 1 d D . . . .
H8W H 0.442(3) 0.792(4) 0.879(7) 0.068 Uiso 1 1 d D U . . .
H8WA H 0.401(6) 0.753(4) 0.9500(11) 0.068 Uiso 1 1 d D U . . .
Cl1 Cl 0.55948(10) 0.92507(9) 0.92322(14) 0.0312(4) Uani 1 1 d . . . . .
O9 O 0.5377(4) 0.8734(4) 0.8521(5) 0.0545(18) Uani 1 1 d D . . . .
O10 O 0.5732(5) 0.8953(5) 1.0021(6) 0.066(2) Uani 1 1 d . . . . .
O11 O 0.5088(4) 0.9443(4) 0.9453(7) 0.062(2) Uani 1 1 d . . . . .
O12 O 0.6227(4) 0.9872(4) 0.8942(6) 0.060(2) Uani 1 1 d . . . . .
Cl2 Cl 0.31120(8) 0.89361(8) 0.72385(12) 0.0229(3) Uani 1 1 d . U . . .
O13 O 0.2832(14) 0.9406(12) 0.7429(14) 0.027(4) Uani 0.65(4) 1 d . U P A 1
O14 O 0.3872(6) 0.9344(7) 0.732(2) 0.065(6) Uani 0.65(4) 1 d . U P A 1
O15 O 0.2851(11) 0.8375(7) 0.7887(9) 0.040(4) Uani 0.65(4) 1 d D U P A 1
O16 O 0.2711(13) 0.8520(8) 0.6456(11) 0.050(5) Uani 0.65(4) 1 d . U P A 1
O13B O 0.280(3) 0.928(2) 0.768(3) 0.035(8) Uani 0.35(4) 1 d . U P A 2
O14B O 0.3750(13) 0.9435(11) 0.6835(19) 0.037(6) Uani 0.35(4) 1 d . U P A 2
O15B O 0.324(2) 0.8517(14) 0.7882(19) 0.053(7) Uani 0.35(4) 1 d . U P A 2
O16B O 0.3072(18) 0.8729(16) 0.6332(16) 0.037(5) Uani 0.35(4) 1 d . U P A 2


_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
Ti1 O4 1.936(5) 2_665 ?
Ti1 O4 1.936(5) 3_565 ?
Ti1 O4 1.936(4) . ?
Ti1 O1 1.942(5) 2_665 ?
Ti1 O1 1.942(5) 3_565 ?
Ti1 O1 1.942(5) . ?
Mo1 O3 1.713(5) . ?
Mo1 O2 1.725(5) . ?
Mo1 O1 1.813(4) . ?
Mo1 N2 2.248(6) . ?
Mo1 N3 2.291(5) . ?
Mo1 N1 2.313(6) . ?
N1 C6 1.479(9) . ?
N1 C1 1.480(9) . ?
C1 C2 1.516(10) . ?
C2 N2 1.488(9) . ?
N2 C3 1.487(9) . ?
C3 C4 1.501(11) . ?
C4 N3 1.482(8) . ?
N3 C5 1.492(8) . ?
C5 C6 1.512(10) . ?
Mo2 O6 1.714(4) . ?
Mo2 O5 1.730(5) . ?
Mo2 O4 1.803(4) . ?
Mo2 N5 2.265(5) . ?
Mo2 N6 2.293(5) . ?
Mo2 N4 2.318(5) . ?
N4 C12 1.471(9) . ?
N4 C7 1.476(10) . ?
C7 C8 1.511(10) . ?
C8 N5 1.478(9) . ?
N5 C9 1.482(9) . ?
C9 C10 1.516(11) . ?
C10 N6 1.455(9) . ?
N6 C11 1.514(9) . ?
C11 C12 1.484(12) . ?
Fe1 O8 2.089(6) 2_665 ?
Fe1 O8 2.089(6) 3_565 ?
Fe1 O8 2.089(6) . ?
Fe1 O7 2.103(6) . ?
Fe1 O7 2.103(6) 2_665 ?
Fe1 O7 2.103(6) 3_565 ?
Cl1 O11 1.394(6) . ?
Cl1 O12 1.424(7) . ?
Cl1 O10 1.426(8) . ?
Cl1 O9 1.427(7) . ?
Cl2 O14B 1.391(18) . ?
Cl2 O13B 1.39(3) . ?
Cl2 O16B 1.39(2) . ?
Cl2 O15 1.420(10) . ?
Cl2 O15B 1.43(2) . ?
Cl2 O14 1.433(12) . ?
Cl2 O16 1.450(12) . ?
Cl2 O13 1.450(15) . ?
O14B O16B 1.67(5) . ?

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 Ti1 O4 89.7(2) 2_665 3_565 ?
O4 Ti1 O4 89.7(2) 2_665 . ?
O4 Ti1 O4 89.7(2) 3_565 . ?
O4 Ti1 O1 89.68(19) 2_665 2_665 ?
O4 Ti1 O1 179.3(2) 3_565 2_665 ?
O4 Ti1 O1 89.97(18) . 2_665 ?
O4 Ti1 O1 89.97(18) 2_665 3_565 ?
O4 Ti1 O1 89.68(19) 3_565 3_565 ?
O4 Ti1 O1 179.3(2) . 3_565 ?
O1 Ti1 O1 90.6(2) 2_665 3_565 ?
O4 Ti1 O1 179.3(2) 2_665 . ?
O4 Ti1 O1 89.97(18) 3_565 . ?
O4 Ti1 O1 89.68(19) . . ?
O1 Ti1 O1 90.6(2) 2_665 . ?
O1 Ti1 O1 90.6(2) 3_565 . ?
O3 Mo1 O2 106.0(2) . . ?
O3 Mo1 O1 106.0(2) . . ?
O2 Mo1 O1 107.5(2) . . ?
O3 Mo1 N2 88.5(2) . . ?
O2 Mo1 N2 87.3(2) . . ?
O1 Mo1 N2 154.84(19) . . ?
O3 Mo1 N3 88.0(2) . . ?
O2 Mo1 N3 155.8(2) . . ?
O1 Mo1 N3 86.6(2) . . ?
N2 Mo1 N3 73.2(2) . . ?
O3 Mo1 N1 156.0(2) . . ?
O2 Mo1 N1 88.6(2) . . ?
O1 Mo1 N1 86.8(2) . . ?
N2 Mo1 N1 73.00(19) . . ?
N3 Mo1 N1 72.3(2) . . ?
Mo1 O1 Ti1 137.1(2) . . ?
C6 N1 C1 111.9(5) . . ?
C6 N1 Mo1 108.2(4) . . ?
C1 N1 Mo1 115.0(4) . . ?
N1 C1 C2 109.6(6) . . ?
N2 C2 C1 109.3(6) . . ?
C3 N2 C2 112.3(6) . . ?
C3 N2 Mo1 115.7(5) . . ?
C2 N2 Mo1 108.4(4) . . ?
N2 C3 C4 110.7(6) . . ?
N3 C4 C3 109.2(6) . . ?
C4 N3 C5 113.1(5) . . ?
C4 N3 Mo1 106.8(4) . . ?
C5 N3 Mo1 116.3(4) . . ?
N3 C5 C6 110.2(5) . . ?
N1 C6 C5 109.5(5) . . ?
O6 Mo2 O5 106.3(2) . . ?
O6 Mo2 O4 105.6(2) . . ?
O5 Mo2 O4 107.3(2) . . ?
O6 Mo2 N5 87.0(2) . . ?
O5 Mo2 N5 89.2(2) . . ?
O4 Mo2 N5 155.0(2) . . ?
O6 Mo2 N6 89.7(2) . . ?
O5 Mo2 N6 155.4(2) . . ?
O4 Mo2 N6 85.4(2) . . ?
N5 Mo2 N6 72.9(2) . . ?
O6 Mo2 N4 156.1(2) . . ?
O5 Mo2 N4 86.9(2) . . ?
O4 Mo2 N4 88.7(2) . . ?
N5 Mo2 N4 73.09(19) . . ?
N6 Mo2 N4 72.1(2) . . ?
Mo2 O4 Ti1 145.0(2) . . ?
C12 N4 C7 114.6(6) . . ?
C12 N4 Mo2 115.0(4) . . ?
C7 N4 Mo2 107.5(4) . . ?
N4 C7 C8 109.7(6) . . ?
N5 C8 C7 112.0(6) . . ?
C8 N5 C9 112.4(6) . . ?
C8 N5 Mo2 115.7(4) . . ?
C9 N5 Mo2 107.1(5) . . ?
N5 C9 C10 110.6(6) . . ?
N6 C10 C9 108.9(6) . . ?
C10 N6 C11 113.5(5) . . ?
C10 N6 Mo2 116.5(5) . . ?
C11 N6 Mo2 106.9(4) . . ?
C12 C11 N6 108.9(6) . . ?
N4 C12 C11 111.6(6) . . ?
O8 Fe1 O8 93.2(3) 2_665 3_565 ?
O8 Fe1 O8 93.2(3) 2_665 . ?
O8 Fe1 O8 93.2(3) 3_565 . ?
O8 Fe1 O7 82.1(3) 2_665 . ?
O8 Fe1 O7 170.4(3) 3_565 . ?
O8 Fe1 O7 95.4(3) . . ?
O8 Fe1 O7 95.4(3) 2_665 2_665 ?
O8 Fe1 O7 82.1(3) 3_565 2_665 ?
O8 Fe1 O7 170.4(3) . 2_665 ?
O7 Fe1 O7 90.0(2) . 2_665 ?
O8 Fe1 O7 170.4(3) 2_665 3_565 ?
O8 Fe1 O7 95.4(3) 3_565 3_565 ?
O8 Fe1 O7 82.1(3) . 3_565 ?
O7 Fe1 O7 90.0(2) . 3_565 ?
O7 Fe1 O7 90.0(2) 2_665 3_565 ?
O11 Cl1 O12 108.4(4) . . ?
O11 Cl1 O10 108.6(5) . . ?
O12 Cl1 O10 110.5(6) . . ?
O11 Cl1 O9 113.8(5) . . ?
O12 Cl1 O9 107.9(5) . . ?
O10 Cl1 O9 107.5(5) . . ?
O14B Cl2 O13B 110(2) . . ?
O14B Cl2 O16B 74(2) . . ?
O13B Cl2 O16B 130(2) . . ?
O14B Cl2 O15B 109.8(16) . . ?
O13B Cl2 O15B 109.6(18) . . ?
O16B Cl2 O15B 115.2(15) . . ?
O15 Cl2 O14 108.2(10) . . ?
O15 Cl2 O16 98.1(13) . . ?
O14 Cl2 O16 126.9(19) . . ?
O15 Cl2 O13 110.2(8) . . ?
O14 Cl2 O13 107.8(12) . . ?
O16 Cl2 O13 104.9(13) . . ?
Cl2 O14B O16B 53.2(13) . . ?
Cl2 O16B O14B 53.0(14) . . ?

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 2.11 3.025(7) 151.7 3_565 yes
N2 H2 O14^a 1.00 2.41 3.15(2) 130.6 . yes
N3 H3 O6 1.00 1.95 2.911(8) 161.5 . yes
N4 H4 O5 1.00 2.02 2.984(6) 161.9 2_665 yes
N5 H5 O11 1.00 1.96 2.930(9) 162.2 1_554 yes
N6 H6 O3 1.00 1.92 2.879(8) 159.5 . yes
O7 H7WA O2 0.845(12) 1.85(2) 2.670(8) 165(7) . yes
O7 H7W O15^a 0.848(12) 1.942(19) 2.777(11) 168(9) . yes
O7 H7W O15B^b 0.848(12) 1.86(3) 2.70(3) 169(9) . yes
O8 H8WA O5 0.849(12) 1.83(2) 2.654(8) 163(8) 1_556 yes
O8 H8W O9 0.848(13) 1.968(19) 2.813(10) 174(12) . yes

_refine_diff_density_max         1.602
_refine_diff_density_min         -1.700
_refine_diff_density_rms         0.115



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

data_CoTiMo6_3p22_104K_a
_database_code_depnum_ccdc_archive 'CCDC 2372555'
loop_
_audit_author_name
_audit_author_address
'Ryoji Mitsuhashi'
;Kanazawa University
Japan
;
_audit_update_record             
;
2024-07-22 deposited with the CCDC.	2024-09-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H90 Mo6 N18 O18 Ti, H12 Co O6, 6(Cl O4)'
_chemical_formula_sum            'C36 H102 Cl6 Co Mo6 N18 O48 Ti'
_chemical_formula_weight         2450.52

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'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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'

_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_H-M_alt        'R 3 :H'
_space_group_name_Hall           'R 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.
;

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'

_cell_length_a                   21.5929(7)
_cell_length_b                   21.5929(7)
_cell_length_c                   14.6575(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     5918.5(4)
_cell_formula_units_Z            3
_cell_measurement_temperature    104(2)
_cell_measurement_reflns_used    5487
_cell_measurement_theta_min      2.5460
_cell_measurement_theta_max      29.5800

_exptl_crystal_description       rhombohedral
_exptl_crystal_colour            pink
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.063
_exptl_crystal_F_000             3693
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.138
_exptl_crystal_size_mid          0.092
_exptl_crystal_size_min          0.051
_exptl_absorpt_coefficient_mu    1.537
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.17287
_exptl_absorpt_correction_T_max  1.00000
_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_absorpt_special_details   ?
_diffrn_ambient_temperature      104(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9959
_diffrn_reflns_av_unetI/netI     0.0504
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.584
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.795
_diffrn_reflns_point_group_measured_fraction_full 0.829
_reflns_number_total             4799
_reflns_number_gt                4393
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.594
_reflns_Friedel_fraction_max     0.592
_reflns_Friedel_fraction_full    0.659

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0743P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.44(5)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         4799
_refine_ls_number_parameters     399
_refine_ls_number_restraints     164
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0410
_refine_ls_wR_factor_ref         0.1091
_refine_ls_wR_factor_gt          0.1056
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.666667 0.333333 0.67762(17) 0.0149(5) Uani 1 3 d S T P . .
Mo1 Mo 0.73635(4) 0.47592(3) 0.83125(6) 0.01703(17) Uani 1 1 d . . . . .
O1 O 0.6728(3) 0.4101(3) 0.7527(4) 0.0202(12) Uani 1 1 d . . . . .
O2 O 0.7436(4) 0.4302(3) 0.9241(3) 0.0236(13) Uani 1 1 d . . . . .
O3 O 0.8171(3) 0.5137(3) 0.7770(4) 0.0262(14) Uani 1 1 d . . . . .
N1 N 0.6396(4) 0.4736(4) 0.9031(5) 0.0226(16) Uani 1 1 d . . . . .
H1 H 0.609027 0.424387 0.928203 0.027 Uiso 1 1 calc DR U . . .
C1 C 0.6581(5) 0.5243(6) 0.9795(7) 0.032(2) Uani 1 1 d . . . . .
H1A H 0.627214 0.499573 1.032664 0.038 Uiso 1 1 calc R U . . .
H1B H 0.649818 0.563797 0.961494 0.038 Uiso 1 1 calc R U . . .
C2 C 0.7356(5) 0.5541(5) 1.0052(6) 0.029(2) Uani 1 1 d . . . . .
H2 H 0.751778 0.597254 1.043606 0.035 Uiso 1 1 calc R U . . .
H2A H 0.741046 0.518203 1.040756 0.035 Uiso 1 1 calc R U . . .
N2 N 0.7796(4) 0.5728(4) 0.9215(5) 0.0229(16) Uani 1 1 d . . . . .
H2B H 0.828435 0.583825 0.940876 0.027 Uiso 1 1 calc R U . . .
C3 C 0.7881(6) 0.6382(5) 0.8769(7) 0.033(2) Uani 1 1 d . . . . .
H3 H 0.836872 0.678521 0.888646 0.040 Uiso 1 1 calc R U . . .
H3A H 0.753544 0.650592 0.903719 0.040 Uiso 1 1 calc R U . . .
C4 C 0.7760(5) 0.6282(5) 0.7761(6) 0.028(2) Uani 1 1 d . . . . .
H4 H 0.767028 0.665553 0.751027 0.034 Uiso 1 1 calc R U . . .
H4A H 0.819055 0.632589 0.745991 0.034 Uiso 1 1 calc R U . . .
N3 N 0.7141(4) 0.5570(4) 0.7578(5) 0.0231(15) Uani 1 1 d . . . . .
H3B H 0.714384 0.548105 0.690910 0.028 Uiso 1 1 calc R U . . .
C5 C 0.6447(5) 0.5525(5) 0.7783(7) 0.029(2) Uani 1 1 d . . . . .
H5 H 0.620553 0.552011 0.720649 0.035 Uiso 1 1 calc R U . . .
H5A H 0.652917 0.594812 0.814080 0.035 Uiso 1 1 calc R U . . .
C6 C 0.5974(5) 0.4848(5) 0.8322(7) 0.029(2) Uani 1 1 d . . . . .
H6 H 0.558088 0.488642 0.861315 0.034 Uiso 1 1 calc R U . . .
H6A H 0.575911 0.443210 0.790367 0.034 Uiso 1 1 calc R U . . .
Mo2 Mo 0.76657(3) 0.47505(4) 0.52071(6) 0.01664(17) Uani 1 1 d . . . . .
O4 O 0.7425(3) 0.4034(3) 0.6010(4) 0.0198(12) Uani 1 1 d . . . . .
O5 O 0.7114(3) 0.4401(3) 0.4275(4) 0.0251(14) Uani 1 1 d D . . . .
O6 O 0.7438(3) 0.5318(3) 0.5727(4) 0.0237(13) Uani 1 1 d . . . . .
N4 N 0.8411(4) 0.4419(4) 0.4490(5) 0.0210(15) Uani 1 1 d . . . . .
H4B H 0.812125 0.389088 0.439392 0.025 Uiso 1 1 calc R U . . .
C7 C 0.8583(6) 0.4742(5) 0.3586(7) 0.036(2) Uani 1 1 d . . . . .
H7 H 0.815561 0.450008 0.319013 0.044 Uiso 1 1 calc R U . . .
H7A H 0.896550 0.467676 0.331160 0.044 Uiso 1 1 calc R U . . .
C8 C 0.8825(6) 0.5519(6) 0.3639(7) 0.035(2) Uani 1 1 d . . . . .
H8 H 0.934227 0.578623 0.378048 0.042 Uiso 1 1 calc R U . . .
H8A H 0.875559 0.568255 0.303679 0.042 Uiso 1 1 calc R U . . .
N5 N 0.8435(4) 0.5684(4) 0.4339(5) 0.0239(16) Uani 1 1 d . . . . .
H5B H 0.814485 0.585568 0.400582 0.029 Uiso 1 1 calc R U . . .
C9 C 0.8910(6) 0.6262(5) 0.4955(8) 0.037(2) Uani 1 1 d . . . . .
H9 H 0.863167 0.644052 0.528628 0.044 Uiso 1 1 calc R U . . .
H9A H 0.928257 0.666210 0.459285 0.044 Uiso 1 1 calc R U . . .
C10 C 0.9264(6) 0.6012(5) 0.5634(7) 0.035(2) Uani 1 1 d . . . . .
H10 H 0.967091 0.599907 0.534105 0.042 Uiso 1 1 calc R U . . .
H10A H 0.945149 0.634899 0.615390 0.042 Uiso 1 1 calc R U . . .
N6 N 0.8749(4) 0.5303(4) 0.5961(5) 0.0226(15) Uani 1 1 d . . . . .
H6B H 0.864310 0.536196 0.660883 0.027 Uiso 1 1 calc R U . . .
C11 C 0.9012(6) 0.4778(6) 0.5970(7) 0.035(2) Uani 1 1 d . . . . .
H11 H 0.949152 0.500079 0.625471 0.042 Uiso 1 1 calc R U . . .
H11A H 0.868380 0.435516 0.633874 0.042 Uiso 1 1 calc R U . . .
C12 C 0.9051(6) 0.4550(5) 0.5035(7) 0.034(2) Uani 1 1 d . . . . .
H12 H 0.907824 0.410577 0.505792 0.041 Uiso 1 1 calc R U . . .
H12A H 0.948978 0.492413 0.473406 0.041 Uiso 1 1 calc R U . . .
Co1 Co 0.666667 0.333333 0.17175(17) 0.0342(5) Uani 1 3 d S T P . .
O7 O 0.7561(4) 0.3865(4) 0.0875(4) 0.0429(19) Uani 1 1 d D . . . .
H7WA H 0.752(4) 0.398(3) 0.0338(16) 0.064 Uiso 1 1 d D U . . .
H7W H 0.793(3) 0.423(2) 0.107(5) 0.064 Uiso 1 1 d D U . . .
O8 O 0.6877(6) 0.4211(5) 0.2501(6) 0.052(2) Uani 1 1 d D . . . .
H8WA H 0.686(7) 0.416(5) 0.3071(10) 0.078 Uiso 1 1 d D U . . .
H8W H 0.682(5) 0.456(3) 0.238(8) 0.078 Uiso 1 1 d D U . . .
Cl1 Cl 0.69933(13) 0.59060(13) 0.27996(17) 0.0321(5) Uani 1 1 d . . . . .
O9 O 0.7694(4) 0.6093(5) 0.3013(7) 0.067(3) Uani 1 1 d D . . . .
O10 O 0.6678(5) 0.5372(5) 0.2108(6) 0.057(2) Uani 1 1 d D . . . .
O11 O 0.6576(6) 0.5640(6) 0.3605(6) 0.075(3) Uani 1 1 d D . . . .
O12 O 0.6985(5) 0.6531(4) 0.2487(7) 0.059(2) Uani 1 1 d D . . . .
Cl2 Cl 0.91486(12) 0.55914(12) 0.08148(15) 0.0257(4) Uani 1 1 d . U . . .
O13 O 0.9881(10) 0.6061(14) 0.0992(17) 0.027(5) Uani 0.54(5) 1 d D U P A 1
O14 O 0.8791(11) 0.6001(10) 0.095(3) 0.055(8) Uani 0.54(5) 1 d D U P A 1
O15 O 0.9014(14) 0.5332(17) -0.0078(11) 0.053(7) Uani 0.54(5) 1 d D U P A 1
O16 O 0.8840(10) 0.5012(10) 0.1453(14) 0.037(5) Uani 0.54(5) 1 d D U P A 1
O13B O 0.9841(15) 0.5948(17) 0.125(3) 0.039(8) Uani 0.46(5) 1 d D U P A 2
O14B O 0.8992(19) 0.6086(11) 0.045(2) 0.045(7) Uani 0.46(5) 1 d D U P A 2
O15B O 0.9171(12) 0.5147(12) 0.0092(19) 0.033(6) Uani 0.46(5) 1 d D U P A 2
O16B O 0.861(2) 0.5155(14) 0.1466(18) 0.059(9) Uani 0.46(5) 1 d D U P A 2


