# Electronic Supplementary Material (ESI) 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_I-1
_database_code_depnum_ccdc_archive 'CCDC 2331117'
loop_
_audit_author_name
_audit_author_address
'Christopher Durr'
;Amherst College
United States of America
;
_audit_update_record             
;
2024-02-05 deposited with the CCDC.	2024-03-19 downloaded from the CCDC.
;
_audit_creation_date             2022-05-16
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C18 H28 N Nb O5'
_chemical_formula_sum            'C18 H28 N Nb O5'
_chemical_formula_weight         431.32
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H N O Nb'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -0.1121 2.4826 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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           9
_space_group_name_H-M_alt        'C 1 c 1'
_space_group_name_Hall           'C -2yc'
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'

_cell_length_a                   30.4282(3)
_cell_length_b                   8.11400(10)
_cell_length_c                   15.99700(10)
_cell_angle_alpha                90
_cell_angle_beta                 98.4580(10)
_cell_angle_gamma                90
_cell_volume                     3906.61(7)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    28134
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      67.9400
_cell_measurement_theta_min      2.9270
_shelx_estimated_absorpt_T_max   0.744
_shelx_estimated_absorpt_T_min   0.391
_exptl_absorpt_coefficient_mu    5.248
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74150
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.110a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1792
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-20 0 1 0.0299
-4 5 -1 0.0900
20 0 -1 0.0282
-18 2 3 0.0395
-2 -1 -10 0.0230
18 -2 -3 0.0419
1 1 10 0.0439
1 -2 0 0.1042

_exptl_crystal_size_max          0.219
_exptl_crystal_size_mid          0.078
_exptl_crystal_size_min          0.06
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-19.6973 -0.0315 0.7189 -0.2983 0.0743 0.9516
-3.9771 5.1028 -1.1600 0.8443 -0.1999 0.4971
19.6948 0.1425 -0.7472 0.3179 -0.0790 -0.9448
-18.2303 1.8343 3.1021 -0.0389 -0.2758 0.9604
-2.0872 -0.9396 -9.8852 0.1272 0.9796 0.1553
18.0881 -1.8550 -3.3906 0.0426 0.3046 -0.9515
1.4252 1.0003 9.9453 -0.1280 -0.9845 -0.1202
1.0003 -1.9988 -0.0026 -0.3238 0.1240 -0.1626

