# Supplementary Information (SI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2025

####################################################################### 
# 
# 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_exp_377
_database_code_depnum_ccdc_archive 'CCDC 2383525'
loop_
_audit_author_name
_audit_author_address
'Mattia Lopresti'
;University of Eastern Piedmont
Italy
;
_audit_update_record             
;
2024-09-12 deposited with the CCDC.	2025-05-29 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_exp_377             
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.900 Why?
RESPONSE: The crystal was low diffracting and solved from a twin cluster
;
_vrf_PLAT411_exp_377             
;
PROBLEM: Short Inter H...H Contact  H00V     ..H00V     .       1.85 Ang.
RESPONSE: The crystal was low diffracting and solved from a twin cluster
;
_vrf_PLAT911_exp_377             
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        359 Report
RESPONSE: The crystal was low diffracting and solved from a twin cluster
;
_vrf_PLAT213_exp_377             
;
PROBLEM: Atom C00R            has ADP max/min Ratio .....        3.3 prolat
RESPONSE: The central ring of the bipiridine can rotate along the N007-C008 axis, therefore all carbons belonging to that ring has large ADP
;
_vrf_PLAT220_exp_377             
;
PROBLEM: NonSolvent   Resd 1  C   Ueq(max)/Ueq(min) Range        3.2 Ratio
RESPONSE: The central ring of the bipiridine can rotate along the N007-C008 axis, therefore all carbons belonging to that ring has large ADP
;
_vrf_PLAT241_exp_377             
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of       C00M Check
RESPONSE: The central ring of the bipiridine can rotate along the N007-C008 axis, therefore all carbons belonging to that ring has large ADP
;
_vrf_PLAT241_exp_377_2           
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of       C00P Check
RESPONSE: The central ring of the bipiridine can rotate along the N007-C008 axis, therefore all carbons belonging to that ring has large ADP
;
_vrf_PLAT241_exp_377_3           
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of       C00R Check
RESPONSE: The central ring of the bipiridine can rotate along the N007-C008 axis, therefore all carbons belonging to that ring has large ADP
;
_vrf_PLAT241_exp_377_4           
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of       C00S Check
RESPONSE: The central ring of the bipiridine can rotate along the N007-C008 axis, therefore all carbons belonging to that ring has large ADP
;
_vrf_PLAT242_exp_377             
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of       N007 Check
RESPONSE: The central ring of the bipiridine can rotate along the N007-C008 axis, therefore all carbons belonging to that ring has large ADP
;
_vrf_PLAT242_exp_377_2           
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of       C008 Check
RESPONSE: The central ring of the bipiridine can rotate along the N007-C008 axis, therefore all carbons belonging to that ring has large ADP
;
_vrf_PLAT242_exp_377_3           
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of       C00A Check
RESPONSE: The central ring of the bipiridine can rotate along the N007-C008 axis, therefore all carbons belonging to that ring has large ADP
;
_vrf_PLAT242_exp_377_4           
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of       C00B Check
RESPONSE: The central ring of the bipiridine can rotate along the N007-C008 axis, therefore all carbons belonging to that ring has large ADP
;
_vrf_PLAT910_exp_377             
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).          5 Note
RESPONSE: The crystal was low diffracting and solved from a twin cluster
;
# Added during the CSD deposition process: Thursday 12 September 2024 10:17 AM
# end Validation Reply Form