_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
Ti1 O1 1.937(6) 2_655 ?
Ti1 O1 1.937(6) . ?
Ti1 O1 1.937(6) 3_665 ?
Ti1 O4 1.938(6) . ?
Ti1 O4 1.939(6) 3_665 ?
Ti1 O4 1.939(6) 2_655 ?
Mo1 O3 1.707(7) . ?
Mo1 O2 1.733(5) . ?
Mo1 O1 1.811(6) . ?
Mo1 N2 2.246(7) . ?
Mo1 N3 2.301(7) . ?
Mo1 N1 2.318(7) . ?
N1 C1 1.475(12) . ?
N1 C6 1.479(12) . ?
C1 C2 1.509(14) . ?
C2 N2 1.479(12) . ?
N2 C3 1.482(12) . ?
C3 C4 1.497(14) . ?
C4 N3 1.472(12) . ?
N3 C5 1.483(11) . ?
C5 C6 1.520(14) . ?
Mo2 O6 1.711(6) . ?
Mo2 O5 1.719(6) . ?
Mo2 O4 1.800(6) . ?
Mo2 N5 2.257(8) . ?
Mo2 N6 2.307(7) . ?
Mo2 N4 2.314(7) . ?
N4 C7 1.456(12) . ?
N4 C12 1.496(13) . ?
C7 C8 1.488(15) . ?
C8 N5 1.480(12) . ?
N5 C9 1.464(13) . ?
C9 C10 1.510(15) . ?
C10 N6 1.450(12) . ?
N6 C11 1.502(12) . ?
C11 C12 1.473(14) . ?
Co1 O8 2.062(8) 3_665 ?
Co1 O8 2.062(8) 2_655 ?
Co1 O8 2.062(8) . ?
Co1 O7 2.086(7) 2_655 ?
Co1 O7 2.086(7) . ?
Co1 O7 2.086(7) 3_665 ?
Cl1 O9 1.393(8) . ?
Cl1 O11 1.421(9) . ?
Cl1 O10 1.427(8) . ?
Cl1 O12 1.435(8) . ?
Cl2 O14B 1.380(16) . ?
Cl2 O15 1.396(17) . ?
Cl2 O13 1.412(18) . ?
Cl2 O16B 1.429(19) . ?
Cl2 O16 1.432(14) . ?
Cl2 O13B 1.44(2) . ?
Cl2 O15B 1.446(16) . ?
Cl2 O14 1.449(17) . ?

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 Ti1 O1 90.9(2) 2_655 . ?
O1 Ti1 O1 90.9(2) 2_655 3_665 ?
O1 Ti1 O1 90.9(2) . 3_665 ?
O1 Ti1 O4 179.2(3) 2_655 . ?
O1 Ti1 O4 89.5(2) . . ?
O1 Ti1 O4 89.8(2) 3_665 . ?
O1 Ti1 O4 89.8(2) 2_655 3_665 ?
O1 Ti1 O4 179.2(3) . 3_665 ?
O1 Ti1 O4 89.5(2) 3_665 3_665 ?
O4 Ti1 O4 89.8(3) . 3_665 ?
O1 Ti1 O4 89.5(2) 2_655 2_655 ?
O1 Ti1 O4 89.8(2) . 2_655 ?
O1 Ti1 O4 179.2(3) 3_665 2_655 ?
O4 Ti1 O4 89.8(3) . 2_655 ?
O4 Ti1 O4 89.8(3) 3_665 2_655 ?
O3 Mo1 O2 106.1(3) . . ?
O3 Mo1 O1 105.7(3) . . ?
O2 Mo1 O1 107.5(3) . . ?
O3 Mo1 N2 88.8(3) . . ?
O2 Mo1 N2 87.4(3) . . ?
O1 Mo1 N2 154.8(3) . . ?
O3 Mo1 N3 88.3(3) . . ?
O2 Mo1 N3 155.9(3) . . ?
O1 Mo1 N3 86.3(3) . . ?
N2 Mo1 N3 73.4(3) . . ?
O3 Mo1 N1 156.3(3) . . ?
O2 Mo1 N1 88.2(3) . . ?
O1 Mo1 N1 87.2(3) . . ?
N2 Mo1 N1 72.7(3) . . ?
N3 Mo1 N1 72.5(3) . . ?
Mo1 O1 Ti1 137.2(3) . . ?
C1 N1 C6 111.9(7) . . ?
C1 N1 Mo1 115.0(6) . . ?
C6 N1 Mo1 107.4(5) . . ?
N1 C1 C2 109.7(8) . . ?
N2 C2 C1 109.5(8) . . ?
C2 N2 C3 112.5(8) . . ?
C2 N2 Mo1 108.9(6) . . ?
C3 N2 Mo1 115.1(6) . . ?
N2 C3 C4 111.5(8) . . ?
N3 C4 C3 109.4(7) . . ?
C4 N3 C5 113.1(7) . . ?
C4 N3 Mo1 106.5(5) . . ?
C5 N3 Mo1 116.4(6) . . ?
N3 C5 C6 109.8(7) . . ?
N1 C6 C5 110.4(7) . . ?
O6 Mo2 O5 106.5(3) . . ?
O6 Mo2 O4 105.2(3) . . ?
O5 Mo2 O4 107.6(3) . . ?
O6 Mo2 N5 87.6(3) . . ?
O5 Mo2 N5 89.0(3) . . ?
O4 Mo2 N5 154.5(3) . . ?
O6 Mo2 N6 89.8(3) . . ?
O5 Mo2 N6 155.3(3) . . ?
O4 Mo2 N6 85.1(3) . . ?
N5 Mo2 N6 72.8(3) . . ?
O6 Mo2 N4 156.4(3) . . ?
O5 Mo2 N4 86.6(3) . . ?
O4 Mo2 N4 88.7(3) . . ?
N5 Mo2 N4 72.8(3) . . ?
N6 Mo2 N4 72.3(3) . . ?
Mo2 O4 Ti1 144.9(3) . . ?
C7 N4 C12 113.9(8) . . ?
C7 N4 Mo2 108.4(6) . . ?
C12 N4 Mo2 114.8(5) . . ?
N4 C7 C8 110.7(8) . . ?
N5 C8 C7 112.8(8) . . ?
C9 N5 C8 113.1(8) . . ?
C9 N5 Mo2 107.6(6) . . ?
C8 N5 Mo2 115.4(6) . . ?
N5 C9 C10 111.5(8) . . ?
N6 C10 C9 109.6(8) . . ?
C10 N6 C11 114.8(8) . . ?
C10 N6 Mo2 115.6(6) . . ?
C11 N6 Mo2 106.4(6) . . ?
C12 C11 N6 110.5(8) . . ?
C11 C12 N4 111.0(8) . . ?
O8 Co1 O8 92.0(4) 3_665 2_655 ?
O8 Co1 O8 92.0(4) 3_665 . ?
O8 Co1 O8 92.0(4) 2_655 . ?
O8 Co1 O7 171.1(4) 3_665 2_655 ?
O8 Co1 O7 96.1(4) 2_655 2_655 ?
O8 Co1 O7 84.0(3) . 2_655 ?
O8 Co1 O7 84.0(3) 3_665 . ?
O8 Co1 O7 171.1(4) 2_655 . ?
O8 Co1 O7 96.1(4) . . ?
O7 Co1 O7 88.6(3) 2_655 . ?
O8 Co1 O7 96.1(4) 3_665 3_665 ?
O8 Co1 O7 84.0(3) 2_655 3_665 ?
O8 Co1 O7 171.1(4) . 3_665 ?
O7 Co1 O7 88.6(3) 2_655 3_665 ?
O7 Co1 O7 88.6(3) . 3_665 ?
O9 Cl1 O11 108.0(6) . . ?
O9 Cl1 O10 113.8(7) . . ?
O11 Cl1 O10 108.3(6) . . ?
O9 Cl1 O12 108.8(5) . . ?
O11 Cl1 O12 110.0(7) . . ?
O10 Cl1 O12 108.0(5) . . ?
O15 Cl2 O13 113.2(13) . . ?
O14B Cl2 O16B 109.9(15) . . ?
O15 Cl2 O16 110.4(11) . . ?
O13 Cl2 O16 111.8(10) . . ?
O14B Cl2 O13B 110.4(14) . . ?
O16B Cl2 O13B 109.6(15) . . ?
O14B Cl2 O15B 109.4(12) . . ?
O16B Cl2 O15B 109.6(12) . . ?
O13B Cl2 O15B 107.9(15) . . ?
O15 Cl2 O14 107.8(12) . . ?
O13 Cl2 O14 106.5(14) . . ?
O16 Cl2 O14 106.7(12) . . ?

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 2.11 3.021(9) 151.1 2_655 yes
N2 H2B O14^a 1.00 2.46 3.19(3) 129.6 1_556 yes
N3 H3B O6 1.00 1.94 2.902(9) 161.1 . yes
N4 H4B O5 1.00 2.02 2.986(9) 162.1 3_665 yes
N5 H5B O9 1.00 1.96 2.920(12) 161.1 . yes
N6 H6B O3 1.00 1.92 2.876(10) 159.7 . yes
O7 H7WA O2 0.8404(13) 1.8004(14) 2.637(6) 174(5) 1_554 yes
O7 H7W O16^a 0.8402(14) 1.930(12) 2.764(14) 171(9) . yes
O8 H8WA O5 0.840(3) 1.84(4) 2.642(10) 159(11) . yes
O8 H8W O10 0.840(3) 1.968(14) 2.808(13) 179(12) . yes

_refine_diff_density_max         1.022
_refine_diff_density_min         -1.449
_refine_diff_density_rms         0.137



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

data_NiTiMo6_3p23_100K_a
_database_code_depnum_ccdc_archive 'CCDC 2372556'
loop_
_audit_author_name
_audit_author_address
'Ryoji Mitsuhashi'
;Kanazawa University
Japan
;
_audit_update_record             
;
2024-07-22 deposited with the CCDC.	2024-09-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H90 Mo6 N18 O18 Ti, H12 Ni O6, 6(Cl O4)'
_chemical_formula_sum            'C36 H102 Cl6 Mo6 N18 Ni O48 Ti'
_chemical_formula_weight         2450.30

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'
Ti Ti 0.2776 0.4457 '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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_H-M_alt        'R 3 :H'
_space_group_name_Hall           'R 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.
;

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'

_cell_length_a                   21.6510(8)
_cell_length_b                   21.6510(8)
_cell_length_c                   14.6425(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     5944.3(5)
_cell_formula_units_Z            3
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4693
_cell_measurement_theta_min      2.5560
_cell_measurement_theta_max      30.3060

_exptl_crystal_description       rhombohedral
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.053
_exptl_crystal_F_000             3696
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.155
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.063
_exptl_absorpt_coefficient_mu    1.559
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.27827
_exptl_absorpt_correction_T_max  1.00000
_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_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10374
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.765
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.699
_diffrn_reflns_point_group_measured_fraction_full 0.725
_reflns_number_total             4240
_reflns_number_gt                3976
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.401
_reflns_Friedel_fraction_max     0.400
_reflns_Friedel_fraction_full    0.452