_audit_creation_date             2024-09-12
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        '4-Phenylpyridine vanadyl-bis(acetylacetonate)'
_chemical_name_common            '4-Phenylpyridine vanadyl-bis(acetylacetonate)'
_chemical_formula_moiety         'C21 H23 N O5 V'
_chemical_formula_sum            'C21 H23 N O5 V'
_chemical_compound_source        Synthesis
_chemical_formula_weight         420.34
_exptl_crystal_recrystallization_method Evaporation
_chemical_melting_point          ?
_exptl_crystal_description       Twins
_exptl_crystal_colour            Red
_diffrn_ambient_temperature      293(2)
_diffrn_ambient_pressure         101.325
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'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'
_chemical_absolute_configuration ?
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   24.2547(15)
_cell_length_b                   8.0765(5)
_cell_length_c                   21.6591(12)
_cell_angle_alpha                90
_cell_angle_beta                 108.968(7)
_cell_angle_gamma                90
_cell_volume                     4012.5(4)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    2921
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.7580
_cell_measurement_theta_min      3.0410
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.526
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91930
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.050
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_Laue_measured_fraction_full 0.900
_diffrn_reflns_Laue_measured_fraction_max 0.890
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            6979
_diffrn_reflns_point_group_measured_fraction_full 0.900
_diffrn_reflns_point_group_measured_fraction_max 0.890
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.332
_diffrn_reflns_theta_min         2.952
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.6225
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.900
_diffrn_measured_fraction_theta_max 0.890
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -37.00  11.00   1.00    5.00    --   19.06 112.00 168.00   48
  2  ω     38.00 105.00   1.00    5.00    --   19.06 179.00 150.00   67
  3  ω    -52.00  61.00   1.00    5.00    --   19.06 -37.00 120.00  113
  4  ω    -60.00   1.00   1.00    5.00    --   19.06  15.00-165.00   61
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0019794000
_diffrn_orient_matrix_UB_12      0.0458397000
_diffrn_orient_matrix_UB_13      0.0285716000
_diffrn_orient_matrix_UB_21      -0.0057212000
_diffrn_orient_matrix_UB_22      -0.0730183000
_diffrn_orient_matrix_UB_23      0.0150881000
_diffrn_orient_matrix_UB_31      0.0303223000
_diffrn_orient_matrix_UB_32      -0.0167453000
_diffrn_orient_matrix_UB_33      0.0124557000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2527
_reflns_number_total             3273
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.054
_refine_diff_density_min         -0.800
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         3273
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0901
_refine_ls_R_factor_gt           0.0708
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0832P)²+16.2737P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1720
_refine_ls_wR_factor_ref         0.1873
_refine_special_details          Twin
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C00D(H00D), C00E(H00E), C00G(H00G), C00H(H00H), C00I(H00I), C00J(H00J),
 C00K(H00K), C00M(H00M), C00P(H00R), C00R(H00V), C00S(H00W)
2.b Idealised Me refined as rotating group:
 C00L(H00A,H00B,H00C), C00N(H00F,H00L,H00N), C00O(H00O,H00P,H00Q), C00Q(H00S,
 H00T,H00U)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
V01 V 0.61099(3) 0.56237(11) 0.41390(4) 0.0463(3) Uani 1 1 d . . . . .
O002 O 0.60313(13) 0.4308(4) 0.33375(14) 0.0450(8) Uani 1 1 d . . . . .
O003 O 0.58281(15) 0.3371(4) 0.44586(16) 0.0530(9) Uani 1 1 d . . . . .
O004 O 0.69082(14) 0.4810(5) 0.45611(16) 0.0574(9) Uani 1 1 d . . . . .
O005 O 0.61163(14) 0.6466(5) 0.49987(15) 0.0591(10) Uani 1 1 d . . . . .
O006 O 0.62475(15) 0.7311(4) 0.38274(18) 0.0597(9) Uani 1 1 d . . . . .
N007 N 0.51874(16) 0.6128(5) 0.38171(17) 0.0419(9) Uani 1 1 d . . . . .
C008 C 0.40224(18) 0.7194(6) 0.3424(2) 0.0406(10) Uani 1 1 d . . . . .
C009 C 0.34293(19) 0.7861(6) 0.3237(2) 0.0426(11) Uani 1 1 d . . . . .
C00A C 0.58722(19) 0.2846(6) 0.3165(2) 0.0484(12) Uani 1 1 d . . . . .
C00B C 0.5687(2) 0.2024(7) 0.4160(3) 0.0579(14) Uani 1 1 d . . . . .
C00C C 0.6550(2) 0.6817(6) 0.5478(2) 0.0554(13) Uani 1 1 d . . . . .
C00D C 0.3180(2) 0.8633(7) 0.2635(3) 0.0575(13) Uani 1 1 d . . . . .
H00D H 0.338185 0.866199 0.233616 0.069 Uiso 1 1 calc R U . . .
C00E C 0.3106(2) 0.7811(7) 0.3660(3) 0.0579(13) Uani 1 1 d . . . . .
H00E H 0.325887 0.729096 0.406263 0.069 Uiso 1 1 calc R U . . .
C00F C 0.7263(2) 0.5314(6) 0.5103(3) 0.0550(13) Uani 1 1 d . . . . .
C00G C 0.2334(2) 0.9309(7) 0.2906(3) 0.0673(16) Uani 1 1 d . . . . .
H00G H 0.196975 0.981269 0.279943 0.081 Uiso 1 1 calc R U . . .
C00H C 0.7114(3) 0.6306(7) 0.5545(3) 0.0648(15) Uani 1 1 d . . . . .
H00H H 0.741187 0.665638 0.591400 0.078 Uiso 1 1 calc R U . . .
C00I C 0.5706(2) 0.1726(7) 0.3536(3) 0.0655(15) Uani 1 1 d . . . . .
H00I H 0.559673 0.067968 0.335880 0.079 Uiso 1 1 calc R U . . .
C00J C 0.2563(2) 0.8524(8) 0.3489(3) 0.0686(16) Uani 1 1 d . . . . .
H00J H 0.234940 0.846819 0.377604 0.082 Uiso 1 1 calc R U . . .
C00K C 0.2637(2) 0.9355(7) 0.2480(3) 0.0664(15) Uani 1 1 d . . . . .
H00K H 0.247791 0.987848 0.207850 0.080 Uiso 1 1 calc R U . . .
C00L C 0.6432(3) 0.7679(8) 0.6031(3) 0.0755(17) Uani 1 1 d . . . . .
H00A H 0.632581 0.880816 0.591248 0.113 Uiso 1 1 calc R U . . .
H00B H 0.677537 0.765071 0.640917 0.113 Uiso 1 1 calc R U . . .
H00C H 0.611803 0.713147 0.612764 0.113 Uiso 1 1 calc R U . . .
C00M C 0.4298(2) 0.6547(9) 0.4012(3) 0.078(2) Uani 1 1 d . . . . .
H00M H 0.409547 0.643512 0.430747 0.094 Uiso 1 1 calc R U . . .
C00N C 0.7878(2) 0.4702(8) 0.5278(3) 0.0754(18) Uani 1 1 d . . . . .
H00F H 0.788601 0.352692 0.534739 0.113 Uiso 1 1 calc R U . . .
H00L H 0.811435 0.523991 0.567006 0.113 Uiso 1 1 calc R U . . .
H00N H 0.802797 0.494678 0.492900 0.113 Uiso 1 1 calc R U . . .
C00O C 0.5868(3) 0.2387(9) 0.2491(3) 0.085(2) Uani 1 1 d . . . . .
H00O H 0.566955 0.323001 0.218790 0.128 Uiso 1 1 calc R U . . .
H00P H 0.567025 0.134900 0.236675 0.128 Uiso 1 1 calc R U . . .
H00Q H 0.626177 0.228855 0.248876 0.128 Uiso 1 1 calc R U . . .
C00P C 0.4869(2) 0.6040(9) 0.4195(3) 0.081(2) Uani 1 1 d . . . . .
H00R H 0.503617 0.561033 0.461215 0.097 Uiso 1 1 calc R U . . .
C00Q C 0.5478(4) 0.0691(9) 0.4514(4) 0.105(3) Uani 1 1 d . . . . .
H00S H 0.562678 0.089319 0.497509 0.158 Uiso 1 1 calc R U . . .
H00T H 0.561299 -0.036597 0.441943 0.158 Uiso 1 1 calc R U . . .
H00U H 0.505929 0.069412 0.437207 0.158 Uiso 1 1 calc R U . . .
C00R C 0.4919(3) 0.6709(14) 0.3247(3) 0.127(4) Uani 1 1 d . . . . .
H00V H 0.512520 0.676469 0.295269 0.153 Uiso 1 1 calc R U . . .
C00S C 0.4360(3) 0.7247(14) 0.3038(3) 0.130(4) Uani 1 1 d . . . . .
H00W H 0.420473 0.766500 0.261722 0.156 Uiso 1 1 calc R U . . .


_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
V01 O002 1.991(3) . ?
V01 O003 2.136(4) . ?
V01 O004 1.966(3) . ?
V01 O005 1.978(3) . ?
V01 O006 1.604(3) . ?
V01 N007 2.155(4) . ?
O002 C00A 1.261(6) . ?
O003 C00B 1.255(6) . ?
O004 C00F 1.276(6) . ?
O005 C00C 1.248(6) . ?
N007 C00P 1.297(6) . ?
N007 C00R 1.283(7) . ?
C008 C009 1.464(6) . ?
C008 C00M 1.336(7) . ?
C008 C00S 1.348(7) . ?
C009 C00D 1.394(7) . ?
C009 C00E 1.385(6) . ?
C00A C00I 1.355(8) . ?
C00A C00O 1.502(7) . ?
C00B C00I 1.390(8) . ?
C00B C00Q 1.502(8) . ?
C00C C00H 1.389(8) . ?
C00C C00L 1.491(7) . ?
C00D H00D 0.9300 . ?
C00D C00K 1.378(7) . ?
C00E H00E 0.9300 . ?
C00E C00J 1.374(7) . ?
C00F C00H 1.385(8) . ?
C00F C00N 1.498(7) . ?
C00G H00G 0.9300 . ?
C00G C00J 1.361(8) . ?
C00G C00K 1.356(8) . ?
C00H H00H 0.9300 . ?
C00I H00I 0.9300 . ?
C00J H00J 0.9300 . ?
C00K H00K 0.9300 . ?
C00L H00A 0.9600 . ?
C00L H00B 0.9600 . ?
C00L H00C 0.9600 . ?
C00M H00M 0.9300 . ?
C00M C00P 1.373(7) . ?
C00N H00F 0.9600 . ?
C00N H00L 0.9600 . ?
C00N H00N 0.9600 . ?
C00O H00O 0.9600 . ?
C00O H00P 0.9600 . ?
C00O H00Q 0.9600 . ?
C00P H00R 0.9300 . ?
C00Q H00S 0.9600 . ?
C00Q H00T 0.9600 . ?
C00Q H00U 0.9600 . ?
C00R H00V 0.9300 . ?
C00R C00S 1.354(8) . ?
C00S H00W 0.9300 . ?

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
O002 V01 O003 82.99(13) . . ?
O002 V01 N007 91.36(13) . . ?
O003 V01 N007 81.83(14) . . ?
O004 V01 O002 91.59(14) . . ?
O004 V01 O003 86.28(15) . . ?
O004 V01 O005 88.39(14) . . ?
O004 V01 N007 167.31(15) . . ?
O005 V01 O002 166.83(15) . . ?
O005 V01 O003 83.86(15) . . ?
O005 V01 N007 85.94(13) . . ?
O006 V01 O002 93.49(16) . . ?
O006 V01 O003 173.02(16) . . ?
O006 V01 O004 99.88(17) . . ?
O006 V01 O005 99.50(18) . . ?
O006 V01 N007 92.26(17) . . ?
C00A O002 V01 133.8(3) . . ?
C00B O003 V01 129.3(3) . . ?
C00F O004 V01 126.1(3) . . ?
C00C O005 V01 127.5(3) . . ?
C00P N007 V01 123.7(3) . . ?
C00R N007 V01 121.9(4) . . ?
C00R N007 C00P 114.0(4) . . ?
C00M C008 C009 123.3(4) . . ?
C00M C008 C00S 112.7(5) . . ?
C00S C008 C009 123.9(4) . . ?
C00D C009 C008 120.8(4) . . ?
C00E C009 C008 121.5(4) . . ?
C00E C009 C00D 117.7(5) . . ?
O002 C00A C00I 124.8(5) . . ?
O002 C00A C00O 115.1(5) . . ?
C00I C00A C00O 120.1(5) . . ?
O003 C00B C00I 124.2(5) . . ?
O003 C00B C00Q 116.1(6) . . ?
C00I C00B C00Q 119.7(6) . . ?
O005 C00C C00H 123.7(5) . . ?
O005 C00C C00L 116.3(5) . . ?
C00H C00C C00L 119.6(5) . . ?
C009 C00D H00D 119.8 . . ?
C00K C00D C009 120.5(5) . . ?
C00K C00D H00D 119.8 . . ?
C009 C00E H00E 119.7 . . ?
C00J C00E C009 120.6(5) . . ?
C00J C00E H00E 119.7 . . ?
O004 C00F C00H 124.8(5) . . ?
O004 C00F C00N 116.5(5) . . ?
C00H C00F C00N 118.6(5) . . ?
C00J C00G H00G 120.1 . . ?
C00K C00G H00G 120.1 . . ?
C00K C00G C00J 119.7(5) . . ?
C00C C00H H00H 117.6 . . ?
C00F C00H C00C 124.7(5) . . ?
C00F C00H H00H 117.6 . . ?
C00A C00I C00B 124.9(5) . . ?
C00A C00I H00I 117.6 . . ?
C00B C00I H00I 117.6 . . ?
C00E C00J H00J 119.6 . . ?
C00G C00J C00E 120.8(5) . . ?
C00G C00J H00J 119.6 . . ?
C00D C00K H00K 119.7 . . ?
C00G C00K C00D 120.7(6) . . ?
C00G C00K H00K 119.7 . . ?
C00C C00L H00A 109.5 . . ?
C00C C00L H00B 109.5 . . ?
C00C C00L H00C 109.5 . . ?
H00A C00L H00B 109.5 . . ?
H00A C00L H00C 109.5 . . ?
H00B C00L H00C 109.5 . . ?
C008 C00M H00M 118.8 . . ?
C008 C00M C00P 122.5(5) . . ?
C00P C00M H00M 118.8 . . ?
C00F C00N H00F 109.5 . . ?
C00F C00N H00L 109.5 . . ?
C00F C00N H00N 109.5 . . ?
H00F C00N H00L 109.5 . . ?
H00F C00N H00N 109.5 . . ?
H00L C00N H00N 109.5 . . ?
C00A C00O H00O 109.5 . . ?
C00A C00O H00P 109.5 . . ?
C00A C00O H00Q 109.5 . . ?
H00O C00O H00P 109.5 . . ?
H00O C00O H00Q 109.5 . . ?
H00P C00O H00Q 109.5 . . ?
N007 C00P C00M 123.6(5) . . ?
N007 C00P H00R 118.2 . . ?
C00M C00P H00R 118.2 . . ?
C00B C00Q H00S 109.5 . . ?
C00B C00Q H00T 109.5 . . ?
C00B C00Q H00U 109.5 . . ?
H00S C00Q H00T 109.5 . . ?
H00S C00Q H00U 109.5 . . ?
H00T C00Q H00U 109.5 . . ?
N007 C00R H00V 117.4 . . ?
N007 C00R C00S 125.3(5) . . ?
C00S C00R H00V 117.4 . . ?
C008 C00S C00R 121.9(5) . . ?
C008 C00S H00W 119.1 . . ?
C00R C00S H00W 119.1 . . ?