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

_computing_data_collection       'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0980P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.06(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         4240
_refine_ls_number_parameters     399
_refine_ls_number_restraints     148
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0428
_refine_ls_wR_factor_ref         0.1174
_refine_ls_wR_factor_gt          0.1153
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_restrained_S_all      0.968
_refine_ls_shift/su_max          0.001
_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
Ti1 Ti 0.333333 0.666667 0.67686(17) 0.0106(5) Uani 1 3 d S T P . .
Mo1 Mo 0.40641(4) 0.59721(4) 0.83062(4) 0.01295(17) Uani 1 1 d . . . . .
O1 O 0.4042(3) 0.6611(3) 0.7521(4) 0.0183(12) Uani 1 1 d . . . . .
O2 O 0.3540(3) 0.5896(4) 0.9228(4) 0.0214(14) Uani 1 1 d . . . . .
O3 O 0.3637(3) 0.5167(3) 0.7762(4) 0.0201(13) Uani 1 1 d . . . . .
N1 N 0.5009(4) 0.6940(4) 0.9017(5) 0.0206(16) Uani 1 1 d . . . . .
H1 H 0.482265 0.724546 0.926579 0.025 Uiso 1 1 calc R U . . .
C1 C 0.5329(5) 0.6756(5) 0.9791(6) 0.0228(19) Uani 1 1 d . . . . .
H1A H 0.538205 0.706033 1.032417 0.027 Uiso 1 1 calc R U . . .
H1B H 0.580770 0.684285 0.961785 0.027 Uiso 1 1 calc R U . . .
C2 C 0.4851(5) 0.5977(5) 1.0038(6) 0.0218(19) Uani 1 1 d . . . . .
H2A H 0.511887 0.581519 1.042211 0.026 Uiso 1 1 calc R U . . .
H2B H 0.443760 0.592128 1.039525 0.026 Uiso 1 1 calc R U . . .
N2 N 0.4598(4) 0.5539(4) 0.9215(5) 0.0189(15) Uani 1 1 d . . . . .
H2 H 0.422007 0.505208 0.941178 0.023 Uiso 1 1 calc R U . . .
C3 C 0.5166(5) 0.5453(5) 0.8755(7) 0.025(2) Uani 1 1 d . . . . .
H3A H 0.508056 0.496613 0.887073 0.031 Uiso 1 1 calc R U . . .
H3B H 0.563452 0.579642 0.902060 0.031 Uiso 1 1 calc R U . . .
C4 C 0.5185(6) 0.5574(5) 0.7743(7) 0.026(2) Uani 1 1 d . . . . .
H4A H 0.564635 0.566176 0.748954 0.031 Uiso 1 1 calc R U . . .
H4B H 0.479770 0.514570 0.744076 0.031 Uiso 1 1 calc R U . . .
N3 N 0.5095(4) 0.6197(4) 0.7570(5) 0.0186(15) Uani 1 1 d . . . . .
H3 H 0.500125 0.619558 0.690140 0.022 Uiso 1 1 calc R U . . .
C5 C 0.5740(5) 0.6889(5) 0.7771(7) 0.0234(19) Uani 1 1 d . . . . .
H5A H 0.597275 0.712790 0.719158 0.028 Uiso 1 1 calc R U . . .
H5B H 0.608221 0.680800 0.812556 0.028 Uiso 1 1 calc R U . . .
C6 C 0.5543(5) 0.7361(5) 0.8309(7) 0.0232(19) Uani 1 1 d . . . . .
H6A H 0.597481 0.774979 0.860118 0.028 Uiso 1 1 calc R U . . .
H6B H 0.534531 0.757828 0.789123 0.028 Uiso 1 1 calc R U . . .
Mo2 Mo 0.37432(4) 0.56656(3) 0.51908(4) 0.01317(17) Uani 1 1 d . . . . .
O4 O 0.3268(3) 0.5909(3) 0.5999(4) 0.0165(12) Uani 1 1 d . . . . .
O5 O 0.3945(4) 0.6221(3) 0.4257(4) 0.0211(14) Uani 1 1 d D . . . .
O6 O 0.4541(3) 0.5895(3) 0.5704(4) 0.0200(13) Uani 1 1 d . . . . .
N4 N 0.2657(4) 0.4914(4) 0.4485(5) 0.0185(15) Uani 1 1 d . . . . .
H4 H 0.241737 0.520137 0.438997 0.022 Uiso 1 1 calc R U . . .
C7 C 0.2814(6) 0.4745(6) 0.3568(7) 0.033(2) Uani 1 1 d . . . . .
H7A H 0.300585 0.517536 0.317735 0.039 Uiso 1 1 calc R U . . .
H7B H 0.236843 0.436881 0.328560 0.039 Uiso 1 1 calc R U . . .
C8 C 0.3345(6) 0.4496(6) 0.3627(7) 0.030(2) Uani 1 1 d . . . . .
H8A H 0.309303 0.398193 0.377956 0.036 Uiso 1 1 calc R U . . .
H8B H 0.357403 0.455543 0.302306 0.036 Uiso 1 1 calc R U . . .
N5 N 0.3908(4) 0.4894(4) 0.4325(5) 0.0199(15) Uani 1 1 d . . . . .
H5 H 0.436600 0.518250 0.398655 0.024 Uiso 1 1 calc R U . . .
C9 C 0.4016(6) 0.4427(6) 0.4943(9) 0.035(3) Uani 1 1 d . . . . .
H9A H 0.446495 0.471053 0.528771 0.042 Uiso 1 1 calc R U . . .
H9B H 0.405882 0.406271 0.458430 0.042 Uiso 1 1 calc R U . . .
C10 C 0.3398(6) 0.4061(5) 0.5607(7) 0.031(2) Uani 1 1 d . . . . .
H10A H 0.298024 0.366807 0.529579 0.037 Uiso 1 1 calc R U . . .
H10B H 0.353327 0.385615 0.612252 0.037 Uiso 1 1 calc R U . . .
N6 N 0.3218(4) 0.4589(4) 0.5949(5) 0.0182(15) Uani 1 1 d . . . . .
H6 H 0.338823 0.469372 0.659603 0.022 Uiso 1 1 calc R U . . .
C11 C 0.2432(5) 0.4325(6) 0.5968(7) 0.032(2) Uani 1 1 d . . . . .
H11A H 0.218006 0.384708 0.625578 0.039 Uiso 1 1 calc R U . . .
H11B H 0.233924 0.465181 0.633918 0.039 Uiso 1 1 calc R U . . .
C12 C 0.2158(5) 0.4282(6) 0.5035(7) 0.029(2) Uani 1 1 d . . . . .
H12A H 0.168764 0.425368 0.506440 0.035 Uiso 1 1 calc R U . . .
H12B H 0.209152 0.384289 0.473448 0.035 Uiso 1 1 calc R U . . .
Ni1 Ni 0.333333 0.666667 0.17005(15) 0.0271(5) Uani 1 3 d S T P . .
O7 O 0.4214(4) 0.7183(4) 0.0884(4) 0.0359(18) Uani 1 1 d D . . . .
H7W H 0.456(3) 0.757(3) 0.109(5) 0.04(3) Uiso 1 1 d D . . . .
H7WA H 0.418(3) 0.728(4) 0.0334(13) 0.053 Uiso 1 1 d D U . . .
O8 O 0.3943(5) 0.6399(5) 0.2458(5) 0.046(2) Uani 1 1 d D . . . .
H8W H 0.435(3) 0.646(8) 0.233(8) 0.069 Uiso 1 1 d D U . . .
H8WA H 0.393(7) 0.641(6) 0.3037(9) 0.069 Uiso 1 1 d D U . . .
Cl1 Cl 0.55629(14) 0.63382(13) 0.27800(17) 0.0292(5) Uani 1 1 d . . . . .
O9 O 0.5044(6) 0.5643(4) 0.2981(8) 0.067(3) Uani 1 1 d . . . . .
O10 O 0.5339(5) 0.6670(5) 0.2101(6) 0.051(2) Uani 1 1 d D . . . .
O12 O 0.6185(5) 0.6343(5) 0.2446(8) 0.058(3) Uani 1 1 d . . . . .
O11 O 0.5729(7) 0.6742(6) 0.3588(7) 0.071(3) Uani 1 1 d . . . . .
Cl2 Cl 0.58166(12) 0.89201(11) 0.08021(15) 0.0218(4) Uani 1 1 d . U . . .
O13 O 0.6567(13) 0.9408(15) 0.0997(18) 0.020(5) Uani 0.52(5) 1 d . U P A 1
O14 O 0.5717(14) 0.8660(18) -0.0102(13) 0.043(7) Uani 0.52(5) 1 d . U P A 1
O15 O 0.5456(12) 0.9327(12) 0.092(3) 0.057(8) Uani 0.52(5) 1 d . U P A 1
O16 O 0.5509(11) 0.8354(10) 0.1437(14) 0.030(5) Uani 0.52(5) 1 d D U P A 1
O13B O 0.6496(16) 0.9260(19) 0.124(3) 0.035(8) Uani 0.48(5) 1 d . U P A 2
O14B O 0.5816(14) 0.8446(13) 0.010(2) 0.035(6) Uani 0.48(5) 1 d . U P A 2
O15B O 0.5666(18) 0.9424(10) 0.043(2) 0.041(8) Uani 0.48(5) 1 d . U P A 2
O16B O 0.527(2) 0.8482(16) 0.1445(19) 0.059(9) Uani 0.48(5) 1 d . U P A 2


_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
Ti1 O4 1.935(6) . ?
Ti1 O4 1.935(6) 3_565 ?
Ti1 O4 1.935(6) 2_665 ?
Ti1 O1 1.941(6) . ?
Ti1 O1 1.941(6) 2_665 ?
Ti1 O1 1.941(6) 3_565 ?
Mo1 O3 1.707(6) . ?
Mo1 O2 1.718(6) . ?
Mo1 O1 1.818(6) . ?
Mo1 N2 2.252(7) . ?
Mo1 N3 2.301(7) . ?
Mo1 N1 2.317(8) . ?
N1 C6 1.480(12) . ?
N1 C1 1.482(11) . ?
C1 C2 1.517(13) . ?
C2 N2 1.461(11) . ?
N2 C3 1.493(12) . ?
C3 C4 1.502(13) . ?
C4 N3 1.478(12) . ?
N3 C5 1.480(11) . ?
C5 C6 1.510(13) . ?
Mo2 O6 1.714(6) . ?
Mo2 O5 1.726(6) . ?
Mo2 O4 1.812(6) . ?
Mo2 N5 2.264(8) . ?
Mo2 N6 2.304(7) . ?
Mo2 N4 2.328(7) . ?
N4 C7 1.473(12) . ?
N4 C12 1.487(13) . ?
C7 C8 1.498(15) . ?
C8 N5 1.491(12) . ?
N5 C9 1.459(13) . ?
C9 C10 1.517(16) . ?
C10 N6 1.469(12) . ?
N6 C11 1.500(12) . ?
C11 C12 1.474(14) . ?
Ni1 O8 2.017(8) 2_665 ?
Ni1 O8 2.017(8) 3_565 ?
Ni1 O8 2.017(8) . ?
Ni1 O7 2.046(8) . ?
Ni1 O7 2.046(7) 2_665 ?
Ni1 O7 2.046(7) 3_565 ?
Cl1 O9 1.387(8) . ?
Cl1 O11 1.407(10) . ?
Cl1 O12 1.427(9) . ?
Cl1 O10 1.445(9) . ?
Cl2 O15B 1.394(18) . ?
Cl2 O16 1.412(16) . ?
Cl2 O14 1.413(19) . ?
Cl2 O13B 1.42(3) . ?
Cl2 O16B 1.44(2) . ?
Cl2 O15 1.45(2) . ?
Cl2 O13 1.46(2) . ?
Cl2 O14B 1.456(19) . ?

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 Ti1 O4 89.5(3) . 3_565 ?
O4 Ti1 O4 89.5(3) . 2_665 ?
O4 Ti1 O4 89.5(3) 3_565 2_665 ?
O4 Ti1 O1 90.2(2) . . ?
O4 Ti1 O1 178.8(3) 3_565 . ?
O4 Ti1 O1 89.3(2) 2_665 . ?
O4 Ti1 O1 178.8(3) . 2_665 ?
O4 Ti1 O1 89.3(2) 3_565 2_665 ?
O4 Ti1 O1 90.2(3) 2_665 2_665 ?
O1 Ti1 O1 91.0(3) . 2_665 ?
O4 Ti1 O1 89.3(2) . 3_565 ?
O4 Ti1 O1 90.2(3) 3_565 3_565 ?
O4 Ti1 O1 178.8(3) 2_665 3_565 ?
O1 Ti1 O1 91.0(3) . 3_565 ?
O1 Ti1 O1 91.0(3) 2_665 3_565 ?
O3 Mo1 O2 105.9(3) . . ?
O3 Mo1 O1 105.9(3) . . ?
O2 Mo1 O1 107.6(3) . . ?
O3 Mo1 N2 88.9(3) . . ?
O2 Mo1 N2 87.0(3) . . ?
O1 Mo1 N2 154.9(3) . . ?
O3 Mo1 N3 88.3(3) . . ?
O2 Mo1 N3 155.9(3) . . ?
O1 Mo1 N3 86.3(3) . . ?
N2 Mo1 N3 73.7(3) . . ?
O3 Mo1 N1 156.2(3) . . ?
O2 Mo1 N1 88.6(3) . . ?
O1 Mo1 N1 86.8(3) . . ?
N2 Mo1 N1 72.9(3) . . ?
N3 Mo1 N1 72.2(3) . . ?
Mo1 O1 Ti1 136.8(4) . . ?
C6 N1 C1 112.0(8) . . ?
C6 N1 Mo1 107.8(5) . . ?
C1 N1 Mo1 114.9(6) . . ?
N1 C1 C2 109.2(7) . . ?
N2 C2 C1 110.6(7) . . ?
C2 N2 C3 112.9(7) . . ?
C2 N2 Mo1 108.7(5) . . ?
C3 N2 Mo1 114.3(5) . . ?
N2 C3 C4 112.2(7) . . ?
N3 C4 C3 108.8(8) . . ?
C4 N3 C5 113.7(7) . . ?
C4 N3 Mo1 106.5(5) . . ?
C5 N3 Mo1 116.5(5) . . ?
N3 C5 C6 110.2(7) . . ?
N1 C6 C5 110.3(7) . . ?
O6 Mo2 O5 106.1(3) . . ?
O6 Mo2 O4 105.5(3) . . ?
O5 Mo2 O4 107.3(3) . . ?
O6 Mo2 N5 87.2(3) . . ?
O5 Mo2 N5 89.6(3) . . ?
O4 Mo2 N5 154.6(3) . . ?
O6 Mo2 N6 89.8(3) . . ?
O5 Mo2 N6 155.7(3) . . ?
O4 Mo2 N6 85.1(3) . . ?
N5 Mo2 N6 72.7(3) . . ?
O6 Mo2 N4 156.4(3) . . ?
O5 Mo2 N4 87.2(3) . . ?
O4 Mo2 N4 88.4(3) . . ?
N5 Mo2 N4 73.3(3) . . ?
N6 Mo2 N4 72.1(3) . . ?
Mo2 O4 Ti1 144.6(4) . . ?
C7 N4 C12 114.7(8) . . ?
C7 N4 Mo2 107.5(6) . . ?
C12 N4 Mo2 114.7(5) . . ?
N4 C7 C8 110.5(8) . . ?
N5 C8 C7 112.6(8) . . ?
C9 N5 C8 113.1(8) . . ?
C9 N5 Mo2 107.6(6) . . ?
C8 N5 Mo2 115.2(6) . . ?
N5 C9 C10 110.8(8) . . ?
N6 C10 C9 108.6(8) . . ?
C10 N6 C11 113.6(8) . . ?
C10 N6 Mo2 115.8(6) . . ?
C11 N6 Mo2 106.7(6) . . ?
C12 C11 N6 110.6(8) . . ?
C11 C12 N4 111.1(8) . . ?
O8 Ni1 O8 92.7(3) 2_665 3_565 ?
O8 Ni1 O8 92.7(3) 2_665 . ?
O8 Ni1 O8 92.7(3) 3_565 . ?
O8 Ni1 O7 93.3(4) 2_665 . ?
O8 Ni1 O7 173.7(4) 3_565 . ?
O8 Ni1 O7 85.0(3) . . ?
O8 Ni1 O7 85.0(3) 2_665 2_665 ?
O8 Ni1 O7 93.3(4) 3_565 2_665 ?
O8 Ni1 O7 173.7(4) . 2_665 ?
O7 Ni1 O7 89.3(3) . 2_665 ?
O8 Ni1 O7 173.7(4) 2_665 3_565 ?
O8 Ni1 O7 85.0(3) 3_565 3_565 ?
O8 Ni1 O7 93.3(4) . 3_565 ?
O7 Ni1 O7 89.3(3) . 3_565 ?
O7 Ni1 O7 89.3(3) 2_665 3_565 ?
O9 Cl1 O11 108.2(7) . . ?
O9 Cl1 O12 109.2(6) . . ?
O11 Cl1 O12 109.7(7) . . ?
O9 Cl1 O10 113.2(7) . . ?
O11 Cl1 O10 108.4(6) . . ?
O12 Cl1 O10 108.1(6) . . ?
O16 Cl2 O14 111.0(13) . . ?
O15B Cl2 O13B 110.7(15) . . ?
O15B Cl2 O16B 109.3(16) . . ?
O13B Cl2 O16B 110.3(17) . . ?
O16 Cl2 O15 106.4(14) . . ?
O14 Cl2 O15 109.7(15) . . ?
O16 Cl2 O13 111.8(11) . . ?
O14 Cl2 O13 111.4(15) . . ?
O15 Cl2 O13 106.3(15) . . ?
O15B Cl2 O14B 111.1(12) . . ?
O13B Cl2 O14B 109(2) . . ?
O16B Cl2 O14B 106.8(15) . . ?

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 2.12 3.041(9) 151.5 2_665 yes
N2 H2 O15^a 1.00 2.42 3.16(4) 130.4 3_566 yes
N2 H2 O15B^b 1.00 2.03 2.93(2) 148.4 3_566 yes
N3 H3 O6 1.00 1.96 2.924(10) 161.0 . yes
N4 H4 O5 1.00 2.03 2.989(9) 160.5 3_565 yes
N6 H6 O3 1.00 1.92 2.880(9) 159.0 . yes
O7 H7W O16^a 0.849(12) 1.97(2) 2.798(18) 165(9) . yes
O7 H7W O16B^b 0.849(12) 1.87(3) 2.71(3) 172(9) . yes
O7 H7WA O2 0.845(10) 1.844(11) 2.678(9) 169(5) 2_664 yes
O8 H8W O10 0.844(12) 1.983(16) 2.826(12) 176(14) . yes
O8 H8WA O5 0.849(12) 1.836(12) 2.664(10) 164(7) . yes

_refine_diff_density_max         2.483
_refine_diff_density_min         -1.447
_refine_diff_density_rms         0.144



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

data_FeZrMo6
_database_code_depnum_ccdc_archive 'CCDC 2372558'
loop_
_audit_author_name
_audit_author_address
'Ryoji Mitsuhashi'
;Kanazawa University
Japan
;
_audit_update_record             
;
2024-07-22 deposited with the CCDC.	2024-09-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H90 Mo6 N18 O18 Zr, H12 Fe O6, 6(Cl O4)'
_chemical_formula_sum            'C36 H102 Cl6 Fe Mo6 N18 O48 Zr'
_chemical_formula_weight         2490.76

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'
Fe Fe 0.3463 0.8444 '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'

_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_H-M_alt        'R 3 :H'
_space_group_name_Hall           'R 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.
;

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'

_cell_length_a                   21.8319(4)
_cell_length_b                   21.8319(4)
_cell_length_c                   14.7616(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     6093.2(3)
_cell_formula_units_Z            3
_cell_measurement_temperature    102(2)
_cell_measurement_reflns_used    8062
_cell_measurement_theta_min      2.9210
_cell_measurement_theta_max      29.7740

_exptl_crystal_description       plate
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.036
_exptl_crystal_F_000             3744
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    1.498
_shelx_estimated_absorpt_T_min   0.865
_shelx_estimated_absorpt_T_max   0.943
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.95349
_exptl_absorpt_correction_T_max  1.00000
_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_absorpt_special_details   ?
_diffrn_ambient_temperature      102(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10009
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.558
_diffrn_reflns_theta_max         27.481
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.877
_diffrn_reflns_point_group_measured_fraction_full 0.901
_reflns_number_total             5470
_reflns_number_gt                5319
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.759
_reflns_Friedel_fraction_max     0.757
_reflns_Friedel_fraction_full    0.802