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
V01 O002 C00A C00I -0.7(7) . . . . ?
V01 O002 C00A C00O 178.6(4) . . . . ?
V01 O003 C00B C00I 1.9(7) . . . . ?
V01 O003 C00B C00Q -177.0(4) . . . . ?
V01 O004 C00F C00H 12.4(8) . . . . ?
V01 O004 C00F C00N -170.8(4) . . . . ?
V01 O005 C00C C00H -16.1(8) . . . . ?
V01 O005 C00C C00L 170.6(4) . . . . ?
V01 N007 C00P C00M 172.1(6) . . . . ?
V01 N007 C00R C00S -171.4(9) . . . . ?
O002 C00A C00I C00B 0.0(9) . . . . ?
O003 C00B C00I C00A -0.7(9) . . . . ?
O004 C00F C00H C00C 3.8(9) . . . . ?
O005 C00C C00H C00F -1.9(9) . . . . ?
N007 C00R C00S C008 -1.0(18) . . . . ?
C008 C009 C00D C00K -175.7(5) . . . . ?
C008 C009 C00E C00J 176.4(5) . . . . ?
C008 C00M C00P N007 -0.6(12) . . . . ?
C009 C008 C00M C00P -175.0(6) . . . . ?
C009 C008 C00S C00R 175.8(8) . . . . ?
C009 C00D C00K C00G -0.8(9) . . . . ?
C009 C00E C00J C00G -0.8(9) . . . . ?
C00D C009 C00E C00J -0.9(8) . . . . ?
C00E C009 C00D C00K 1.6(8) . . . . ?
C00J C00G C00K C00D -0.9(9) . . . . ?
C00K C00G C00J C00E 1.7(9) . . . . ?
C00L C00C C00H C00F 171.2(6) . . . . ?
C00M C008 C009 C00D 175.1(6) . . . . ?
C00M C008 C009 C00E -2.1(8) . . . . ?
C00M C008 C00S C00R -0.8(14) . . . . ?
C00N C00F C00H C00C -173.0(5) . . . . ?
C00O C00A C00I C00B -179.3(5) . . . . ?
C00P N007 C00R C00S 2.0(14) . . . . ?
C00Q C00B C00I C00A 178.2(6) . . . . ?
C00R N007 C00P C00M -1.2(11) . . . . ?
C00S C008 C009 C00D -1.1(9) . . . . ?
C00S C008 C009 C00E -178.3(7) . . . . ?
C00S C008 C00M C00P 1.6(11) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.149
_oxdiff_exptl_absorpt_empirical_full_min 0.701

####################################################################### 
# 
# 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_Nb-1
_database_code_depnum_ccdc_archive 'CCDC 2391112'
loop_
_audit_author_name
_audit_author_address
'Radoslaw Kaminski'
;University of Warsaw
Poland
;
_audit_update_record             
;
2024-10-15 deposited with the CCDC.	2025-05-29 downloaded from the CCDC.
;
#=======================================================================

# CHEMICAL DATA

_chemical_formula_moiety         'C6 H14 Cl3 N2 Nb O3'
_chemical_formula_sum            'C6 H14 Cl3 N2 Nb O3'
_chemical_formula_weight         361.5

#=======================================================================

# CRYSTAL DATA

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2

loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,-y,-z

_cell_length_a                   6.196(2)
_cell_length_b                   8.560(2)
_cell_length_c                   13.574(3)
_cell_angle_alpha                77.68(3)
_cell_angle_beta                 83.50(3)
_cell_angle_gamma                68.93(3)
_cell_volume                     655.8(3)

_cell_formula_units_Z            2

_cell_measurement_reflns_used    5312
_cell_measurement_theta_min      3.21
_cell_measurement_theta_max      75.18
_cell_measurement_temperature    100

_exptl_crystal_density_diffrn    1.8304
_exptl_crystal_F_000             360

_exptl_absorpt_coefficient_mu    13.061
_exptl_crystal_description       'small block'
_exptl_crystal_size_max          0.096
_exptl_crystal_size_mid          0.069
_exptl_crystal_size_min          0.036
_exptl_crystal_colour            colourless
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.43.113a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.45
_exptl_absorpt_correction_T_max  1

#=======================================================================

# EXPERIMENTAL DATA

_diffrn_ambient_temperature      100
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Atlas'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2687
_diffrn_measurement_method       'ω scans'

_diffrn_reflns_number            9586
_diffrn_reflns_theta_min         3.34
_diffrn_reflns_theta_max         76
_diffrn_reflns_theta_full        76
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measured_fraction_theta_full 0.99
_diffrn_reflns_av_R_equivalents  0.0585
_diffrn_reflns_av_unetI/netI     0.0414
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       17

_diffrn_radiation_probe          X-ray

#=======================================================================

# REFINEMENT DATA

_reflns_number_total             2695
_reflns_number_gt                2257
_reflns_threshold_expression     I>3σ(I)

_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_gt           0.0635
_refine_ls_wR_factor_gt          0.1507
_refine_ls_R_factor_all          0.0738
_refine_ls_wR_factor_ref         0.1638
_refine_ls_goodness_of_fit_ref   2.7650
_refine_ls_goodness_of_fit_gt    2.7921
_refine_ls_number_reflns         2695
_refine_ls_number_parameters     136
_refine_ls_number_restraints     0
_refine_ls_number_constraints    56
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.02P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_shift/su_max          0.0187
_refine_ls_shift/su_mean         0.0019
_refine_diff_density_max         2.09
_refine_diff_density_min         -1.67
_refine_ls_extinction_method     none

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
C 0.0181 0.0091 'International Tables Vol C tables 4.2.6.8 and 6.1.1.4' 2.31
20.843901 1.02 10.2075 1.5886 0.5687 0.865 51.651199 0.2156
H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.4'
0.493002 10.5109 0.322912 26.1257 0.140191 3.14236 0.04081 57.799702 0.003038
Cl 0.3639 0.7018 'International Tables Vol C tables 4.2.6.8 and 6.1.1.4'
11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574
N 0.0311 0.0180 'International Tables Vol C tables 4.2.6.8 and 6.1.1.4' 12.2126
0.0057 3.1322 9.8933 2.0125 28.997499 1.1663 0.5826 -11.529
Nb -0.1121 2.4826 'International Tables Vol C tables 4.2.6.8 and 6.1.1.4'
17.614201 1.18865 12.0144 11.766 4.04183 0.204785 3.53346 69.7957 3.75591
O 0.0492 0.0322 'International Tables Vol C tables 4.2.6.8 and 6.1.1.4' 3.0485
13.2771 2.2868 5.7011 1.5463 0.3239 0.867 32.908901 0.2508

_computing_data_collection       
'CrysAlisPro system (CCD 42.94a (release 21-06-2023))'
_computing_cell_refinement       'CrysAlisPro 1.171.43.113a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.113a (Rigaku OD, 2024)'

#=======================================================================

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_adp_type
_atom_site_U_iso_or_equiv
_atom_site_site_symmetry_multiplicity
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb -0.52795(10) 0.74980(8) 0.73502(5) Uani 0.0285(2) 2 1 d . . .
Cl1 Cl -0.6180(3) 0.5216(2) 0.69310(14) Uani 0.0335(6) 2 1 d . . .
Cl2 Cl -0.6782(3) 0.7088(3) 0.90289(14) Uani 0.0356(7) 2 1 d . . .
Cl3 Cl -0.3429(3) 0.9305(3) 0.77478(14) Uani 0.0363(7) 2 1 d . . .
O3 O -0.7646(10) 0.9080(8) 0.6815(4) Uani 0.038(2) 2 1 d . . .
O1 O -0.3266(9) 0.7522(7) 0.5984(4) Uani 0.0318(19) 2 1 d . . .
N1 N -0.0354(11) 0.7490(9) 0.4838(5) Uani 0.032(2) 2 1 d . . .
C1 C -0.1431(13) 0.7775(10) 0.5719(5) Uani 0.029(3) 2 1 d . . .
C2 C -0.1374(15) 0.6897(11) 0.4140(6) Uani 0.036(3) 2 1 d . . .
C3 C 0.1800(13) 0.7825(10) 0.4516(6) Uani 0.034(3) 2 1 d . . .
H1 H -0.075843 0.819115 0.616389 Uiso 0.0352 2 1 d . . .
H2a H -0.024414 0.650317 0.361985 Uiso 0.0433 2 1 d . . .
H2b H -0.186689 0.598051 0.449842 Uiso 0.0433 2 1 d . . .
H2c H -0.268237 0.781776 0.384064 Uiso 0.0433 2 1 d . . .
H3a H 0.150052 0.880052 0.397961 Uiso 0.0412 2 1 d . . .
H3b H 0.239872 0.804185 0.507495 Uiso 0.0412 2 1 d . . .
H3c H 0.291365 0.685134 0.428133 Uiso 0.0412 2 1 d . . .
O2 O -0.2085(9) 0.5351(7) 0.7866(5) Uani 0.035(2) 2 1 d . . .
N2 N 0.0466(12) 0.3150(9) 0.8816(5) Uani 0.035(3) 2 1 d . . .
C4 C -0.0437(12) 0.4739(9) 0.8462(6) Uani 0.030(2) 2 1 d . . .
C5 C -0.0387(16) 0.1885(9) 0.8594(7) Uani 0.042(3) 2 1 d . . .
C6 C 0.2462(17) 0.2541(17) 0.9451(8) Uani 0.057(4) 2 1 d . . .
H4 H 0.016888 0.550856 0.865854 Uiso 0.036 2 1 d . . .
H5a H 0.089452 0.09472 0.840782 Uiso 0.0504 2 1 d . . .
H5b H -0.119398 0.148057 0.918133 Uiso 0.0504 2 1 d . . .
H5c H -0.142292 0.239447 0.804729 Uiso 0.0504 2 1 d . . .
H6a H 0.377901 0.182518 0.911712 Uiso 0.0687 2 1 d . . .
H6b H 0.279432 0.349685 0.956874 Uiso 0.0687 2 1 d . . .
H6c H 0.212587 0.190183 1.008325 Uiso 0.0687 2 1 d . . .


#=======================================================================

# MOLECULAR GEOMETRY

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Nb1 Cl1 . . 2.404(3) ?
Nb1 Cl2 . . 2.366(2) ?
Nb1 Cl3 . . 2.402(3) ?
Nb1 O3 . . 1.704(6) ?
O1 C1 . . 1.233(10) ?
N1 C1 . . 1.326(10) ?
N1 C2 . . 1.459(13) ?
N1 C3 . . 1.465(12) ?
C1 H1 . . 0.96 ?
C2 H2a . . 0.96 ?
C2 H2b . . 0.96 ?
C2 H2c . . 0.96 ?
C3 H3a . . 0.96 ?
C3 H3b . . 0.96 ?
C3 H3c . . 0.96 ?
O2 C4 . . 1.262(9) ?
N2 C4 . . 1.277(10) ?
N2 C5 . . 1.459(14) ?
N2 C6 . . 1.459(13) ?
C4 H4 . . 0.96 ?
C5 H5a . . 0.96 ?
C5 H5b . . 0.96 ?
C5 H5c . . 0.96 ?
C6 H6a . . 0.96 ?
C6 H6b . . 0.96 ?
C6 H6c . . 0.96 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl1 Nb1 Cl2 . . . 93.62(8) ?
Cl1 Nb1 Cl3 . . . 166.03(7) ?
Cl1 Nb1 O3 . . . 95.3(3) ?
Cl2 Nb1 Cl3 . . . 90.93(9) ?
Cl2 Nb1 O3 . . . 98.9(2) ?
Cl3 Nb1 O3 . . . 97.1(3) ?
C1 N1 C2 . . . 119.8(8) ?
C1 N1 C3 . . . 122.1(8) ?
C2 N1 C3 . . . 118.1(7) ?
O1 C1 N1 . . . 122.2(9) ?
O1 C1 H1 . . . 118.92 ?
N1 C1 H1 . . . 118.92 ?
N1 C2 H2a . . . 109.47 ?
N1 C2 H2b . . . 109.47 ?
N1 C2 H2c . . . 109.47 ?
H2a C2 H2b . . . 109.47 ?
H2a C2 H2c . . . 109.47 ?
H2b C2 H2c . . . 109.47 ?
N1 C3 H3a . . . 109.47 ?
N1 C3 H3b . . . 109.47 ?
N1 C3 H3c . . . 109.47 ?
H3a C3 H3b . . . 109.47 ?
H3a C3 H3c . . . 109.47 ?
H3b C3 H3c . . . 109.47 ?
C4 N2 C5 . . . 122.5(7) ?
C4 N2 C6 . . . 119.7(10) ?
C5 N2 C6 . . . 117.7(8) ?
O2 C4 N2 . . . 123.4(9) ?
O2 C4 H4 . . . 118.32 ?
N2 C4 H4 . . . 118.32 ?
N2 C5 H5a . . . 109.47 ?
N2 C5 H5b . . . 109.47 ?
N2 C5 H5c . . . 109.47 ?
H5a C5 H5b . . . 109.47 ?
H5a C5 H5c . . . 109.47 ?
H5b C5 H5c . . . 109.47 ?
N2 C6 H6a . . . 109.47 ?
N2 C6 H6b . . . 109.47 ?
N2 C6 H6c . . . 109.47 ?
H6a C6 H6b . . . 109.47 ?
H6a C6 H6c . . . 109.47 ?
H6b C6 H6c . . . 109.47 ?