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

_computing_data_collection       'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0387P)²+24.1811P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2217 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.019(18)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5470
_refine_ls_number_parameters     399
_refine_ls_number_restraints     152
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0308
_refine_ls_wR_factor_ref         0.0790
_refine_ls_wR_factor_gt          0.0785
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_restrained_S_all      1.079
_refine_ls_shift/su_max          0.001
_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
Zr1 Zr 0.666667 0.333333 0.32105(7) 0.00993(19) Uani 1 3 d S T P . .
Mo1 Mo 0.52024(3) 0.25926(2) 0.47702(3) 0.01163(12) Uani 1 1 d . . . . .
O1 O 0.5860(2) 0.2592(2) 0.4018(3) 0.0159(9) Uani 1 1 d . . . . .
O2 O 0.5651(2) 0.3124(2) 0.5680(3) 0.0188(10) Uani 1 1 d D . . . .
O3 O 0.4836(2) 0.3009(2) 0.4190(3) 0.0181(9) Uani 1 1 d . . . . .
N1 N 0.5237(3) 0.1667(3) 0.5491(4) 0.0143(10) Uani 1 1 d . . . . .
H1 H 0.572404 0.185998 0.574571 0.017 Uiso 1 1 calc R U . . .
C1 C 0.4731(4) 0.1350(4) 0.6256(5) 0.0227(15) Uani 1 1 d . . . . .
H1A H 0.497819 0.129848 0.678856 0.027 Uiso 1 1 calc R U . . .
H1B H 0.434605 0.087319 0.608291 0.027 Uiso 1 1 calc R U . . .
C2 C 0.4423(4) 0.1812(4) 0.6501(5) 0.0236(15) Uani 1 1 d . . . . .
H2 H 0.399550 0.154194 0.687848 0.028 Uiso 1 1 calc R U . . .
H2A H 0.477220 0.222621 0.685273 0.028 Uiso 1 1 calc R U . . .
N2 N 0.4236(3) 0.2052(3) 0.5652(4) 0.0179(11) Uani 1 1 d . . . . .
H2B H 0.412101 0.242406 0.583570 0.021 Uiso 1 1 calc R U . . .
C3 C 0.3593(3) 0.1483(4) 0.5207(5) 0.0242(15) Uani 1 1 d . . . . .
H3 H 0.319148 0.156402 0.531620 0.029 Uiso 1 1 calc R U . . .
H3A H 0.347326 0.102188 0.547847 0.029 Uiso 1 1 calc R U . . .
C4 C 0.3699(3) 0.1460(4) 0.4201(5) 0.0236(15) Uani 1 1 d . . . . .
H4 H 0.333689 0.099775 0.395305 0.028 Uiso 1 1 calc R U . . .
H4A H 0.365039 0.183653 0.389407 0.028 Uiso 1 1 calc R U . . .
N3 N 0.4419(3) 0.1565(3) 0.4036(4) 0.0150(10) Uani 1 1 d . . . . .
H3B H 0.451382 0.165581 0.337265 0.018 Uiso 1 1 calc R U . . .
C5 C 0.4469(4) 0.0923(3) 0.4252(5) 0.0216(14) Uani 1 1 d . . . . .
H5 H 0.447637 0.068635 0.368294 0.026 Uiso 1 1 calc R U . . .
H5A H 0.405054 0.058601 0.460769 0.026 Uiso 1 1 calc R U . . .
C6 C 0.5140(4) 0.1133(4) 0.4792(5) 0.0224(15) Uani 1 1 d . . . . .
H6 H 0.510585 0.071052 0.508860 0.027 Uiso 1 1 calc R U . . .
H6A H 0.555322 0.133412 0.437981 0.027 Uiso 1 1 calc R U . . .
Mo2 Mo 0.52040(3) 0.28845(3) 0.16153(3) 0.01284(12) Uani 1 1 d . . . . .
O4 O 0.5919(2) 0.3384(2) 0.2395(3) 0.0167(9) Uani 1 1 d . . . . .
O5 O 0.5558(2) 0.2670(3) 0.0702(3) 0.0193(10) Uani 1 1 d . . . . .
O6 O 0.4643(3) 0.2103(2) 0.2156(3) 0.0194(10) Uani 1 1 d . . . . .
N4 N 0.5546(3) 0.3958(3) 0.0895(4) 0.0169(11) Uani 1 1 d . . . . .
H4B H 0.606932 0.419450 0.080287 0.020 Uiso 1 1 calc R U . . .
C7 C 0.5221(4) 0.3797(4) -0.0006(5) 0.0263(16) Uani 1 1 d . . . . .
H7 H 0.544914 0.359600 -0.038984 0.032 Uiso 1 1 calc R U . . .
H7A H 0.529410 0.423754 -0.029504 0.032 Uiso 1 1 calc R U . . .
C8 C 0.4444(4) 0.3279(4) 0.0064(5) 0.0277(16) Uani 1 1 d . . . . .
H8 H 0.419361 0.353508 0.023112 0.033 Uiso 1 1 calc R U . . .
H8A H 0.426619 0.305625 -0.053448 0.033 Uiso 1 1 calc R U . . .
N5 N 0.4283(3) 0.2721(3) 0.0742(4) 0.0186(12) Uani 1 1 d . . . . .
H5B H 0.411612 0.226793 0.040355 0.022 Uiso 1 1 calc R U . . .
C9 C 0.3697(4) 0.2617(4) 0.1372(6) 0.0294(17) Uani 1 1 d . . . . .
H9 H 0.352998 0.217364 0.171884 0.035 Uiso 1 1 calc R U . . .
H9A H 0.329460 0.257829 0.101668 0.035 Uiso 1 1 calc R U . . .
C10 C 0.3967(4) 0.3243(4) 0.2023(6) 0.0257(16) Uani 1 1 d . . . . .
H10 H 0.399474 0.365634 0.170664 0.031 Uiso 1 1 calc R U . . .
H10A H 0.363515 0.312030 0.253827 0.031 Uiso 1 1 calc R U . . .
N6 N 0.4664(3) 0.3419(3) 0.2355(4) 0.0192(11) Uani 1 1 d . . . . .
H6B H 0.460029 0.325503 0.299905 0.023 Uiso 1 1 calc R U . . .
C11 C 0.5406(4) 0.4458(4) 0.1427(6) 0.0284(16) Uani 1 1 d . . . . .
H11 H 0.584052 0.492865 0.144383 0.034 Uiso 1 1 calc R U . . .
H11A H 0.503102 0.451138 0.112447 0.034 Uiso 1 1 calc R U . . .
C12 C 0.5183(4) 0.4202(4) 0.2368(5) 0.0271(16) Uani 1 1 d . . . . .
H12 H 0.496006 0.445543 0.264589 0.032 Uiso 1 1 calc R U . . .
H12A H 0.560147 0.429899 0.273546 0.032 Uiso 1 1 calc R U . . .
Cl1 Cl 0.69935(9) 0.59213(9) 0.92472(13) 0.0279(4) Uani 1 1 d . . . . .
O9 O 0.6720(4) 0.5419(4) 0.8522(5) 0.0514(18) Uani 1 1 d . . . . .
O10 O 0.6560(4) 0.5605(4) 1.0031(5) 0.0572(19) Uani 1 1 d . . . . .
O11 O 0.6971(4) 0.6536(3) 0.8977(6) 0.055(2) Uani 1 1 d . . . . .
O12 O 0.7695(3) 0.6119(4) 0.9459(5) 0.0531(19) Uani 1 1 d . . . . .
Fe1 Fe 0.666667 0.333333 0.81604(14) 0.0259(4) Uani 1 3 d DS T P . .
O7 O 0.6108(3) 0.3679(3) 0.7334(4) 0.0352(13) Uani 1 1 d D . . . .
H7WA H 0.607(4) 0.3559(11) 0.6760(15) 0.053 Uiso 1 1 d D U . . .
H7W H 0.577(4) 0.380(6) 0.713(7) 0.053 Uiso 1 1 d D U . . .
O8 O 0.6844(4) 0.4208(3) 0.8936(4) 0.0386(14) Uani 1 1 d D . . . .
H8W H 0.679(6) 0.455(4) 0.873(6) 0.058 Uiso 1 1 d D U . . .
H8WA H 0.672(8) 0.416(4) 0.949(3) 0.12(7) Uiso 1 1 d D . . . .
Cl2 Cl 0.44065(8) 0.35715(9) 0.72397(11) 0.0201(3) Uani 1 1 d . U . . .
O13 O 0.3966(10) 0.3872(11) 0.7457(11) 0.027(3) Uani 0.67(4) 1 d . U P A 1
O14 O 0.3915(7) 0.2910(7) 0.6878(14) 0.046(5) Uani 0.67(4) 1 d . U P A 1
O15 O 0.4871(8) 0.4026(9) 0.6523(13) 0.042(4) Uani 0.67(4) 1 d D U P A 1
O16 O 0.4911(7) 0.3730(12) 0.7920(7) 0.044(5) Uani 0.67(4) 1 d . U P A 1
O13B O 0.407(2) 0.385(2) 0.777(3) 0.047(10) Uani 0.33(4) 1 d . U P A 2
O14B O 0.4008(12) 0.2797(11) 0.738(3) 0.041(7) Uani 0.33(4) 1 d . U P A 2
O15B O 0.464(2) 0.370(3) 0.6346(15) 0.043(8) Uani 0.33(4) 1 d . U P A 2
O16B O 0.4841(13) 0.3357(16) 0.780(2) 0.048(7) Uani 0.33(4) 1 d . U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr1 O1 2.072(4) 2_655 ?
Zr1 O1 2.072(4) . ?
Zr1 O1 2.072(4) 3_665 ?
Zr1 O4 2.075(4) . ?
Zr1 O4 2.075(4) 2_655 ?
Zr1 O4 2.075(4) 3_665 ?
Mo1 O3 1.710(5) . ?
Mo1 O2 1.725(5) . ?
Mo1 O1 1.815(5) . ?
Mo1 N2 2.246(5) . ?
Mo1 N3 2.301(5) . ?
Mo1 N1 2.319(5) . ?
N1 C1 1.487(9) . ?
N1 C6 1.490(9) . ?
C1 C2 1.509(10) . ?
C2 N2 1.492(9) . ?
N2 C3 1.484(9) . ?
C3 C4 1.508(10) . ?
C4 N3 1.490(8) . ?
N3 C5 1.494(8) . ?
C5 C6 1.524(10) . ?
Mo2 O6 1.720(5) . ?
Mo2 O5 1.730(5) . ?
Mo2 O4 1.802(5) . ?
Mo2 N5 2.261(6) . ?
Mo2 N6 2.305(6) . ?
Mo2 N4 2.329(5) . ?
N4 C7 1.465(9) . ?
N4 C11 1.496(9) . ?
C7 C8 1.499(10) . ?
C8 N5 1.475(9) . ?
N5 C9 1.504(9) . ?
C9 C10 1.528(11) . ?
C10 N6 1.457(9) . ?
N6 C12 1.508(9) . ?
C11 C12 1.485(11) . ?
Cl1 O12 1.402(6) . ?
Cl1 O11 1.423(7) . ?
Cl1 O9 1.433(7) . ?
Cl1 O10 1.435(7) . ?
Fe1 O8 2.090(6) 3_665 ?
Fe1 O8 2.090(6) 2_655 ?
Fe1 O8 2.090(6) . ?
Fe1 O7 2.114(6) 2_655 ?
Fe1 O7 2.114(6) 3_665 ?
Fe1 O7 2.114(6) . ?
Cl2 O15B 1.39(2) . ?
Cl2 O16 1.400(10) . ?
Cl2 O13B 1.40(3) . ?
Cl2 O14 1.405(11) . ?
Cl2 O13 1.446(13) . ?
Cl2 O15 1.458(12) . ?
Cl2 O14B 1.48(2) . ?
Cl2 O16B 1.49(2) . ?
O14B O16B 1.72(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 90.22(18) 2_655 . ?
O1 Zr1 O1 90.22(18) 2_655 3_665 ?
O1 Zr1 O1 90.22(18) . 3_665 ?
O1 Zr1 O4 179.14(18) 2_655 . ?
O1 Zr1 O4 89.47(17) . . ?
O1 Zr1 O4 90.59(17) 3_665 . ?
O1 Zr1 O4 89.48(17) 2_655 2_655 ?
O1 Zr1 O4 90.59(17) . 2_655 ?
O1 Zr1 O4 179.1(2) 3_665 2_655 ?
O4 Zr1 O4 89.72(19) . 2_655 ?
O1 Zr1 O4 90.59(17) 2_655 3_665 ?
O1 Zr1 O4 179.14(19) . 3_665 ?
O1 Zr1 O4 89.48(17) 3_665 3_665 ?
O4 Zr1 O4 89.72(19) . 3_665 ?
O4 Zr1 O4 89.72(19) 2_655 3_665 ?
O3 Mo1 O2 107.0(2) . . ?
O3 Mo1 O1 105.9(2) . . ?
O2 Mo1 O1 107.1(2) . . ?
O3 Mo1 N2 90.2(2) . . ?
O2 Mo1 N2 88.3(2) . . ?
O1 Mo1 N2 152.8(2) . . ?
O3 Mo1 N3 88.0(2) . . ?
O2 Mo1 N3 156.6(2) . . ?
O1 Mo1 N3 85.05(19) . . ?
N2 Mo1 N3 73.5(2) . . ?
O3 Mo1 N1 157.0(2) . . ?
O2 Mo1 N1 88.5(2) . . ?
O1 Mo1 N1 84.8(2) . . ?
N2 Mo1 N1 73.01(19) . . ?
N3 Mo1 N1 72.48(19) . . ?
Mo1 O1 Zr1 135.7(2) . . ?
C1 N1 C6 112.3(5) . . ?
C1 N1 Mo1 114.4(4) . . ?
C6 N1 Mo1 108.0(4) . . ?
N1 C1 C2 110.2(5) . . ?
N2 C2 C1 109.1(6) . . ?
C3 N2 C2 112.8(5) . . ?
C3 N2 Mo1 115.5(4) . . ?
C2 N2 Mo1 108.7(4) . . ?
N2 C3 C4 111.5(5) . . ?
N3 C4 C3 108.9(5) . . ?
C4 N3 C5 112.8(5) . . ?
C4 N3 Mo1 106.6(4) . . ?
C5 N3 Mo1 116.5(4) . . ?
N3 C5 C6 109.8(5) . . ?
N1 C6 C5 109.7(5) . . ?
O6 Mo2 O5 106.6(2) . . ?
O6 Mo2 O4 106.0(2) . . ?
O5 Mo2 O4 107.0(2) . . ?
O6 Mo2 N5 88.4(2) . . ?
O5 Mo2 N5 89.7(2) . . ?
O4 Mo2 N5 153.2(2) . . ?
O6 Mo2 N6 89.5(2) . . ?
O5 Mo2 N6 156.4(2) . . ?
O4 Mo2 N6 84.2(2) . . ?
N5 Mo2 N6 73.2(2) . . ?
O6 Mo2 N4 157.0(2) . . ?
O5 Mo2 N4 87.4(2) . . ?
O4 Mo2 N4 86.4(2) . . ?
N5 Mo2 N4 73.2(2) . . ?
N6 Mo2 N4 72.27(19) . . ?
Mo2 O4 Zr1 143.6(3) . . ?
C7 N4 C11 113.6(6) . . ?
C7 N4 Mo2 107.4(4) . . ?
C11 N4 Mo2 114.5(4) . . ?
N4 C7 C8 110.3(6) . . ?
N5 C8 C7 112.5(6) . . ?
C8 N5 C9 112.2(6) . . ?
C8 N5 Mo2 115.5(4) . . ?
C9 N5 Mo2 107.0(5) . . ?
N5 C9 C10 109.6(6) . . ?
N6 C10 C9 109.3(6) . . ?
C10 N6 C12 113.3(6) . . ?
C10 N6 Mo2 116.0(5) . . ?
C12 N6 Mo2 107.2(4) . . ?
C12 C11 N4 111.4(6) . . ?
C11 C12 N6 109.5(6) . . ?
O12 Cl1 O11 108.6(4) . . ?
O12 Cl1 O9 112.1(5) . . ?
O11 Cl1 O9 108.4(4) . . ?
O12 Cl1 O10 108.9(5) . . ?
O11 Cl1 O10 110.7(5) . . ?
O9 Cl1 O10 108.2(5) . . ?
O8 Fe1 O8 92.9(3) 3_665 2_655 ?
O8 Fe1 O8 92.9(3) 3_665 . ?
O8 Fe1 O8 92.9(3) 2_655 . ?
O8 Fe1 O7 95.5(3) 3_665 2_655 ?
O8 Fe1 O7 82.3(2) 2_655 2_655 ?
O8 Fe1 O7 170.5(3) . 2_655 ?
O8 Fe1 O7 82.3(2) 3_665 3_665 ?
O8 Fe1 O7 170.5(3) 2_655 3_665 ?
O8 Fe1 O7 95.5(3) . 3_665 ?
O7 Fe1 O7 90.0(2) 2_655 3_665 ?
O8 Fe1 O7 170.5(3) 3_665 . ?
O8 Fe1 O7 95.5(3) 2_655 . ?
O8 Fe1 O7 82.3(2) . . ?
O7 Fe1 O7 90.0(2) 2_655 . ?
O7 Fe1 O7 90.0(2) 3_665 . ?
O15B Cl2 O13B 132(3) . . ?
O16 Cl2 O14 128.9(18) . . ?
O16 Cl2 O13 110.4(8) . . ?
O14 Cl2 O13 102.2(11) . . ?
O16 Cl2 O15 99.2(13) . . ?
O14 Cl2 O15 109.7(8) . . ?
O13 Cl2 O15 104.2(10) . . ?
O15B Cl2 O14B 107.9(17) . . ?
O13B Cl2 O14B 106(2) . . ?
O15B Cl2 O16B 110.6(18) . . ?
O13B Cl2 O16B 112.1(18) . . ?
O14B Cl2 O16B 71(2) . . ?
Cl2 O14B O16B 55.2(14) . . ?
Cl2 O16B O14B 54.3(13) . . ?

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 47.1(4) . . . . ?
O2 Mo1 O1 Zr1 -66.8(4) . . . . ?
N2 Mo1 O1 Zr1 171.2(3) . . . . ?
N3 Mo1 O1 Zr1 133.6(4) . . . . ?
N1 Mo1 O1 Zr1 -153.6(4) . . . . ?
C6 N1 C1 C2 -135.6(6) . . . . ?
Mo1 N1 C1 C2 -11.9(7) . . . . ?
N1 C1 C2 N2 43.4(8) . . . . ?
C1 C2 N2 C3 74.0(7) . . . . ?
C1 C2 N2 Mo1 -55.5(6) . . . . ?
C2 N2 C3 C4 -134.3(6) . . . . ?
Mo1 N2 C3 C4 -8.4(7) . . . . ?
N2 C3 C4 N3 41.5(8) . . . . ?
C3 C4 N3 C5 75.5(7) . . . . ?
C3 C4 N3 Mo1 -53.6(6) . . . . ?
C4 N3 C5 C6 -134.8(6) . . . . ?
Mo1 N3 C5 C6 -11.0(7) . . . . ?
C1 N1 C6 C5 73.3(7) . . . . ?
Mo1 N1 C6 C5 -53.8(6) . . . . ?
N3 C5 C6 N1 42.6(7) . . . . ?
O6 Mo2 O4 Zr1 51.6(5) . . . . ?
O5 Mo2 O4 Zr1 -61.9(5) . . . . ?
N5 Mo2 O4 Zr1 171.7(4) . . . . ?
N6 Mo2 O4 Zr1 139.4(5) . . . . ?
N4 Mo2 O4 Zr1 -148.1(4) . . . . ?
C11 N4 C7 C8 -77.1(7) . . . . ?
Mo2 N4 C7 C8 50.6(7) . . . . ?
N4 C7 C8 N5 -40.0(9) . . . . ?
C7 C8 N5 C9 131.6(7) . . . . ?
C7 C8 N5 Mo2 8.6(8) . . . . ?
C8 N5 C9 C10 -72.3(8) . . . . ?
Mo2 N5 C9 C10 55.3(6) . . . . ?
N5 C9 C10 N6 -43.8(8) . . . . ?
C9 C10 N6 C12 136.3(6) . . . . ?
C9 C10 N6 Mo2 11.6(7) . . . . ?
C7 N4 C11 C12 133.2(6) . . . . ?
Mo2 N4 C11 C12 9.2(7) . . . . ?
N4 C11 C12 N6 -42.6(8) . . . . ?
C10 N6 C12 C11 -73.5(8) . . . . ?
Mo2 N6 C12 C11 55.8(7) . . . . ?
O15B Cl2 O14B O16B 106(2) . . . . ?
O13B Cl2 O14B O16B -108(2) . . . . ?
O15B Cl2 O16B O14B -102.5(19) . . . . ?
O13B Cl2 O16B O14B 100(3) . . . . ?