#=======================================================================

# STRUCTURE-FACTOR LIST



####################################################################### 
# 
# 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_Ta-1
_database_code_depnum_ccdc_archive 'CCDC 2391113'
loop_
_audit_author_name
_audit_author_address
'Radoslaw Kaminski'
;University of Warsaw
Poland
;
_audit_update_record             
;
2024-10-15 deposited with the CCDC.	2025-05-29 downloaded from the CCDC.
;
#=======================================================================

# CHEMICAL DATA

_chemical_formula_moiety         '2(C11 H10 N), Cl6 Ta, C H2 Cl2, Cl'
_chemical_formula_sum            'C23 H22 Cl9 N2 Ta'
_chemical_formula_weight         826.5

#=======================================================================

# CRYSTAL DATA

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2

loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,-y,-z

_cell_length_a                   7.283(2)
_cell_length_b                   15.243(3)
_cell_length_c                   15.412(3)
_cell_angle_alpha                60.45(3)
_cell_angle_beta                 88.99(3)
_cell_angle_gamma                86.12(3)
_cell_volume                     1484.8(7)

_cell_formula_units_Z            2

_cell_measurement_reflns_used    7485
_cell_measurement_theta_min      3.23
_cell_measurement_theta_max      75.86
_cell_measurement_temperature    100

_exptl_crystal_density_diffrn    1.8486
_exptl_crystal_F_000             800

_exptl_absorpt_coefficient_mu    14.425
_exptl_crystal_description       'small cut crystal'
_exptl_crystal_size_max          0.052
_exptl_crystal_size_mid          0.037
_exptl_crystal_size_min          0.022
_exptl_crystal_colour            colourless
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.43.113a (Rigaku Oxford Diffraction, 2024)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.184
_exptl_absorpt_correction_T_max  0.277

#=======================================================================

# EXPERIMENTAL DATA

_diffrn_ambient_temperature      100
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Atlas'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2687
_diffrn_measurement_method       'ω scans'

_diffrn_reflns_number            15934
_diffrn_reflns_theta_min         3.3
_diffrn_reflns_theta_max         76.13
_diffrn_reflns_theta_full        73.6
_diffrn_measured_fraction_theta_max 0.96
_diffrn_measured_fraction_theta_full 0.98
_diffrn_reflns_av_R_equivalents  0.05
_diffrn_reflns_av_unetI/netI     0.0513
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19

_diffrn_radiation_probe          X-ray

#=======================================================================

# REFINEMENT DATA

_reflns_number_total             5995
_reflns_number_gt                4764
_reflns_threshold_expression     I>3σ(I)

_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_gt           0.0412
_refine_ls_wR_factor_gt          0.1109
_refine_ls_R_factor_all          0.0546
_refine_ls_wR_factor_ref         0.1207
_refine_ls_goodness_of_fit_ref   1.8029
_refine_ls_goodness_of_fit_gt    1.8699
_refine_ls_number_reflns         5995
_refine_ls_number_parameters     316
_refine_ls_number_restraints     0
_refine_ls_number_constraints    88
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.02P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_shift/su_max          0.0454
_refine_ls_shift/su_mean         0.0037
_refine_diff_density_max         1.96
_refine_diff_density_min         -1.35
_refine_ls_extinction_method     none

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
C 0.0181 0.0091 'International Tables Vol C tables 4.2.6.8 and 6.1.1.4' 2.31
20.843901 1.02 10.2075 1.5886 0.5687 0.865 51.651199 0.2156
H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.4'
0.493002 10.5109 0.322912 26.1257 0.140191 3.14236 0.04081 57.799702 0.003038
Cl 0.3639 0.7018 'International Tables Vol C tables 4.2.6.8 and 6.1.1.4'
11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574
N 0.0311 0.0180 'International Tables Vol C tables 4.2.6.8 and 6.1.1.4' 12.2126
0.0057 3.1322 9.8933 2.0125 28.997499 1.1663 0.5826 -11.529
Ta -5.7959 5.2718 'International Tables Vol C tables 4.2.6.8 and 6.1.1.4'
29.2024 1.77333 15.2293 9.37046 14.5135 0.295977 4.76492 63.364399 9.24354

_computing_data_collection       
'CrysAlisPro system (CCD 42.94a (release 21-06-2023))'
_computing_cell_refinement       'CrysAlisPro 1.171.43.113a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.113a (Rigaku OD, 2024)'

#=======================================================================

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_adp_type
_atom_site_U_iso_or_equiv
_atom_site_site_symmetry_multiplicity
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ta1 Ta 0.31792(5) 0.20726(2) 1.12954(2) Uani 0.02478(12) 2 1 d . . .
Cl1 Cl 0.3119(3) 0.19844(12) 1.28420(11) Uani 0.0288(6) 2 1 d . . .
Cl2 Cl 0.0712(3) 0.33199(13) 1.07176(12) Uani 0.0316(6) 2 1 d . . .
Cl3 Cl 0.5266(3) 0.33302(15) 1.07224(14) Uani 0.0390(8) 2 1 d . . .
Cl4 Cl 0.3246(2) 0.21460(12) 0.97252(11) Uani 0.0282(6) 2 1 d . . .
Cl5 Cl 0.5571(3) 0.07984(14) 1.18601(13) Uani 0.0364(7) 2 1 d . . .
Cl6 Cl 0.1038(3) 0.08247(13) 1.18211(12) Uani 0.0322(7) 2 1 d . . .
Cl7 Cl 0.4963(3) 0.32345(12) 0.59131(12) Uani 0.0302(6) 2 1 d . . .
N1 N 0.6979(8) 0.2251(4) 0.7914(4) Uani 0.026(2) 2 1 d . . .
C1 C 0.6749(11) 0.1245(5) 0.8368(5) Uani 0.029(3) 2 1 d . . .
C2 C 0.7322(10) 0.0635(5) 0.9339(5) Uani 0.029(3) 2 1 d . . .
C3 C 0.8099(11) 0.1064(5) 0.9843(5) Uani 0.031(3) 2 1 d . . .
C4 C 0.8348(10) 0.2092(5) 0.9363(5) Uani 0.026(3) 2 1 d . . .
C5 C 0.7761(10) 0.2695(5) 0.8367(5) Uani 0.025(3) 2 1 d . . .
C6 C 0.7925(11) 0.3788(5) 0.7793(5) Uani 0.029(3) 2 1 d . . .
C7 C 0.8356(11) 0.4256(5) 0.6763(5) Uani 0.029(3) 2 1 d . . .
C8 C 0.8454(11) 0.5289(6) 0.6212(6) Uani 0.036(3) 2 1 d . . .
C9 C 0.8153(12) 0.5880(6) 0.6670(6) Uani 0.040(3) 2 1 d . . .
C10 C 0.7786(12) 0.5428(6) 0.7682(6) Uani 0.035(3) 2 1 d . . .
C11 C 0.7684(11) 0.4386(5) 0.8232(6) Uani 0.031(3) 2 1 d . . .
H1 H 0.618733 0.096264 0.801062 Uiso 0.0352 2 1 d . . .
H2 H 0.718646 -0.007965 0.96651 Uiso 0.0351 2 1 d . . .
H3 H 0.846864 0.064628 1.053081 Uiso 0.0374 2 1 d . . .
H4 H 0.89149 0.238545 0.970803 Uiso 0.0308 2 1 d . . .
H7 H 0.857968 0.384993 0.64496 Uiso 0.0347 2 1 d . . .
H8 H 0.872949 0.560218 0.551516 Uiso 0.0433 2 1 d . . .
H9 H 0.819959 0.660045 0.62834 Uiso 0.0475 2 1 d . . .
H10 H 0.760348 0.583196 0.799969 Uiso 0.0421 2 1 d . . .
H11 H 0.743966 0.407597 0.893204 Uiso 0.0366 2 1 d . . .
H24 H 0.660163 0.262733 0.729749 Uiso 0.0394 2 1 d . . .
N2 N 0.3397(9) 0.6088(4) 0.6141(4) Uani 0.027(2) 2 1 d . . .
C12 C 0.3495(11) 0.5081(5) 0.6480(5) Uani 0.032(3) 2 1 d . . .
C13 C 0.3033(11) 0.4443(5) 0.7463(6) Uani 0.035(3) 2 1 d . . .
C14 C 0.2572(12) 0.4857(6) 0.8055(5) Uani 0.036(3) 2 1 d . . .
C15 C 0.2486(11) 0.5888(5) 0.7689(5) Uani 0.032(3) 2 1 d . . .
C16 C 0.2920(10) 0.6528(5) 0.6686(5) Uani 0.027(3) 2 1 d . . .
C17 C 0.2809(11) 0.7636(5) 0.6201(5) Uani 0.031(3) 2 1 d . . .
C18 C 0.3680(11) 0.8225(6) 0.5300(5) Uani 0.032(3) 2 1 d . . .
C19 C 0.3478(12) 0.9270(6) 0.4831(6) Uani 0.035(3) 2 1 d . . .
C20 C 0.2406(12) 0.9741(6) 0.5254(6) Uani 0.038(3) 2 1 d . . .
C21 C 0.1558(11) 0.9180(6) 0.6135(5) Uani 0.032(3) 2 1 d . . .
C22 C 0.1726(11) 0.8133(6) 0.6624(5) Uani 0.033(3) 2 1 d . . .
H12 H 0.387466 0.481439 0.605161 Uiso 0.0384 2 1 d . . .
H13 H 0.303607 0.372634 0.772133 Uiso 0.0421 2 1 d . . .
H14 H 0.230135 0.441861 0.87433 Uiso 0.0433 2 1 d . . .
H15 H 0.213588 0.616407 0.81139 Uiso 0.0381 2 1 d . . .
H18 H 0.442487 0.790215 0.500411 Uiso 0.038 2 1 d . . .
H19 H 0.408146 0.966757 0.421189 Uiso 0.0425 2 1 d . . .
H20 H 0.226151 1.046585 0.492553 Uiso 0.046 2 1 d . . .
H21 H 0.083004 0.951567 0.642411 Uiso 0.038 2 1 d . . .
H22 H 0.111292 0.774751 0.724254 Uiso 0.0393 2 1 d . . .
H25 H 0.36648 0.647995 0.551943 Uiso 0.0406 2 1 d . . .
Cl8 Cl 1.0260(3) -0.2036(2) 1.39439(17) Uani 0.0523(10) 2 1 d . . .
Cl9 Cl 0.8308(3) -0.15616(14) 1.21056(13) Uani 0.0355(7) 2 1 d . . .
C23 C 0.8256(11) -0.1444(6) 1.3188(5) Uani 0.034(3) 2 1 d . . .
H23a H 0.815095 -0.074178 1.300172 Uiso 0.0404 2 1 d . . .
H23b H 0.7187 -0.174258 1.356563 Uiso 0.0404 2 1 d . . .