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(7) 152.7 2_655 yes
N2 H2B O14^a 1.00 2.04 2.930(13) 146.7 . yes
N3 H3B O6 1.00 2.00 2.957(7) 160.5 . yes
N4 H4B O5 1.00 2.07 3.045(7) 165.9 3_665 yes
N5 H5B O12 1.00 1.93 2.901(9) 163.6 2_654 yes
N6 H6B O3 1.00 1.98 2.935(8) 158.7 . yes
O7 H7WA O2 0.88(2) 1.847(14) 2.685(7) 159(6) . yes
O8 H8W O9 0.87(3) 2.00(4) 2.854(9) 167(10) . yes
O8 H8WA O5 0.85(3) 1.95(10) 2.665(8) 141(15) 3_666 yes
O7 H7W O15^a 0.96(3) 2.41(3) 3.369(16) 175(9) . yes
O7 H7W O15B^b 0.96(3) 2.62(5) 3.53(3) 161(9) . yes

_refine_diff_density_max         0.745
_refine_diff_density_min         -1.606
_refine_diff_density_rms         0.109



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

data_NiZrMo6
_database_code_depnum_ccdc_archive 'CCDC 2372560'
loop_
_audit_author_name
_audit_author_address
'Ryoji Mitsuhashi'
;Kanazawa University
Japan
;
_audit_update_record             
;
2024-07-22 deposited with the CCDC.	2024-09-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_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

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'

_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_H-M_alt        'R 3 :H'
_space_group_name_Hall           'R 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.
;

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'

_cell_length_a                   21.7869(4)
_cell_length_b                   21.7869(4)
_cell_length_c                   14.6803(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     6034.7(3)
_cell_formula_units_Z            3
_cell_measurement_temperature    102(2)
_cell_measurement_reflns_used    6994
_cell_measurement_theta_min      2.5660
_cell_measurement_theta_max      30.0500

_exptl_crystal_description       plate
_exptl_crystal_colour            'pale green'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.058
_exptl_crystal_F_000             3750
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    1.566
_shelx_estimated_absorpt_T_min   0.885
_shelx_estimated_absorpt_T_max   0.940
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.97140
_exptl_absorpt_correction_T_max  1.00000
_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_absorpt_special_details   ?
_diffrn_ambient_temperature      102(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8842
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_av_R_equivalents  0.0194
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.566
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.869
_diffrn_reflns_point_group_measured_fraction_full 0.892
_reflns_number_total             5351
_reflns_number_gt                5241
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.746
_reflns_Friedel_fraction_max     0.742
_reflns_Friedel_fraction_full    0.785

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0499P)²+39.1925P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.00(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5351
_refine_ls_number_parameters     401
_refine_ls_number_restraints     202
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0337
_refine_ls_wR_factor_ref         0.0902
_refine_ls_wR_factor_gt          0.0897
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.001
_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
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 . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr1 O1 2.066(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_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_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) . . . . ?

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

_refine_diff_density_max         0.759
_refine_diff_density_min         -2.051
_refine_diff_density_rms         0.126



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

data_ZnZrMo6
_database_code_depnum_ccdc_archive 'CCDC 2372561'
loop_
_audit_author_name
_audit_author_address
'Ryoji Mitsuhashi'
;Kanazawa University
Japan
;
_audit_update_record             
;
2024-07-22 deposited with the CCDC.	2024-09-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H90 Mo6 N18 O18 Zr, H12 O6 Zn, 6(Cl O4)'
_chemical_formula_sum            'C36 H102 Cl6 Mo6 N18 O48 Zn Zr'
_chemical_formula_weight         2500.28

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'
Zn Zn 0.2839 1.4301 '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'

_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_H-M_alt        'R 3 :H'
_space_group_name_Hall           'R 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.
;

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'

_cell_length_a                   21.7780(3)
_cell_length_b                   21.7780(3)
_cell_length_c                   14.7532(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     6059.72(19)
_cell_formula_units_Z            3
_cell_measurement_temperature    102(2)
_cell_measurement_reflns_used    9360
_cell_measurement_theta_min      2.5350
_cell_measurement_theta_max      30.2120

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.055
_exptl_crystal_F_000             3756
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    1.623
_shelx_estimated_absorpt_T_min   0.781
_shelx_estimated_absorpt_T_max   0.909
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.95117
_exptl_absorpt_correction_T_max  1.00000
_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_absorpt_special_details   ?
_diffrn_ambient_temperature      102(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10949
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_av_R_equivalents  0.0183
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.563
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.817
_diffrn_reflns_point_group_measured_fraction_full 0.853
_reflns_number_total             5055
_reflns_number_gt                4990
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.636
_reflns_Friedel_fraction_max     0.635
_reflns_Friedel_fraction_full    0.707

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0363P)²+17.7532P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.15(2)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5055
_refine_ls_number_parameters     400
_refine_ls_number_restraints     169
_refine_ls_R_factor_all          0.0242
_refine_ls_R_factor_gt           0.0238
_refine_ls_wR_factor_ref         0.0640
_refine_ls_wR_factor_gt          0.0637
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_restrained_S_all      1.070
_refine_ls_shift/su_max          0.001
_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
Zr1 Zr 0.333333 0.666667 0.67369(5) 0.00825(15) Uani 1 3 d S T P . .
Mo1 Mo 0.40787(2) 0.59449(2) 0.82931(3) 0.01018(10) Uani 1 1 d . . . . .
O1 O 0.40773(19) 0.66041(19) 0.7545(2) 0.0144(7) Uani 1 1 d . . . . .
O2 O 0.35463(19) 0.5857(2) 0.9203(2) 0.0160(7) Uani 1 1 d D . . . .
O3 O 0.36612(19) 0.51616(19) 0.7715(2) 0.0160(7) Uani 1 1 d . . . . .
N1 N 0.5009(2) 0.6909(2) 0.9014(3) 0.0147(8) Uani 1 1 d . . . . .
H1 H 0.481586 0.720332 0.926933 0.018 Uiso 1 1 calc R U . . .
C1 C 0.5325(3) 0.6718(3) 0.9777(4) 0.0199(11) Uani 1 1 d . . . . .
H1A H 0.537570 0.701548 1.031029 0.024 Uiso 1 1 calc R U . . .
H1B H 0.580265 0.680959 0.960361 0.024 Uiso 1 1 calc R U . . .
C2 C 0.4864(3) 0.5947(3) 1.0020(3) 0.0201(11) Uani 1 1 d . . . . .
H2 H 0.513613 0.578874 1.039520 0.024 Uiso 1 1 calc R U . . .
H2A H 0.445011 0.588115 1.037731 0.024 Uiso 1 1 calc R U . . .
N2 N 0.4616(2) 0.5514(2) 0.9172(3) 0.0167(9) Uani 1 1 d . . . . .
H2B H 0.424472 0.502557 0.935613 0.020 Uiso 1 1 calc R U . . .
C3 C 0.5208(3) 0.5574(3) 0.7714(4) 0.0212(12) Uani 1 1 d . . . . .
H3 H 0.566853 0.566991 0.745936 0.025 Uiso 1 1 calc R U . . .
H3A H 0.482628 0.514742 0.741232 0.025 Uiso 1 1 calc R U . . .
C4 C 0.5193(3) 0.5447(3) 0.8727(4) 0.0224(12) Uani 1 1 d . . . . .
H4 H 0.511923 0.496690 0.883781 0.027 Uiso 1 1 calc R U . . .
H4A H 0.565447 0.579575 0.899445 0.027 Uiso 1 1 calc R U . . .
N3 N 0.5107(2) 0.6190(2) 0.7555(3) 0.0145(8) Uani 1 1 d . . . . .
H3B H 0.501468 0.619528 0.689150 0.017 Uiso 1 1 calc R U . . .
C5 C 0.5744(3) 0.6881(3) 0.7770(4) 0.0202(11) Uani 1 1 d . . . . .
H5 H 0.597831 0.712699 0.720059 0.024 Uiso 1 1 calc R U . . .
H5A H 0.608416 0.680034 0.812158 0.024 Uiso 1 1 calc R U . . .
C6 C 0.5538(3) 0.7342(3) 0.8315(4) 0.0201(11) Uani 1 1 d . . . . .
H6 H 0.596413 0.773048 0.861016 0.024 Uiso 1 1 calc R U . . .
H6A H 0.533645 0.755710 0.790674 0.024 Uiso 1 1 calc R U . . .
Mo2 Mo 0.37717(2) 0.56463(2) 0.51375(3) 0.01112(10) Uani 1 1 d . . . . .
O4 O 0.3277(2) 0.58674(19) 0.5922(2) 0.0156(7) Uani 1 1 d . . . . .
O5 O 0.3980(2) 0.62115(19) 0.4219(2) 0.0172(8) Uani 1 1 d . . . . .
O6 O 0.45557(19) 0.5869(2) 0.5673(3) 0.0176(8) Uani 1 1 d . . . . .
N4 N 0.2695(2) 0.4913(2) 0.4429(3) 0.0144(9) Uani 1 1 d . . . . .
H4B H 0.245617 0.519930 0.434166 0.017 Uiso 1 1 calc R U . . .
C7 C 0.2852(3) 0.4748(3) 0.3518(4) 0.0241(12) Uani 1 1 d . . . . .
H7 H 0.305178 0.517864 0.313436 0.029 Uiso 1 1 calc R U . . .
H7A H 0.240847 0.438007 0.323076 0.029 Uiso 1 1 calc R U . . .
C8 C 0.3367(3) 0.4491(3) 0.3583(4) 0.0247(12) Uani 1 1 d . . . . .
H8 H 0.310941 0.398075 0.374246 0.030 Uiso 1 1 calc R U . . .
H8A H 0.359191 0.453990 0.298372 0.030 Uiso 1 1 calc R U . . .
N5 N 0.3928(2) 0.4885(2) 0.4270(3) 0.0157(9) Uani 1 1 d . . . . .
H5B H 0.438210 0.517123 0.393082 0.019 Uiso 1 1 calc R U . . .
C9 C 0.3422(3) 0.4051(3) 0.5542(4) 0.0236(12) Uani 1 1 d . . . . .
H9 H 0.300698 0.366349 0.522828 0.028 Uiso 1 1 calc R U . . .
H9A H 0.355069 0.384461 0.605400 0.028 Uiso 1 1 calc R U . . .
C10 C 0.4037(3) 0.4409(3) 0.4892(5) 0.0265(13) Uani 1 1 d . . . . .
H10 H 0.448263 0.468823 0.523560 0.032 Uiso 1 1 calc R U . . .
H10A H 0.407703 0.404563 0.453484 0.032 Uiso 1 1 calc R U . . .
N6 N 0.3241(2) 0.4578(2) 0.5884(3) 0.0149(8) Uani 1 1 d . . . . .
H6B H 0.340924 0.468004 0.652589 0.018 Uiso 1 1 calc R U . . .
C11 C 0.2456(3) 0.4307(3) 0.5904(4) 0.0237(12) Uani 1 1 d . . . . .
H11 H 0.220717 0.382910 0.618213 0.028 Uiso 1 1 calc R U . . .
H11A H 0.235716 0.462674 0.627347 0.028 Uiso 1 1 calc R U . . .
C12 C 0.2197(3) 0.4272(3) 0.4960(4) 0.0244(12) Uani 1 1 d . . . . .
H12 H 0.172483 0.423344 0.497707 0.029 Uiso 1 1 calc R U . . .
H12A H 0.214625 0.384368 0.465647 0.029 Uiso 1 1 calc R U . . .
Zn1 Zn 0.333333 0.666667 1.16700(8) 0.0220(2) Uani 1 3 d S T P . .
O8 O 0.3995(3) 0.6460(3) 1.2444(3) 0.0343(11) Uani 1 1 d D . . . .
H8WA H 0.439(2) 0.653(5) 1.226(6) 0.052 Uiso 1 1 d D U . . .
H8W H 0.399(7) 0.646(5) 1.3020(9) 0.26(12) Uiso 1 1 d D . . . .
O7 O 0.2977(3) 0.5778(2) 1.0840(3) 0.0289(10) Uani 1 1 d D . . . .
H7W H 0.296(4) 0.539(2) 1.098(5) 0.043 Uiso 1 1 d D U . . .
H7WA H 0.309(2) 0.583(3) 1.0287(10) 0.043 Uiso 1 1 d D U . . .
Cl1 Cl 0.55733(8) 0.63356(7) 1.27572(10) 0.0255(3) Uani 1 1 d D . . . .
O9 O 0.6205(3) 0.6348(3) 1.2467(4) 0.0510(16) Uani 1 1 d D . . . .
O10 O 0.5345(3) 0.6631(3) 1.2048(3) 0.0454(13) Uani 1 1 d D . . . .
O11 O 0.5056(3) 0.5629(2) 1.2953(4) 0.0504(15) Uani 1 1 d D . . . .
O12 O 0.5705(4) 0.6760(3) 1.3550(4) 0.0543(15) Uani 1 1 d D . . . .
Cl2 Cl 0.30890(7) 0.41738(7) 1.07649(9) 0.0187(3) Uani 1 1 d D U . . .
O13 O 0.3210(18) 0.4717(14) 1.1407(12) 0.057(5) Uani 0.57(5) 1 d D U P A 1
O14 O 0.2798(12) 0.3491(10) 1.1184(19) 0.047(6) Uani 0.57(5) 1 d D U P A 1
O15 O 0.2622(7) 0.4156(9) 1.0073(13) 0.035(4) Uani 0.57(5) 1 d D U P A 1
O16 O 0.3748(8) 0.4341(11) 1.0381(12) 0.039(4) Uani 0.57(5) 1 d D U P A 1
O13B O 0.2876(12) 0.4502(8) 1.1423(12) 0.024(4) Uani 0.43(5) 1 d D U P A 2
O14B O 0.2788(17) 0.3441(9) 1.0964(16) 0.025(5) Uani 0.43(5) 1 d D U P A 2
O15B O 0.290(2) 0.4283(15) 0.9888(12) 0.059(8) Uani 0.43(5) 1 d D U P A 2
O16B O 0.3847(9) 0.4508(14) 1.078(3) 0.062(9) Uani 0.43(5) 1 d D U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr1 O4 2.068(4) 3_565 ?
Zr1 O4 2.068(4) 2_665 ?
Zr1 O4 2.068(4) . ?
Zr1 O1 2.070(4) 2_665 ?
Zr1 O1 2.070(4) 3_565 ?
Zr1 O1 2.070(4) . ?
Mo1 O3 1.707(4) . ?
Mo1 O2 1.720(4) . ?
Mo1 O1 1.812(4) . ?
Mo1 N2 2.243(4) . ?
Mo1 N3 2.300(4) . ?
Mo1 N1 2.321(4) . ?
N1 C6 1.481(7) . ?
N1 C1 1.484(7) . ?
C1 C2 1.507(8) . ?
C2 N2 1.495(7) . ?
N2 C4 1.488(7) . ?
C3 N3 1.483(7) . ?
C3 C4 1.516(8) . ?
N3 C5 1.485(7) . ?
C5 C6 1.519(8) . ?
Mo2 O6 1.717(4) . ?
Mo2 O5 1.731(4) . ?
Mo2 O4 1.803(4) . ?
Mo2 N5 2.252(4) . ?
Mo2 N6 2.296(4) . ?
Mo2 N4 2.323(4) . ?
N4 C7 1.475(7) . ?
N4 C12 1.491(7) . ?
C7 C8 1.488(8) . ?
C8 N5 1.485(7) . ?
N5 C10 1.489(7) . ?
C9 N6 1.475(7) . ?
C9 C10 1.509(9) . ?
N6 C11 1.504(7) . ?
C11 C12 1.491(8) . ?
Zn1 O8 2.058(4) 2_665 ?
Zn1 O8 2.058(5) 3_565 ?
Zn1 O8 2.058(4) . ?
Zn1 O7 2.084(4) 3_565 ?
Zn1 O7 2.084(4) . ?
Zn1 O7 2.084(4) 2_665 ?
Cl1 O11 1.409(5) . ?
Cl1 O9 1.426(5) . ?
Cl1 O12 1.429(5) . ?
Cl1 O10 1.442(5) . ?
Cl2 O16 1.412(11) . ?
Cl2 O15B 1.412(17) . ?
Cl2 O13B 1.414(13) . ?
Cl2 O14B 1.420(18) . ?
Cl2 O15 1.427(11) . ?
Cl2 O14 1.432(14) . ?
Cl2 O16B 1.432(18) . ?
Cl2 O13 1.433(13) . ?