#=======================================================================

# MOLECULAR GEOMETRY

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ta1 Cl1 . . 2.320(2) ?
Ta1 Cl2 . . 2.358(2) ?
Ta1 Cl3 . . 2.333(3) ?
Ta1 Cl4 . . 2.366(2) ?
Ta1 Cl5 . . 2.344(2) ?
Ta1 Cl6 . . 2.354(2) ?
N1 C1 . . 1.357(9) ?
N1 C5 . . 1.343(12) ?
N1 H24 . . 0.87 ?
C1 C2 . . 1.369(9) ?
C1 H1 . . 0.96 ?
C2 C3 . . 1.385(14) ?
C2 H2 . . 0.96 ?
C3 C4 . . 1.388(10) ?
C3 H3 . . 0.96 ?
C4 C5 . . 1.401(9) ?
C4 H4 . . 0.96 ?
C5 C6 . . 1.463(9) ?
C6 C7 . . 1.422(10) ?
C6 C11 . . 1.379(14) ?
C7 C8 . . 1.379(10) ?
C7 H7 . . 0.96 ?
C8 C9 . . 1.396(16) ?
C8 H8 . . 0.96 ?
C9 C10 . . 1.390(12) ?
C9 H9 . . 0.96 ?
C10 C11 . . 1.390(10) ?
C10 H10 . . 0.96 ?
C11 H11 . . 0.96 ?
N2 C12 . . 1.352(10) ?
N2 C16 . . 1.339(12) ?
N2 H25 . . 0.87 ?
C12 C13 . . 1.388(10) ?
C12 H12 . . 0.96 ?
C13 C14 . . 1.369(15) ?
C13 H13 . . 0.96 ?
C14 C15 . . 1.380(12) ?
C14 H14 . . 0.96 ?
C15 C16 . . 1.407(9) ?
C15 H15 . . 0.96 ?
C16 C17 . . 1.469(11) ?
C17 C18 . . 1.398(10) ?
C17 C22 . . 1.416(13) ?
C18 C19 . . 1.384(11) ?
C18 H18 . . 0.96 ?
C19 C20 . . 1.386(14) ?
C19 H19 . . 0.96 ?
C20 C21 . . 1.361(10) ?
C20 H20 . . 0.96 ?
C21 C22 . . 1.386(11) ?
C21 H21 . . 0.96 ?
C22 H22 . . 0.96 ?
C23 H23a . . 0.96 ?
C23 H23b . . 0.96 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl1 Ta1 Cl2 . . . 90.73(7) ?
Cl1 Ta1 Cl3 . . . 90.76(8) ?
Cl1 Ta1 Cl4 . . . 179.47(6) ?
Cl1 Ta1 Cl5 . . . 90.20(8) ?
Cl1 Ta1 Cl6 . . . 90.85(7) ?
Cl2 Ta1 Cl3 . . . 90.03(8) ?
Cl2 Ta1 Cl4 . . . 89.68(7) ?
Cl2 Ta1 Cl5 . . . 178.11(8) ?
Cl2 Ta1 Cl6 . . . 89.09(7) ?
Cl3 Ta1 Cl4 . . . 89.58(8) ?
Cl3 Ta1 Cl5 . . . 91.61(8) ?
Cl3 Ta1 Cl6 . . . 178.18(7) ?
Cl4 Ta1 Cl5 . . . 89.38(8) ?
Cl4 Ta1 Cl6 . . . 88.82(7) ?
Cl5 Ta1 Cl6 . . . 89.24(8) ?
C1 N1 C5 . . . 123.3(6) ?
C1 N1 H24 . . . 118.34 ?
C5 N1 H24 . . . 118.34 ?
N1 C1 C2 . . . 119.6(8) ?
N1 C1 H1 . . . 120.18 ?
C2 C1 H1 . . . 120.18 ?
C1 C2 C3 . . . 119.1(7) ?
C1 C2 H2 . . . 120.47 ?
C3 C2 H2 . . . 120.47 ?
C2 C3 C4 . . . 120.5(6) ?
C2 C3 H3 . . . 119.75 ?
C4 C3 H3 . . . 119.75 ?
C3 C4 C5 . . . 119.1(8) ?
C3 C4 H4 . . . 120.45 ?
C5 C4 H4 . . . 120.46 ?
N1 C5 C4 . . . 118.4(6) ?
N1 C5 C6 . . . 117.9(6) ?
C4 C5 C6 . . . 123.8(8) ?
C5 C6 C7 . . . 120.3(8) ?
C5 C6 C11 . . . 121.3(7) ?
C7 C6 C11 . . . 118.4(6) ?
C6 C7 C8 . . . 120.4(9) ?
C6 C7 H7 . . . 119.79 ?
C8 C7 H7 . . . 119.79 ?
C7 C8 C9 . . . 119.9(8) ?
C7 C8 H8 . . . 120.05 ?
C9 C8 H8 . . . 120.05 ?
C8 C9 C10 . . . 120.2(7) ?
C8 C9 H9 . . . 119.9 ?
C10 C9 H9 . . . 119.9 ?
C9 C10 C11 . . . 119.5(10) ?
C9 C10 H10 . . . 120.23 ?
C11 C10 H10 . . . 120.23 ?
C6 C11 C10 . . . 121.5(7) ?
C6 C11 H11 . . . 119.27 ?
C10 C11 H11 . . . 119.27 ?
C12 N2 C16 . . . 125.1(6) ?
C12 N2 H25 . . . 117.46 ?
C16 N2 H25 . . . 117.46 ?
N2 C12 C13 . . . 118.4(9) ?
N2 C12 H12 . . . 120.78 ?
C13 C12 H12 . . . 120.78 ?
C12 C13 C14 . . . 118.5(7) ?
C12 C13 H13 . . . 120.73 ?
C14 C13 H13 . . . 120.73 ?
C13 C14 C15 . . . 121.8(7) ?
C13 C14 H14 . . . 119.12 ?
C15 C14 H14 . . . 119.12 ?
C14 C15 C16 . . . 119.1(9) ?
C14 C15 H15 . . . 120.47 ?
C16 C15 H15 . . . 120.47 ?
N2 C16 C15 . . . 117.1(7) ?
N2 C16 C17 . . . 118.8(6) ?
C15 C16 C17 . . . 124.1(8) ?
C16 C17 C18 . . . 121.6(8) ?
C16 C17 C22 . . . 119.8(6) ?
C18 C17 C22 . . . 118.5(7) ?
C17 C18 C19 . . . 120.6(9) ?
C17 C18 H18 . . . 119.71 ?
C19 C18 H18 . . . 119.71 ?
C18 C19 C20 . . . 120.0(7) ?
C18 C19 H19 . . . 119.98 ?
C20 C19 H19 . . . 119.98 ?
C19 C20 C21 . . . 120.1(7) ?
C19 C20 H20 . . . 119.93 ?
C21 C20 H20 . . . 119.93 ?
C20 C21 C22 . . . 121.3(9) ?
C20 C21 H21 . . . 119.33 ?
C22 C21 H21 . . . 119.33 ?
C17 C22 C21 . . . 119.4(7) ?
C17 C22 H22 . . . 120.31 ?
C21 C22 H22 . . . 120.31 ?
H23a C23 H23b . . . 107.29 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N1 H24 Cl7 . . . 0.87 2.20 3.035(7) 161.74 ?
N2 H25 Cl7 . . 2_666 0.87 2.26 3.053(7) 152.02 ?

#=======================================================================

# STRUCTURE-FACTOR LIST