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 O4 89.61(15) 3_565 2_665 ?
O4 Zr1 O4 89.61(15) 3_565 . ?
O4 Zr1 O4 89.61(15) 2_665 . ?
O4 Zr1 O1 90.34(14) 3_565 2_665 ?
O4 Zr1 O1 89.89(14) 2_665 2_665 ?
O4 Zr1 O1 179.49(17) . 2_665 ?
O4 Zr1 O1 89.88(14) 3_565 3_565 ?
O4 Zr1 O1 179.49(16) 2_665 3_565 ?
O4 Zr1 O1 90.34(14) . 3_565 ?
O1 Zr1 O1 90.16(15) 2_665 3_565 ?
O4 Zr1 O1 179.49(16) 3_565 . ?
O4 Zr1 O1 90.34(14) 2_665 . ?
O4 Zr1 O1 89.89(14) . . ?
O1 Zr1 O1 90.16(15) 2_665 . ?
O1 Zr1 O1 90.17(15) 3_565 . ?
O3 Mo1 O2 106.61(18) . . ?
O3 Mo1 O1 106.04(17) . . ?
O2 Mo1 O1 107.19(17) . . ?
O3 Mo1 N2 89.98(17) . . ?
O2 Mo1 N2 88.04(17) . . ?
O1 Mo1 N2 153.06(17) . . ?
O3 Mo1 N3 88.01(17) . . ?
O2 Mo1 N3 156.78(17) . . ?
O1 Mo1 N3 85.12(16) . . ?
N2 Mo1 N3 73.72(16) . . ?
O3 Mo1 N1 157.02(16) . . ?
O2 Mo1 N1 88.76(17) . . ?
O1 Mo1 N1 84.78(16) . . ?
N2 Mo1 N1 73.22(16) . . ?
N3 Mo1 N1 72.49(15) . . ?
Mo1 O1 Zr1 135.6(2) . . ?
C6 N1 C1 112.6(4) . . ?
C6 N1 Mo1 107.9(3) . . ?
C1 N1 Mo1 114.3(3) . . ?
N1 C1 C2 110.4(4) . . ?
N2 C2 C1 109.4(4) . . ?
C4 N2 C2 112.0(4) . . ?
C4 N2 Mo1 115.3(3) . . ?
C2 N2 Mo1 108.7(3) . . ?
N3 C3 C4 108.7(4) . . ?
N2 C4 C3 111.2(4) . . ?
C3 N3 C5 113.4(4) . . ?
C3 N3 Mo1 106.5(3) . . ?
C5 N3 Mo1 116.2(3) . . ?
N3 C5 C6 110.5(4) . . ?
N1 C6 C5 109.8(4) . . ?
O6 Mo2 O5 106.80(18) . . ?
O6 Mo2 O4 105.80(18) . . ?
O5 Mo2 O4 106.96(17) . . ?
O6 Mo2 N5 88.49(18) . . ?
O5 Mo2 N5 89.80(17) . . ?
O4 Mo2 N5 153.16(17) . . ?
O6 Mo2 N6 89.48(17) . . ?
O5 Mo2 N6 156.32(16) . . ?
O4 Mo2 N6 84.12(16) . . ?
N5 Mo2 N6 73.21(16) . . ?
O6 Mo2 N4 157.01(17) . . ?
O5 Mo2 N4 87.28(17) . . ?
O4 Mo2 N4 86.57(16) . . ?
N5 Mo2 N4 73.15(16) . . ?
N6 Mo2 N4 72.27(15) . . ?
Mo2 O4 Zr1 143.7(2) . . ?
C7 N4 C12 113.5(4) . . ?
C7 N4 Mo2 107.5(3) . . ?
C12 N4 Mo2 114.7(3) . . ?
N4 C7 C8 110.1(5) . . ?
N5 C8 C7 112.6(5) . . ?
C8 N5 C10 112.9(5) . . ?
C8 N5 Mo2 115.4(3) . . ?
C10 N5 Mo2 107.3(4) . . ?
N6 C9 C10 109.2(4) . . ?
N5 C10 C9 110.0(5) . . ?
C9 N6 C11 113.2(4) . . ?
C9 N6 Mo2 115.4(3) . . ?
C11 N6 Mo2 107.8(3) . . ?
C12 C11 N6 109.1(5) . . ?
C11 C12 N4 111.4(5) . . ?
O8 Zn1 O8 92.15(19) 2_665 3_565 ?
O8 Zn1 O8 92.15(19) 2_665 . ?
O8 Zn1 O8 92.15(19) 3_565 . ?
O8 Zn1 O7 83.73(19) 2_665 3_565 ?
O8 Zn1 O7 95.7(2) 3_565 3_565 ?
O8 Zn1 O7 171.3(2) . 3_565 ?
O8 Zn1 O7 171.3(2) 2_665 . ?
O8 Zn1 O7 83.73(19) 3_565 . ?
O8 Zn1 O7 95.7(2) . . ?
O7 Zn1 O7 88.99(19) 3_565 . ?
O8 Zn1 O7 95.7(2) 2_665 2_665 ?
O8 Zn1 O7 171.3(2) 3_565 2_665 ?
O8 Zn1 O7 83.73(19) . 2_665 ?
O7 Zn1 O7 88.99(19) 3_565 2_665 ?
O7 Zn1 O7 88.99(19) . 2_665 ?
O11 Cl1 O9 108.6(3) . . ?
O11 Cl1 O12 109.3(4) . . ?
O9 Cl1 O12 110.7(4) . . ?
O11 Cl1 O10 111.7(4) . . ?
O9 Cl1 O10 108.6(3) . . ?
O12 Cl1 O10 107.9(4) . . ?
O15B Cl2 O13B 110.4(12) . . ?
O15B Cl2 O14B 111.6(14) . . ?
O13B Cl2 O14B 110.0(12) . . ?
O16 Cl2 O15 109.9(8) . . ?
O16 Cl2 O14 107.8(11) . . ?
O15 Cl2 O14 110.0(10) . . ?
O15B Cl2 O16B 106.8(13) . . ?
O13B Cl2 O16B 108.3(14) . . ?
O14B Cl2 O16B 109.6(15) . . ?
O16 Cl2 O13 108.0(10) . . ?
O15 Cl2 O13 109.2(9) . . ?
O14 Cl2 O13 112.0(10) . . ?

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 46.6(3) . . . . ?
O2 Mo1 O1 Zr1 -67.0(3) . . . . ?
N2 Mo1 O1 Zr1 171.0(3) . . . . ?
N3 Mo1 O1 Zr1 133.1(3) . . . . ?
N1 Mo1 O1 Zr1 -154.1(3) . . . . ?
C6 N1 C1 C2 -135.3(5) . . . . ?
Mo1 N1 C1 C2 -11.7(5) . . . . ?
N1 C1 C2 N2 43.0(6) . . . . ?
C1 C2 N2 C4 73.7(5) . . . . ?
C1 C2 N2 Mo1 -54.9(5) . . . . ?
C2 N2 C4 C3 -134.6(5) . . . . ?
Mo1 N2 C4 C3 -9.5(6) . . . . ?
N3 C3 C4 N2 42.7(6) . . . . ?
C4 C3 N3 C5 74.7(6) . . . . ?
C4 C3 N3 Mo1 -54.3(5) . . . . ?
C3 N3 C5 C6 -134.4(5) . . . . ?
Mo1 N3 C5 C6 -10.6(5) . . . . ?
C1 N1 C6 C5 73.6(6) . . . . ?
Mo1 N1 C6 C5 -53.5(5) . . . . ?
N3 C5 C6 N1 42.4(6) . . . . ?
O6 Mo2 O4 Zr1 51.3(4) . . . . ?
O5 Mo2 O4 Zr1 -62.3(4) . . . . ?
N5 Mo2 O4 Zr1 171.2(3) . . . . ?
N6 Mo2 O4 Zr1 139.1(4) . . . . ?
N4 Mo2 O4 Zr1 -148.4(4) . . . . ?
C12 N4 C7 C8 -77.1(6) . . . . ?
Mo2 N4 C7 C8 50.9(5) . . . . ?
N4 C7 C8 N5 -39.4(7) . . . . ?
C7 C8 N5 C10 131.6(5) . . . . ?
C7 C8 N5 Mo2 7.7(6) . . . . ?
C8 N5 C10 C9 -72.6(6) . . . . ?
Mo2 N5 C10 C9 55.7(5) . . . . ?
N6 C9 C10 N5 -43.9(6) . . . . ?
C10 C9 N6 C11 136.3(5) . . . . ?
C10 C9 N6 Mo2 11.4(6) . . . . ?
C9 N6 C11 C12 -73.5(6) . . . . ?
Mo2 N6 C11 C12 55.4(5) . . . . ?
N6 C11 C12 N4 -42.4(6) . . . . ?
C7 N4 C12 C11 133.8(5) . . . . ?
Mo2 N4 C12 C11 9.6(6) . . . . ?

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 2.20 3.119(5) 152.6 2_665 yes
N2 H2B O16^a 1.00 2.02 2.908(16) 147.1 . yes
N2 H2B O16B^b 1.00 2.34 3.10(3) 131.6 . yes
N3 H3B O6 1.00 2.01 2.967(6) 160.0 . yes
N4 H4B O5 1.00 2.08 3.059(6) 164.7 3_565 yes
N5 H5B O11 1.00 1.94 2.908(7) 161.8 1_554 yes
N6 H6B O3 1.00 1.98 2.931(6) 158.9 . yes
O8 H8WA O10 0.849(13) 1.99(2) 2.832(7) 170(9) . yes
O8 H8W O5 0.849(14) 1.849(14) 2.671(6) 163(6) 1_556 yes
O7 H7W O13^a 0.844(13) 1.92(3) 2.733(17) 163(8) . yes
O7 H7W O13B^b 0.844(13) 1.97(2) 2.810(15) 175(7) . yes
O7 H7WA O2 0.844(13) 1.87(2) 2.681(6) 162(6) . yes

_refine_diff_density_max         0.533
_refine_diff_density_min         -1.556
_refine_diff_density_rms         0.094



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

data_CoZrMo6
_database_code_depnum_ccdc_archive 'CCDC 2372559'
loop_
_audit_author_name
_audit_author_address
'Ryoji Mitsuhashi'
;Kanazawa University
Japan
;
_audit_update_record             
;
2024-07-22 deposited with the CCDC.	2024-09-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H90 Mo6 N18 O18 Zr, H12 Co O6, 6(Cl O4)'
_chemical_formula_sum            'C36 H102 Cl6 Co Mo6 N18 O48 Zr'
_chemical_formula_weight         2493.84

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'
Co Co 0.3494 0.9721 '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'

_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_H-M_alt        'R 3 :H'
_space_group_name_Hall           'R 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.
;

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'

_cell_length_a                   21.7971(4)
_cell_length_b                   21.7971(4)
_cell_length_c                   14.7552(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     6071.2(3)
_cell_formula_units_Z            3
_cell_measurement_temperature    102(2)
_cell_measurement_reflns_used    11503
_cell_measurement_theta_min      2.5290
_cell_measurement_theta_max      29.9240

_exptl_crystal_description       plate
_exptl_crystal_colour            'pale pink'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.046
_exptl_crystal_F_000             3747
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    1.529
_shelx_estimated_absorpt_T_min   0.887
_shelx_estimated_absorpt_T_max   0.941
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.84418
_exptl_absorpt_correction_T_max  1.00000
_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_absorpt_special_details   ?
_diffrn_ambient_temperature      102(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17067
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.562
_diffrn_reflns_theta_max         28.489
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_point_group_measured_fraction_full 0.987
_reflns_number_total             6463
_reflns_number_gt                6121
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.910
_reflns_Friedel_fraction_max     0.897
_reflns_Friedel_fraction_full    0.975

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

_computing_data_collection       'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0535P)²+10.1962P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2739 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.004(15)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         6463
_refine_ls_number_parameters     411
_refine_ls_number_restraints     252
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0354
_refine_ls_wR_factor_ref         0.0902
_refine_ls_wR_factor_gt          0.0886
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_restrained_S_all      1.065
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr1 Zr 0.666667 0.333333 0.31935(7) 0.0116(2) Uani 1 3 d S T P . .
Mo1 Mo 0.74105(3) 0.48007(3) 0.47516(3) 0.01336(13) Uani 1 1 d . . . . .
O1 O 0.7408(3) 0.4138(2) 0.4000(3) 0.0183(10) Uani 1 1 d . . . . .
O2 O 0.6875(3) 0.4356(3) 0.5661(3) 0.0209(10) Uani 1 1 d D . . . .
O3 O 0.6996(2) 0.5169(3) 0.4175(3) 0.0192(10) Uani 1 1 d . . . . .
N1 N 0.8336(3) 0.4765(3) 0.5471(4) 0.0161(11) Uani 1 1 d . . . . .
H1 H 0.814258 0.427807 0.572600 0.019 Uiso 1 1 calc R U . . .
C1 C 0.8655(4) 0.5272(4) 0.6236(5) 0.0251(15) Uani 1 1 d . . . . .
H1A H 0.913224 0.565652 0.606120 0.030 Uiso 1 1 calc R U . . .
H1B H 0.870591 0.502397 0.676715 0.030 Uiso 1 1 calc R U . . .
C2 C 0.8198(4) 0.5585(4) 0.6486(4) 0.0223(14) Uani 1 1 d . . . . .
H2 H 0.778491 0.523842 0.684399 0.027 Uiso 1 1 calc R U . . .
H2A H 0.847302 0.601487 0.685927 0.027 Uiso 1 1 calc R U . . .
N2 N 0.7951(3) 0.5770(3) 0.5634(4) 0.0200(12) Uani 1 1 d . . . . .
H2B H 0.758010 0.588804 0.581710 0.024 Uiso 1 1 calc R U . . .
C3 C 0.8523(4) 0.6410(4) 0.5183(5) 0.0259(16) Uani 1 1 d . . . . .
H3 H 0.898448 0.652671 0.545513 0.031 Uiso 1 1 calc R U . . .
H3A H 0.844686 0.681486 0.529009 0.031 Uiso 1 1 calc R U . . .
C4 C 0.8547(4) 0.6303(4) 0.4183(5) 0.0261(16) Uani 1 1 d . . . . .
H4 H 0.817135 0.635349 0.387507 0.031 Uiso 1 1 calc R U . . .
H4A H 0.901104 0.666574 0.393600 0.031 Uiso 1 1 calc R U . . .
N3 N 0.8441(3) 0.5586(3) 0.4018(4) 0.0166(11) Uani 1 1 d . . . . .
H3B H 0.834982 0.549203 0.335442 0.020 Uiso 1 1 calc R U . . .
C5 C 0.9080(4) 0.5530(4) 0.4230(5) 0.0241(15) Uani 1 1 d . . . . .
H5 H 0.942296 0.595107 0.457990 0.029 Uiso 1 1 calc R U . . .
H5A H 0.931175 0.551519 0.366029 0.029 Uiso 1 1 calc R U . . .
C6 C 0.8866(4) 0.4861(4) 0.4780(5) 0.0251(15) Uani 1 1 d . . . . .
H6 H 0.866512 0.444527 0.437119 0.030 Uiso 1 1 calc R U . . .
H6A H 0.928883 0.489623 0.507942 0.030 Uiso 1 1 calc R U . . .
Mo2 Mo 0.71130(3) 0.47965(3) 0.15950(3) 0.01470(13) Uani 1 1 d . . . . .
O4 O 0.6614(3) 0.4081(2) 0.2373(3) 0.0191(10) Uani 1 1 d . . . . .
O5 O 0.7326(3) 0.4442(3) 0.0679(3) 0.0218(10) Uani 1 1 d . . . . .
O6 O 0.7896(3) 0.5357(3) 0.2136(3) 0.0211(10) Uani 1 1 d . . . . .
N4 N 0.6036(3) 0.4450(3) 0.0881(4) 0.0193(12) Uani 1 1 d . . . . .
H4B H 0.579807 0.392596 0.078821 0.023 Uiso 1 1 calc R U . . .
C7 C 0.6196(5) 0.4780(4) -0.0022(5) 0.0302(17) Uani 1 1 d . . . . .
H7 H 0.639505 0.455069 -0.040925 0.036 Uiso 1 1 calc R U . . .
H7A H 0.575428 0.470777 -0.030802 0.036 Uiso 1 1 calc R U . . .
C8 C 0.6706(4) 0.5541(4) 0.0045(5) 0.0311(18) Uani 1 1 d . . . . .
H8 H 0.644867 0.579241 0.020819 0.037 Uiso 1 1 calc R U . . .
H8A H 0.692669 0.571661 -0.055629 0.037 Uiso 1 1 calc R U . . .
N5 N 0.7271(3) 0.5713(3) 0.0722(4) 0.0214(12) Uani 1 1 d . . . . .
H5B H 0.772408 0.588236 0.038135 0.026 Uiso 1 1 calc R U . . .
C9 C 0.7372(4) 0.6298(4) 0.1346(6) 0.0316(18) Uani 1 1 d . . . . .
H9 H 0.740664 0.669889 0.098835 0.038 Uiso 1 1 calc R U . . .
H9A H 0.781814 0.647051 0.169020 0.038 Uiso 1 1 calc R U . . .
C10 C 0.6756(5) 0.6034(4) 0.1996(5) 0.0287(17) Uani 1 1 d . . . . .
H10 H 0.688261 0.636983 0.250831 0.034 Uiso 1 1 calc R U . . .
H10A H 0.634102 0.600578 0.168236 0.034 Uiso 1 1 calc R U . . .
N6 N 0.6577(3) 0.5335(3) 0.2339(4) 0.0195(12) Uani 1 1 d . . . . .
H6B H 0.673980 0.539991 0.298324 0.023 Uiso 1 1 calc R U . . .
C11 C 0.5793(4) 0.4816(5) 0.2346(5) 0.0297(17) Uani 1 1 d . . . . .
H11 H 0.569487 0.439748 0.271415 0.036 Uiso 1 1 calc R U . . .
H11A H 0.553927 0.504025 0.262175 0.036 Uiso 1 1 calc R U . . .
C12 C 0.5538(4) 0.4592(4) 0.1409(6) 0.0317(18) Uani 1 1 d . . . . .
H12 H 0.548626 0.496873 0.110417 0.038 Uiso 1 1 calc R U . . .
H12A H 0.506604 0.415866 0.142634 0.038 Uiso 1 1 calc R U . . .
Co1 Co 0.666667 0.333333 0.81293(12) 0.0276(4) Uani 1 3 d S T P . .
O7 O 0.6316(4) 0.3870(3) 0.7302(4) 0.0370(14) Uani 1 1 d D . . . .
H7W H 0.628(6) 0.424(4) 0.740(7) 0.055 Uiso 1 1 d D U . . .
H7WA H 0.642(3) 0.388(5) 0.6733(17) 0.055 Uiso 1 1 d D U . . .
O8 O 0.5803(4) 0.3133(4) 0.8912(4) 0.0411(15) Uani 1 1 d D . . . .
H8W H 0.546(3) 0.319(5) 0.870(5) 0.02(2) Uiso 1 1 d D . . . .
H8WA H 0.584(6) 0.321(6) 0.9483(19) 0.18(10) Uiso 1 1 d D . . . .
Cl1 Cl 0.40906(10) 0.30026(10) 0.92173(13) 0.0302(4) Uani 1 1 d D . . . .
O9 O 0.3895(4) 0.2299(3) 0.9417(5) 0.057(2) Uani 1 1 d D . . . .
O10 O 0.4617(4) 0.3296(4) 0.8520(5) 0.0536(19) Uani 1 1 d D . . . .
O11 O 0.3469(4) 0.3016(4) 0.8935(6) 0.057(2) Uani 1 1 d D . . . .
O12 O 0.4389(4) 0.3423(4) 1.0019(5) 0.062(2) Uani 1 1 d D . . . .
Cl2 Cl 0.64269(9) 0.55832(9) 0.72212(11) 0.0213(3) Uani 1 1 d D U . . .
O13 O 0.6107(12) 0.5970(11) 0.7595(14) 0.049(5) Uani 0.7 1 d D U P A .
O14 O 0.7039(9) 0.6115(10) 0.6750(14) 0.035(5) Uani 0.4 1 d D U P A 1
O15 O 0.5932(18) 0.5097(17) 0.658(2) 0.040(8) Uani 0.4 1 d D U P A 1
O16 O 0.6443(19) 0.5167(13) 0.7933(15) 0.040(7) Uani 0.4 1 d D U P A 1
O14B O 0.7129(16) 0.6032(17) 0.696(2) 0.017(6) Uiso 0.3 1 d . U P A 2
O15B O 0.601(2) 0.517(3) 0.641(3) 0.026(9) Uiso 0.3 1 d . U P A 2
O16B O 0.661(2) 0.512(2) 0.774(2) 0.055(11) Uiso 0.3 1 d . U P A 2
O13C O 0.616(2) 0.604(2) 0.741(3) 0.038(6) Uani 0.3 1 d D U P A 3
O14C O 0.7202(9) 0.5998(11) 0.736(2) 0.034(5) Uani 0.3 1 d D U P A 3
O15C O 0.6347(14) 0.5363(13) 0.6315(12) 0.038(5) Uani 0.3 1 d D U P A 3
O16C O 0.6169(12) 0.5018(14) 0.7830(19) 0.022(6) Uani 0.3 1 d D U P A 3


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr1 O1 2.066(5) . ?
Zr1 O1 2.066(5) 3_665 ?
Zr1 O1 2.066(5) 2_655 ?
Zr1 O4 2.078(5) 3_665 ?
Zr1 O4 2.078(5) 2_655 ?
Zr1 O4 2.078(5) . ?
Mo1 O3 1.706(5) . ?
Mo1 O2 1.724(5) . ?
Mo1 O1 1.819(5) . ?
Mo1 N2 2.249(6) . ?
Mo1 N3 2.303(6) . ?
Mo1 N1 2.315(5) . ?
N1 C6 1.474(9) . ?
N1 C1 1.486(9) . ?
N1 H1 1.0000 . ?
C1 C2 1.507(10) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 N2 1.501(9) . ?
C2 H2 0.9900 . ?
C2 H2A 0.9900 . ?
N2 C3 1.484(10) . ?
N2 H2B 1.0000 . ?
C3 C4 1.499(10) . ?
C3 H3 0.9900 . ?
C3 H3A 0.9900 . ?
C4 N3 1.481(9) . ?
C4 H4 0.9900 . ?
C4 H4A 0.9900 . ?
N3 C5 1.490(9) . ?
N3 H3B 1.0000 . ?
C5 C6 1.524(11) . ?
C5 H5 0.9900 . ?
C5 H5A 0.9900 . ?
C6 H6 0.9900 . ?
C6 H6A 0.9900 . ?
Mo2 O6 1.720(5) . ?
Mo2 O5 1.732(5) . ?
Mo2 O4 1.799(5) . ?
Mo2 N5 2.255(6) . ?
Mo2 N6 2.306(6) . ?
Mo2 N4 2.328(5) . ?
N4 C7 1.471(9) . ?
N4 C12 1.489(10) . ?
N4 H4B 1.0000 . ?
C7 C8 1.468(12) . ?
C7 H7 0.9900 . ?
C7 H7A 0.9900 . ?
C8 N5 1.481(10) . ?
C8 H8 0.9900 . ?
C8 H8A 0.9900 . ?
N5 C9 1.497(10) . ?
N5 H5B 1.0000 . ?
C9 C10 1.510(12) . ?
C9 H9 0.9900 . ?
C9 H9A 0.9900 . ?
C10 N6 1.462(10) . ?
C10 H10 0.9900 . ?
C10 H10A 0.9900 . ?
N6 C11 1.505(9) . ?
N6 H6B 1.0000 . ?
C11 C12 1.478(12) . ?
C11 H11 0.9900 . ?
C11 H11A 0.9900 . ?
C12 H12 0.9900 . ?
C12 H12A 0.9900 . ?
Co1 O8 2.060(6) 2_655 ?
Co1 O8 2.060(6) 3_665 ?
Co1 O8 2.060(6) . ?
Co1 O7 2.082(6) 2_655 ?
Co1 O7 2.082(6) 3_665 ?
Co1 O7 2.082(6) . ?
O7 H7W 0.86(3) . ?
O7 H7WA 0.86(3) . ?
O8 H8W 0.87(3) . ?
O8 H8WA 0.86(3) . ?
Cl1 O9 1.402(7) . ?
Cl1 O10 1.432(7) . ?
Cl1 O11 1.432(7) . ?
Cl1 O12 1.438(7) . ?
Cl2 O16C 1.40(2) . ?
Cl2 O14B 1.40(3) . ?
Cl2 O16 1.400(17) . ?
Cl2 O13C 1.40(3) . ?
Cl2 O15C 1.402(18) . ?
Cl2 O15 1.43(2) . ?
Cl2 O14 1.435(16) . ?
Cl2 O13 1.446(13) . ?
Cl2 O14C 1.477(18) . ?
Cl2 O16B 1.49(3) . ?
Cl2 O15B 1.51(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 90.12(19) . 3_665 ?
O1 Zr1 O1 90.13(19) . 2_655 ?
O1 Zr1 O1 90.12(19) 3_665 2_655 ?
O1 Zr1 O4 90.60(19) . 3_665 ?
O1 Zr1 O4 89.82(18) 3_665 3_665 ?
O1 Zr1 O4 179.3(2) 2_655 3_665 ?
O1 Zr1 O4 179.3(2) . 2_655 ?
O1 Zr1 O4 90.60(19) 3_665 2_655 ?
O1 Zr1 O4 89.82(18) 2_655 2_655 ?
O4 Zr1 O4 89.46(19) 3_665 2_655 ?
O1 Zr1 O4 89.82(18) . . ?
O1 Zr1 O4 179.3(2) 3_665 . ?
O1 Zr1 O4 90.60(19) 2_655 . ?
O4 Zr1 O4 89.46(19) 3_665 . ?
O4 Zr1 O4 89.46(19) 2_655 . ?
O3 Mo1 O2 106.5(2) . . ?
O3 Mo1 O1 106.2(2) . . ?
O2 Mo1 O1 107.2(2) . . ?
O3 Mo1 N2 89.9(2) . . ?
O2 Mo1 N2 88.1(2) . . ?
O1 Mo1 N2 153.0(2) . . ?
O3 Mo1 N3 88.0(2) . . ?
O2 Mo1 N3 156.7(2) . . ?
O1 Mo1 N3 85.3(2) . . ?
N2 Mo1 N3 73.5(2) . . ?
O3 Mo1 N1 156.9(2) . . ?
O2 Mo1 N1 88.9(2) . . ?
O1 Mo1 N1 84.8(2) . . ?
N2 Mo1 N1 73.2(2) . . ?
N3 Mo1 N1 72.39(19) . . ?
Mo1 O1 Zr1 135.7(3) . . ?
C6 N1 C1 112.2(6) . . ?
C6 N1 Mo1 108.2(4) . . ?
C1 N1 Mo1 114.5(4) . . ?
C6 N1 H1 107.2 . . ?
C1 N1 H1 107.2 . . ?
Mo1 N1 H1 107.2 . . ?
N1 C1 C2 110.7(6) . . ?
N1 C1 H1A 109.5 . . ?
C2 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 108.1 . . ?
N2 C2 C1 108.9(6) . . ?
N2 C2 H2 109.9 . . ?
C1 C2 H2 109.9 . . ?
N2 C2 H2A 109.9 . . ?
C1 C2 H2A 109.9 . . ?
H2 C2 H2A 108.3 . . ?
C3 N2 C2 112.4(6) . . ?
C3 N2 Mo1 115.0(4) . . ?
C2 N2 Mo1 108.8(4) . . ?
C3 N2 H2B 106.7 . . ?
C2 N2 H2B 106.7 . . ?
Mo1 N2 H2B 106.7 . . ?
N2 C3 C4 111.9(6) . . ?
N2 C3 H3 109.2 . . ?
C4 C3 H3 109.2 . . ?
N2 C3 H3A 109.2 . . ?
C4 C3 H3A 109.2 . . ?
H3 C3 H3A 107.9 . . ?
N3 C4 C3 109.0(6) . . ?
N3 C4 H4 109.9 . . ?
C3 C4 H4 109.9 . . ?
N3 C4 H4A 109.9 . . ?
C3 C4 H4A 109.9 . . ?
H4 C4 H4A 108.3 . . ?
C4 N3 C5 113.1(6) . . ?
C4 N3 Mo1 106.7(4) . . ?
C5 N3 Mo1 116.4(4) . . ?
C4 N3 H3B 106.7 . . ?
C5 N3 H3B 106.7 . . ?
Mo1 N3 H3B 106.7 . . ?
N3 C5 C6 109.8(6) . . ?
N3 C5 H5 109.7 . . ?
C6 C5 H5 109.7 . . ?
N3 C5 H5A 109.7 . . ?
C6 C5 H5A 109.7 . . ?
H5 C5 H5A 108.2 . . ?
N1 C6 C5 110.3(6) . . ?
N1 C6 H6 109.6 . . ?
C5 C6 H6 109.6 . . ?
N1 C6 H6A 109.6 . . ?
C5 C6 H6A 109.6 . . ?
H6 C6 H6A 108.1 . . ?
O6 Mo2 O5 106.7(2) . . ?
O6 Mo2 O4 105.9(2) . . ?
O5 Mo2 O4 106.9(2) . . ?
O6 Mo2 N5 88.7(2) . . ?
O5 Mo2 N5 89.6(2) . . ?
O4 Mo2 N5 153.1(2) . . ?
O6 Mo2 N6 89.6(2) . . ?
O5 Mo2 N6 156.3(2) . . ?
O4 Mo2 N6 84.1(2) . . ?
N5 Mo2 N6 73.3(2) . . ?
O6 Mo2 N4 157.2(2) . . ?
O5 Mo2 N4 87.4(2) . . ?
O4 Mo2 N4 86.2(2) . . ?
N5 Mo2 N4 73.2(2) . . ?
N6 Mo2 N4 72.2(2) . . ?
Mo2 O4 Zr1 143.7(3) . . ?
C7 N4 C12 113.1(6) . . ?
C7 N4 Mo2 107.2(4) . . ?
C12 N4 Mo2 114.7(4) . . ?
C7 N4 H4B 107.1 . . ?
C12 N4 H4B 107.1 . . ?
Mo2 N4 H4B 107.1 . . ?
C8 C7 N4 110.7(6) . . ?
C8 C7 H7 109.5 . . ?
N4 C7 H7 109.5 . . ?
C8 C7 H7A 109.5 . . ?
N4 C7 H7A 109.5 . . ?
H7 C7 H7A 108.1 . . ?
C7 C8 N5 113.3(6) . . ?
C7 C8 H8 108.9 . . ?
N5 C8 H8 108.9 . . ?
C7 C8 H8A 108.9 . . ?
N5 C8 H8A 108.9 . . ?
H8 C8 H8A 107.7 . . ?
C8 N5 C9 112.4(6) . . ?
C8 N5 Mo2 114.9(5) . . ?
C9 N5 Mo2 107.2(5) . . ?
C8 N5 H5B 107.3 . . ?
C9 N5 H5B 107.3 . . ?
Mo2 N5 H5B 107.3 . . ?
N5 C9 C10 110.0(6) . . ?
N5 C9 H9 109.7 . . ?
C10 C9 H9 109.7 . . ?
N5 C9 H9A 109.7 . . ?
C10 C9 H9A 109.7 . . ?
H9 C9 H9A 108.2 . . ?
N6 C10 C9 109.9(6) . . ?
N6 C10 H10 109.7 . . ?
C9 C10 H10 109.7 . . ?
N6 C10 H10A 109.7 . . ?
C9 C10 H10A 109.7 . . ?
H10 C10 H10A 108.2 . . ?
C10 N6 C11 113.4(6) . . ?
C10 N6 Mo2 115.3(5) . . ?
C11 N6 Mo2 107.2(4) . . ?
C10 N6 H6B 106.9 . . ?
C11 N6 H6B 106.9 . . ?
Mo2 N6 H6B 106.9 . . ?
C12 C11 N6 109.9(6) . . ?
C12 C11 H11 109.7 . . ?
N6 C11 H11 109.7 . . ?
C12 C11 H11A 109.7 . . ?
N6 C11 H11A 109.7 . . ?
H11 C11 H11A 108.2 . . ?
C11 C12 N4 111.4(6) . . ?
C11 C12 H12 109.3 . . ?
N4 C12 H12 109.3 . . ?
C11 C12 H12A 109.3 . . ?
N4 C12 H12A 109.3 . . ?
H12 C12 H12A 108.0 . . ?
O8 Co1 O8 91.6(3) 2_655 3_665 ?
O8 Co1 O8 91.6(3) 2_655 . ?
O8 Co1 O8 91.6(3) 3_665 . ?
O8 Co1 O7 83.9(3) 2_655 2_655 ?
O8 Co1 O7 171.4(3) 3_665 2_655 ?
O8 Co1 O7 95.9(3) . 2_655 ?
O8 Co1 O7 95.9(3) 2_655 3_665 ?
O8 Co1 O7 83.9(3) 3_665 3_665 ?
O8 Co1 O7 171.4(3) . 3_665 ?
O7 Co1 O7 89.1(3) 2_655 3_665 ?
O8 Co1 O7 171.4(3) 2_655 . ?
O8 Co1 O7 95.9(3) 3_665 . ?
O8 Co1 O7 83.9(3) . . ?
O7 Co1 O7 89.1(3) 2_655 . ?
O7 Co1 O7 89.1(3) 3_665 . ?
Co1 O7 H7W 131(7) . . ?
Co1 O7 H7WA 115(4) . . ?
H7W O7 H7WA 106(9) . . ?
Co1 O8 H8W 121(6) . . ?
Co1 O8 H8WA 122(8) . . ?
H8W O8 H8WA 110(7) . . ?
O9 Cl1 O10 112.2(5) . . ?
O9 Cl1 O11 108.1(4) . . ?
O10 Cl1 O11 109.6(4) . . ?
O9 Cl1 O12 108.5(5) . . ?
O10 Cl1 O12 107.5(5) . . ?
O11 Cl1 O12 110.9(5) . . ?
O16C Cl2 O13C 112(2) . . ?
O16C Cl2 O15C 112.7(16) . . ?
O13C Cl2 O15C 114(2) . . ?
O16 Cl2 O15 105.8(18) . . ?
O16 Cl2 O14 124.9(16) . . ?
O15 Cl2 O14 109.2(17) . . ?
O16C Cl2 O13 99.8(18) . . ?
O14B Cl2 O13 112.0(17) . . ?
O16 Cl2 O13 105.5(14) . . ?
O13C Cl2 O13 12(3) . . ?
O15C Cl2 O13 123.4(14) . . ?
O15 Cl2 O13 106.3(18) . . ?
O14 Cl2 O13 103.8(12) . . ?
O16C Cl2 O14C 106.6(14) . . ?
O13C Cl2 O14C 107(2) . . ?
O15C Cl2 O14C 104.3(15) . . ?
O13 Cl2 O14C 109.2(13) . . ?
O14B Cl2 O16B 92(2) . . ?
O13 Cl2 O16B 125.4(15) . . ?
O14B Cl2 O15B 109(2) . . ?
O13 Cl2 O15B 109(2) . . ?
O16B Cl2 O15B 107(2) . . ?

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 -46.7(4) . . . . ?
O2 Mo1 O1 Zr1 66.9(4) . . . . ?
N2 Mo1 O1 Zr1 -171.0(4) . . . . ?
N3 Mo1 O1 Zr1 -133.2(4) . . . . ?
N1 Mo1 O1 Zr1 154.1(4) . . . . ?
C6 N1 C1 C2 135.6(6) . . . . ?
Mo1 N1 C1 C2 11.8(7) . . . . ?
N1 C1 C2 N2 -42.9(8) . . . . ?
C1 C2 N2 C3 -73.8(7) . . . . ?
C1 C2 N2 Mo1 54.7(6) . . . . ?
C2 N2 C3 C4 134.0(6) . . . . ?
Mo1 N2 C3 C4 8.8(8) . . . . ?
N2 C3 C4 N3 -41.8(8) . . . . ?
C3 C4 N3 C5 -75.6(8) . . . . ?
C3 C4 N3 Mo1 53.6(6) . . . . ?
C4 N3 C5 C6 134.0(6) . . . . ?
Mo1 N3 C5 C6 10.0(7) . . . . ?
C1 N1 C6 C5 -73.7(7) . . . . ?
Mo1 N1 C6 C5 53.6(6) . . . . ?
N3 C5 C6 N1 -41.8(8) . . . . ?
O6 Mo2 O4 Zr1 -51.0(5) . . . . ?
O5 Mo2 O4 Zr1 62.5(5) . . . . ?
N5 Mo2 O4 Zr1 -171.8(4) . . . . ?
N6 Mo2 O4 Zr1 -138.9(5) . . . . ?
N4 Mo2 O4 Zr1 148.6(5) . . . . ?
C12 N4 C7 C8 77.2(8) . . . . ?
Mo2 N4 C7 C8 -50.2(7) . . . . ?
N4 C7 C8 N5 39.6(10) . . . . ?
C7 C8 N5 C9 -131.2(8) . . . . ?
C7 C8 N5 Mo2 -8.2(9) . . . . ?
C8 N5 C9 C10 72.1(8) . . . . ?
Mo2 N5 C9 C10 -55.0(7) . . . . ?
N5 C9 C10 N6 43.5(8) . . . . ?
C9 C10 N6 C11 -135.4(7) . . . . ?
C9 C10 N6 Mo2 -11.4(8) . . . . ?
C10 N6 C11 C12 72.9(8) . . . . ?
Mo2 N6 C11 C12 -55.4(7) . . . . ?
N6 C11 C12 N4 42.8(9) . . . . ?
C7 N4 C12 C11 -133.0(7) . . . . ?
Mo2 N4 C12 C11 -9.6(8) . . . . ?

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 3.111(7) 152.9 3_665 yes
N2 H2B O14^a 1.00 2.03 2.95(2) 152.8 . yes
N3 H3B O6 1.00 2.00 2.963(7) 160.5 . yes
N4 H4B O5 1.00 2.07 3.045(8) 165.5 2_655 yes
N5 H5B O9 1.00 1.93 2.903(10) 162.6 3_664 yes
N6 H6B O3 1.00 1.98 2.939(7) 158.7 . yes
O7 H7WA O2 0.86(3) 1.88(4) 2.679(8) 153(8) . yes
O7 H7W O16^a 0.86(3) 2.03(4) 2.86(3) 161(10) . yes
O7 H7W O16B^b 0.86(3) 1.75(6) 2.54(4) 153(11) . yes
O7 H7W O16C^c 0.86(3) 1.94(5) 2.79(3) 171(11) . yes
O8 H8W O10 0.87(3) 1.99(4) 2.841(10) 166(8) . yes
O8 H8WA O5 0.86(3) 1.89(5) 2.662(8) 150(11) 2_656 yes

_refine_diff_density_max         0.628
_refine_diff_density_min         -1.739
_refine_diff_density_rms         0.124



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

data_ZnTiMo6_3p22_104K_a
_database_code_depnum_ccdc_archive 'CCDC 2372557'
loop_
_audit_author_name
_audit_author_address
'Ryoji Mitsuhashi'
;Kanazawa University
Japan
;
_audit_update_record             
;
2024-07-22 deposited with the CCDC.	2024-09-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H90 Mo6 N18 O18 Ti, H12 Zn O6, 6(Cl O4)'
_chemical_formula_sum            'C36 H102 Cl6 Mo6 N18 O48 Ti Zn'
_chemical_formula_weight         2456.96

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'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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'

_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_H-M_alt        'R 3 :H'
_space_group_name_Hall           'R 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.
;

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'

_cell_length_a                   21.6448(3)
_cell_length_b                   21.6448(3)
_cell_length_c                   14.6822(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     5957.0(2)
_cell_formula_units_Z            3
_cell_measurement_temperature    104(2)
_cell_measurement_reflns_used    9535
_cell_measurement_theta_min      2.5560
_cell_measurement_theta_max      30.1060

_exptl_crystal_description       rhombohedral
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.055
_exptl_crystal_F_000             3702
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.217
_exptl_crystal_size_mid          0.162
_exptl_crystal_size_min          0.117
_exptl_absorpt_coefficient_mu    1.621
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.87943
_exptl_absorpt_correction_T_max  1.00000
_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_absorpt_special_details   ?
_diffrn_ambient_temperature      104(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10464
_diffrn_reflns_av_unetI/netI     0.0175
_diffrn_reflns_av_R_equivalents  0.0123
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.882
_diffrn_reflns_theta_max         27.476
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.784
_diffrn_reflns_point_group_measured_fraction_full 0.826
_reflns_number_total             4770
_reflns_number_gt                4721
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.575
_reflns_Friedel_fraction_max     0.572
_reflns_Friedel_fraction_full    0.652

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0526P)²+34.5070P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.39(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         4770
_refine_ls_number_parameters     399
_refine_ls_number_restraints     170
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0292
_refine_ls_wR_factor_ref         0.0826
_refine_ls_wR_factor_gt          0.0823
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_restrained_S_all      1.072
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.333333 0.666667 0.68185(13) 0.0109(3) Uani 1 3 d S T P . .
Mo1 Mo 0.40605(2) 0.59694(3) 0.83547(3) 0.01334(12) Uani 1 1 d . . . . .
O1 O 0.4037(2) 0.6607(2) 0.7571(3) 0.0163(8) Uani 1 1 d . . . . .
O2 O 0.3534(2) 0.5895(3) 0.9275(3) 0.0198(9) Uani 1 1 d . . . . .
O3 O 0.3636(2) 0.5166(2) 0.7815(3) 0.0207(9) Uani 1 1 d . . . . .
N1 N 0.5004(3) 0.6937(3) 0.9071(4) 0.0202(11) Uani 1 1 d . . . . .
H1 H 0.481743 0.724107 0.932174 0.024 Uiso 1 1 calc R U . . .
C1 C 0.5324(4) 0.6749(4) 0.9839(5) 0.0263(14) Uani 1 1 d . . . . .
H1A H 0.538413 0.705609 1.037006 0.032 Uiso 1 1 calc R U . . .
H1B H 0.579985 0.682982 0.966149 0.032 Uiso 1 1 calc R U . . .
C2 C 0.4847(4) 0.5978(4) 1.0093(5) 0.0245(14) Uani 1 1 d . . . . .
H2 H 0.511321 0.581563 1.048080 0.029 Uiso 1 1 calc R U . . .
H2A H 0.443271 0.592387 1.044440 0.029 Uiso 1 1 calc R U . . .
N2 N 0.4596(3) 0.5534(3) 0.9256(4) 0.0203(11) Uani 1 1 d . . . . .
H2B H 0.421689 0.504747 0.945077 0.024 Uiso 1 1 calc R U . . .
C3 C 0.5164(4) 0.5447(4) 0.8808(5) 0.0289(16) Uani 1 1 d . . . . .
H3 H 0.507893 0.495991 0.892714 0.035 Uiso 1 1 calc R U . . .
H3A H 0.563288 0.579164 0.907227 0.035 Uiso 1 1 calc R U . . .
C4 C 0.5180(4) 0.5564(4) 0.7802(5) 0.0261(15) Uani 1 1 d . . . . .
H4 H 0.479083 0.513470 0.750418 0.031 Uiso 1 1 calc R U . . .
H4A H 0.563980 0.565018 0.754713 0.031 Uiso 1 1 calc R U . . .
N3 N 0.5089(3) 0.6192(3) 0.7622(4) 0.0197(11) Uani 1 1 d . . . . .
H3B H 0.499769 0.619108 0.695457 0.024 Uiso 1 1 calc R U . . .
C5 C 0.5740(3) 0.6884(4) 0.7829(5) 0.0240(14) Uani 1 1 d . . . . .
H5 H 0.597946 0.712282 0.725425 0.029 Uiso 1 1 calc R U . . .
H5A H 0.607623 0.680009 0.819148 0.029 Uiso 1 1 calc R U . . .
C6 C 0.5539(4) 0.7361(3) 0.8359(5) 0.0264(15) Uani 1 1 d . . . . .
H6 H 0.596928 0.775376 0.864830 0.032 Uiso 1 1 calc R U . . .
H6A H 0.533738 0.757249 0.793920 0.032 Uiso 1 1 calc R U . . .
Mo2 Mo 0.37490(2) 0.56674(2) 0.52488(3) 0.01229(12) Uani 1 1 d . . . . .
O4 O 0.3274(2) 0.5911(2) 0.6050(3) 0.0162(8) Uani 1 1 d . . . . .
O5 O 0.3953(2) 0.6223(2) 0.4319(3) 0.0198(9) Uani 1 1 d D . . . .
O6 O 0.4547(2) 0.5894(2) 0.5760(3) 0.0190(9) Uani 1 1 d . . . . .
N4 N 0.2671(3) 0.4920(3) 0.4539(4) 0.0166(10) Uani 1 1 d . . . . .
H4B H 0.243072 0.520804 0.444511 0.020 Uiso 1 1 calc R U . . .
C7 C 0.2824(4) 0.4750(5) 0.3623(5) 0.0311(16) Uani 1 1 d . . . . .
H7 H 0.301903 0.517972 0.323241 0.037 Uiso 1 1 calc R U . . .
H7A H 0.237781 0.437440 0.334167 0.037 Uiso 1 1 calc R U . . .
C8 C 0.3354(4) 0.4496(4) 0.3688(5) 0.0306(16) Uani 1 1 d . . . . .
H8 H 0.310082 0.398340 0.385130 0.037 Uiso 1 1 calc R U . . .
H8A H 0.358019 0.454627 0.308521 0.037 Uiso 1 1 calc R U . . .
N5 N 0.3916(3) 0.4900(3) 0.4374(4) 0.0198(11) Uani 1 1 d . . . . .
H5B H 0.437375 0.518826 0.403500 0.024 Uiso 1 1 calc R U . . .
C9 C 0.4019(4) 0.4422(4) 0.4997(6) 0.0319(17) Uani 1 1 d . . . . .
H9 H 0.447249 0.470093 0.533457 0.038 Uiso 1 1 calc R U . . .
H9A H 0.405111 0.405152 0.463903 0.038 Uiso 1 1 calc R U . . .
C10 C 0.3400(4) 0.4066(4) 0.5672(6) 0.0301(16) Uani 1 1 d . . . . .
H10 H 0.298048 0.366846 0.537054 0.036 Uiso 1 1 calc R U . . .
H10A H 0.353797 0.386898 0.619191 0.036 Uiso 1 1 calc R U . . .
N6 N 0.3221(3) 0.4593(3) 0.5999(4) 0.0188(11) Uani 1 1 d . . . . .
H6B H 0.338593 0.469783 0.664529 0.023 Uiso 1 1 calc R U . . .
C11 C 0.2427(4) 0.4322(4) 0.6011(5) 0.0298(16) Uani 1 1 d . . . . .
H11 H 0.217420 0.384278 0.629292 0.036 Uiso 1 1 calc R U . . .
H11A H 0.232895 0.464654 0.637945 0.036 Uiso 1 1 calc R U . . .
C12 C 0.2170(4) 0.4286(4) 0.5082(6) 0.0301(16) Uani 1 1 d . . . . .
H12 H 0.169727 0.425346 0.510045 0.036 Uiso 1 1 calc R U . . .
H12A H 0.211018 0.384922 0.478229 0.036 Uiso 1 1 calc R U . . .
Zn1 Zn 0.333333 0.666667 0.17613(11) 0.0312(3) Uani 1 3 d S T P . .
O7 O 0.2965(3) 0.5773(3) 0.0927(4) 0.0387(14) Uani 1 1 d D . . . .
H7W H 0.300(5) 0.542(3) 0.110(6) 0.058 Uiso 1 1 d D U . . .
H7WA H 0.3093(16) 0.584(3) 0.0379(10) 0.058 Uiso 1 1 d D U . . .
O8 O 0.3987(4) 0.6447(4) 0.2530(4) 0.0488(17) Uani 1 1 d D . . . .
H8W H 0.439(3) 0.650(7) 0.236(6) 0.073 Uiso 1 1 d D U . . .
H8WA H 0.397(6) 0.645(5) 0.3109(10) 0.073 Uiso 1 1 d D U . . .
Cl1 Cl 0.55780(10) 0.63410(9) 0.28449(13) 0.0309(4) Uani 1 1 d D . . . .
O9 O 0.5059(4) 0.5640(3) 0.3048(6) 0.063(2) Uani 1 1 d D . . . .
O10 O 0.5359(4) 0.6656(4) 0.2149(5) 0.0543(18) Uani 1 1 d D . . . .
O11 O 0.6206(4) 0.6346(4) 0.2536(6) 0.062(2) Uani 1 1 d D . . . .
O12 O 0.5726(5) 0.6763(5) 0.3646(5) 0.068(2) Uani 1 1 d D . . . .
Cl2 Cl 0.31096(9) 0.41860(8) 0.08607(11) 0.0217(3) Uani 1 1 d D U . . .
O13 O 0.2829(12) 0.3449(7) 0.1042(12) 0.024(3) Uani 0.57(4) 1 d D U P A 1
O14 O 0.3870(6) 0.4539(9) 0.097(2) 0.061(6) Uani 0.57(4) 1 d D U P A 1
O15 O 0.2972(17) 0.4312(10) -0.0044(9) 0.055(5) Uani 0.57(4) 1 d D U P A 1
O16 O 0.2847(11) 0.4490(8) 0.1504(9) 0.035(4) Uani 0.57(4) 1 d D U P A 1
O13B O 0.2800(16) 0.3519(13) 0.132(2) 0.038(7) Uani 0.43(4) 1 d D U P A 2
O14B O 0.3762(12) 0.4342(14) 0.0469(19) 0.041(6) Uani 0.43(4) 1 d D U P A 2
O15B O 0.2642(11) 0.4156(10) 0.0151(16) 0.033(5) Uani 0.43(4) 1 d D U P A 2
O16B O 0.324(2) 0.4747(15) 0.1493(15) 0.060(7) Uani 0.43(4) 1 d D U P A 2


_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
Ti1 O4 1.937(4) 3_565 ?
Ti1 O4 1.937(4) 2_665 ?
Ti1 O4 1.937(4) . ?
Ti1 O1 1.937(4) . ?
Ti1 O1 1.937(4) 2_665 ?
Ti1 O1 1.937(4) 3_565 ?
Mo1 O3 1.702(5) . ?
Mo1 O2 1.723(4) . ?
Mo1 O1 1.817(4) . ?
Mo1 N2 2.252(5) . ?
Mo1 N3 2.296(5) . ?
Mo1 N1 2.320(6) . ?
N1 C1 1.483(9) . ?
N1 C6 1.487(9) . ?
C1 C2 1.506(10) . ?
C2 N2 1.485(9) . ?
N2 C3 1.489(9) . ?
C3 C4 1.497(11) . ?
C4 N3 1.490(8) . ?
N3 C5 1.487(9) . ?
C5 C6 1.518(10) . ?
Mo2 O6 1.714(4) . ?
Mo2 O5 1.725(4) . ?
Mo2 O4 1.806(4) . ?
Mo2 N5 2.268(5) . ?
Mo2 N6 2.296(5) . ?
Mo2 N4 2.318(5) . ?
N4 C7 1.475(9) . ?
N4 C12 1.487(9) . ?
C7 C8 1.503(10) . ?
C8 N5 1.481(9) . ?
N5 C9 1.479(9) . ?
C9 C10 1.530(11) . ?
C10 N6 1.457(9) . ?
N6 C11 1.512(9) . ?
C11 C12 1.461(11) . ?
Zn1 O8 2.044(6) . ?
Zn1 O8 2.044(6) 2_665 ?
Zn1 O8 2.044(6) 3_565 ?
Zn1 O7 2.082(6) 3_565 ?
Zn1 O7 2.082(6) 2_665 ?
Zn1 O7 2.082(6) . ?
Cl1 O9 1.396(6) . ?
Cl1 O12 1.424(7) . ?
Cl1 O11 1.428(7) . ?
Cl1 O10 1.434(7) . ?
Cl2 O14B 1.401(13) . ?
Cl2 O15 1.417(12) . ?
Cl2 O13 1.420(12) . ?
Cl2 O16 1.422(9) . ?
Cl2 O16B 1.441(16) . ?
Cl2 O13B 1.423(18) . ?
Cl2 O15B 1.431(14) . ?
Cl2 O14 1.437(12) . ?

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 Ti1 O4 89.5(2) 3_565 2_665 ?
O4 Ti1 O4 89.5(2) 3_565 . ?
O4 Ti1 O4 89.50(19) 2_665 . ?
O4 Ti1 O1 179.2(2) 3_565 . ?
O4 Ti1 O1 89.90(17) 2_665 . ?
O4 Ti1 O1 89.92(18) . . ?
O4 Ti1 O1 89.89(17) 3_565 2_665 ?
O4 Ti1 O1 89.92(18) 2_665 2_665 ?
O4 Ti1 O1 179.2(2) . 2_665 ?
O1 Ti1 O1 90.68(19) . 2_665 ?
O4 Ti1 O1 89.92(18) 3_565 3_565 ?
O4 Ti1 O1 179.2(2) 2_665 3_565 ?
O4 Ti1 O1 89.89(17) . 3_565 ?
O1 Ti1 O1 90.68(19) . 3_565 ?
O1 Ti1 O1 90.68(19) 2_665 3_565 ?
O3 Mo1 O2 106.0(2) . . ?
O3 Mo1 O1 106.0(2) . . ?
O2 Mo1 O1 107.4(2) . . ?
O3 Mo1 N2 88.6(2) . . ?
O2 Mo1 N2 87.4(2) . . ?
O1 Mo1 N2 154.9(2) . . ?
O3 Mo1 N3 88.2(2) . . ?
O2 Mo1 N3 156.1(2) . . ?
O1 Mo1 N3 86.39(19) . . ?
N2 Mo1 N3 73.5(2) . . ?
O3 Mo1 N1 156.2(2) . . ?
O2 Mo1 N1 88.4(2) . . ?
O1 Mo1 N1 87.0(2) . . ?
N2 Mo1 N1 72.92(19) . . ?
N3 Mo1 N1 72.5(2) . . ?
Mo1 O1 Ti1 137.2(2) . . ?
C1 N1 C6 112.2(5) . . ?
C1 N1 Mo1 114.7(4) . . ?
C6 N1 Mo1 107.5(4) . . ?
N1 C1 C2 109.7(6) . . ?
N2 C2 C1 109.8(6) . . ?
C2 N2 C3 112.9(5) . . ?
C2 N2 Mo1 108.4(4) . . ?
C3 N2 Mo1 115.1(4) . . ?
N2 C3 C4 111.4(5) . . ?
C3 C4 N3 109.1(5) . . ?
C5 N3 C4 113.2(5) . . ?
C5 N3 Mo1 116.5(4) . . ?
C4 N3 Mo1 106.4(4) . . ?
N3 C5 C6 109.9(5) . . ?
N1 C6 C5 109.9(5) . . ?
O6 Mo2 O5 106.1(2) . . ?
O6 Mo2 O4 105.7(2) . . ?
O5 Mo2 O4 107.2(2) . . ?
O6 Mo2 N5 87.2(2) . . ?
O5 Mo2 N5 89.1(2) . . ?
O4 Mo2 N5 154.9(2) . . ?
O6 Mo2 N6 90.0(2) . . ?
O5 Mo2 N6 155.6(2) . . ?
O4 Mo2 N6 85.2(2) . . ?
N5 Mo2 N6 73.2(2) . . ?
O6 Mo2 N4 156.3(2) . . ?
O5 Mo2 N4 87.0(2) . . ?
O4 Mo2 N4 88.59(19) . . ?
N5 Mo2 N4 73.01(18) . . ?
N6 Mo2 N4 72.01(19) . . ?
Mo2 O4 Ti1 145.0(3) . . ?
C7 N4 C12 114.1(6) . . ?
C7 N4 Mo2 108.1(4) . . ?
C12 N4 Mo2 114.7(4) . . ?
N4 C7 C8 110.0(6) . . ?
N5 C8 C7 112.2(6) . . ?
C9 N5 C8 112.0(6) . . ?
C9 N5 Mo2 107.2(4) . . ?
C8 N5 Mo2 115.7(4) . . ?
N5 C9 C10 110.7(6) . . ?
N6 C10 C9 109.1(6) . . ?
C10 N6 C11 113.3(5) . . ?
C10 N6 Mo2 116.3(4) . . ?
C11 N6 Mo2 107.0(4) . . ?
C12 C11 N6 109.8(6) . . ?
C11 C12 N4 111.6(6) . . ?
O8 Zn1 O8 92.5(3) . 2_665 ?
O8 Zn1 O8 92.5(3) . 3_565 ?
O8 Zn1 O8 92.5(3) 2_665 3_565 ?
O8 Zn1 O7 171.2(3) . 3_565 ?
O8 Zn1 O7 83.6(3) 2_665 3_565 ?
O8 Zn1 O7 95.6(3) 3_565 3_565 ?
O8 Zn1 O7 83.6(3) . 2_665 ?
O8 Zn1 O7 95.6(3) 2_665 2_665 ?
O8 Zn1 O7 171.2(3) 3_565 2_665 ?
O7 Zn1 O7 88.9(2) 3_565 2_665 ?
O8 Zn1 O7 95.6(3) . . ?
O8 Zn1 O7 171.2(3) 2_665 . ?
O8 Zn1 O7 83.6(3) 3_565 . ?
O7 Zn1 O7 88.9(2) 3_565 . ?
O7 Zn1 O7 88.9(2) 2_665 . ?
O9 Cl1 O12 108.7(5) . . ?
O9 Cl1 O11 108.8(4) . . ?
O12 Cl1 O11 110.5(6) . . ?
O9 Cl1 O10 113.0(5) . . ?
O12 Cl1 O10 107.8(5) . . ?
O11 Cl1 O10 108.1(4) . . ?
O15 Cl2 O13 112.2(9) . . ?
O15 Cl2 O16 111.3(9) . . ?
O13 Cl2 O16 110.5(8) . . ?
O14B Cl2 O16B 108.4(13) . . ?
O14B Cl2 O13B 110.2(13) . . ?
O16B Cl2 O13B 110.1(13) . . ?
O14B Cl2 O15B 108.5(10) . . ?
O16B Cl2 O15B 109.8(11) . . ?
O13B Cl2 O15B 109.7(13) . . ?
O15 Cl2 O14 107.6(10) . . ?
O13 Cl2 O14 108.0(11) . . ?
O16 Cl2 O14 107.0(10) . . ?

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 2.11 3.024(7) 151.1 2_665 yes
N2 H2B O14^a 1.00 2.44 3.18(3) 130.0 1_556 yes
N3 H3B O6 1.00 1.95 2.917(7) 161.2 . yes
N4 H4B O5 1.00 2.02 2.986(7) 161.5 3_565 yes
N5 H5B O9 1.00 1.95 2.917(9) 161.8 . yes
N6 H6B O3 1.00 1.93 2.889(7) 159.9 . yes
O7 H7W O16^a 0.851(13) 1.95(2) 2.792(12) 168(9) . yes
O7 H7W O16B^b 0.851(13) 1.86(3) 2.70(2) 170(9) . yes
O7 H7WA O2 0.841(12) 1.85(2) 2.673(7) 164(7) 1_554 yes
O8 H8W O10 0.846(12) 1.987(18) 2.826(9) 171(9) . yes
O8 H8WA O5 0.852(13) 1.84(2) 2.666(8) 164(8) . yes

_refine_diff_density_max         0.826
_refine_diff_density_min         -2.077
_refine_diff_density_rms         0.115