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            36703
_diffrn_reflns_point_group_measured_fraction_full 0.882
_diffrn_reflns_point_group_measured_fraction_max 0.881
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.942
_diffrn_reflns_theta_min         2.936
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -19.00  77.00   0.50    0.40    --   41.95-101.00 106.00  192
  2  ω    -77.00  19.00   0.50    0.40    --  -42.26 101.00-149.00  192
  3  ω     84.00 165.00   0.50    1.20    --   93.72 101.00-149.00  162
  4  ω     23.00 107.00   0.50    1.20    --   93.72-101.00 106.00  168
  5  ω   -107.00 -23.00   0.50    1.20    --  -94.03 101.00-149.00  168
  6  ω   -165.00 -84.00   0.50    1.20    --  -94.03-101.00 106.00  162
  7  ω     27.00 108.00   0.50    0.40    --   41.95  43.00 150.00  162
  8  ω    -23.00  48.00   0.50    0.40    --   41.95 -43.00 -30.00  142
  9  ω     19.00  99.00   0.50    0.40    --   41.95-138.00  60.00  160
 10  ω    -33.00  24.00   0.50    0.40    --   41.95 -11.00 120.00  114
 11  ω     28.00 112.00   0.50    0.40    --   41.95  21.00  60.00  168
 12  ω    -25.00  68.00   0.50    0.40    --   41.95 -77.00-120.00  186
 13  ω    -33.00  24.00   0.50    0.40    --   41.95 -11.00-180.00  114
 14  ω   -112.00 -29.00   0.50    0.40    --  -42.26 -21.00 -60.00  166
 15  ω    -28.00  28.00   0.50    0.40    --  -42.26  21.00 150.00  112
 16  ω   -109.00 -79.00   0.50    0.40    --  -42.26-138.00  90.00   60
 17  ω   -109.00 -79.00   0.50    0.40    --  -42.26-138.00 150.00   60
 18  ω    -24.00  32.00   0.50    0.40    --  -42.26  11.00 150.00  112
 19  ω   -109.00 -79.00   0.50    0.40    --  -42.26-138.00-120.00   60
 20  ω    -24.00  32.00   0.50    0.40    --  -42.26  11.00 -30.00  112
 21  ω    -37.00  24.00   0.50    0.40    --  -42.26  32.00-150.00  122
 22  ω     28.00 109.00   0.50    1.20    --   93.72-117.00 -90.00  162
 23  ω     28.00  57.00   0.50    1.20    --   93.72 -50.00 150.00   58
 24  ω     83.00 162.00   0.50    1.20    --   93.72  25.00-180.00  158
 25  ω     76.00 160.00   0.50    1.20    --   93.72  50.00  60.00  168
 26  ω     28.00  57.00   0.50    1.20    --   93.72 -50.00 120.00   58
 27  ω     28.00  57.00   0.50    1.20    --   93.72 -50.00-180.00   58
 28  ω     27.00 127.00   0.50    1.20    --   93.72-145.00 120.00  200
 29  ω     25.00 105.00   0.50    1.20    --   93.72 -77.00 120.00  160
 30  ω     28.00  57.00   0.50    1.20    --   93.72 -50.00  90.00   58
 31  ω     79.00 160.00   0.50    1.20    --   93.72  42.00 -30.00  162
 32  ω     26.00  83.00   0.50    1.20    --   93.72 -68.00  90.00  114
 33  ω     28.00 109.00   0.50    1.20    --   93.72-117.00 -60.00  162
 34  ω     92.00 159.00   0.50    1.20    --   93.72 117.00  90.00  134
 35  ω     87.00 161.00   0.50    1.20    --   93.72  59.00-180.00  148
 36  ω    101.00 162.00   0.50    1.20    --   93.72  77.00-120.00  122
 37  ω     97.00 162.00   0.50    1.20    --   93.72  68.00 -30.00  130
 38  ω   -109.00 -29.00   0.50    1.20    --  -94.03 117.00 120.00  160
 39  ω   -162.00-101.00   0.50    1.20    --  -94.03 -77.00-120.00  122
 40  ω    -83.00 -26.00   0.50    1.20    --  -94.03  68.00-150.00  114
 41  ω   -163.00-101.00   0.50    1.20    --  -94.03 -87.00   0.00  124
 42  ω   -161.00 -97.00   0.50    1.20    --  -94.03 -68.00 -30.00  128
 43  ω    -68.00 -27.00   0.50    1.20    --  -94.03  59.00-120.00   82
 44  ω   -160.00 -87.00   0.50    1.20    --  -94.03 -59.00-180.00  146
 45  ω   -106.00 -22.00   0.50    1.20    --  -94.03  96.00  30.00  168
 46  ω   -109.00 -29.00   0.50    1.20    --  -94.03 117.00  30.00  160
 47  ω   -160.00 -87.00   0.50    1.20    --  -94.03 -59.00  60.00  146
 48  ω    -57.00 -28.00   0.50    1.20    --  -94.03  50.00  60.00   58
 49  ω   -159.00 -92.00   0.50    1.20    --  -94.03-117.00 150.00  134
 50  ω   -163.00 -83.00   0.50    1.20    --  -94.03 -25.00   0.00  160
 51  ω     23.00 108.00   0.50    0.40    --   41.95  54.00 120.00  170
 52  ω     23.00 108.00   0.50    0.40    --   41.95  54.00 150.00  170
 53  ω     23.00 108.00   0.50    0.40    --   41.95  54.00-180.00  170
 54  ω     23.00 108.00   0.50    0.40    --   41.95  54.00 -30.00  170
 55  ω     23.00 108.00   0.50    0.40    --   41.95  54.00  90.00  170
 56  ω     23.00 108.00   0.50    0.40    --   41.95  54.00  30.00  170
 57  ω     23.00 108.00   0.50    0.40    --   41.95  54.00-120.00  170
 58  ω     23.00 108.00   0.50    0.40    --   41.95  54.00 -90.00  170
 59  ω     23.00 108.00   0.50    0.40    --   41.95  54.00-150.00  170
 60  ω     23.00 108.00   0.50    0.40    --   41.95  54.00  60.00  170
 61  ω   -108.00 -24.00   0.50    0.40    --  -42.26 -54.00-120.00  168
 62  ω   -108.00 -24.00   0.50    0.40    --  -42.26 -54.00 -60.00  168
 63  ω   -108.00 -24.00   0.50    0.40    --  -42.26 -54.00-150.00  168
 64  ω   -108.00 -24.00   0.50    0.40    --  -42.26 -54.00-180.00  168
 65  ω   -108.00 -24.00   0.50    0.40    --  -42.26 -54.00 -90.00  168
 66  ω     76.00 160.00   0.50    1.20    --   93.72  50.00   0.00  168
 67  ω     28.00  57.00   0.50    1.20    --   93.72 -50.00 -90.00   58
 68  ω     76.00 160.00   0.50    1.20    --   93.72  50.00 -90.00  168
 69  ω     76.00 160.00   0.50    1.20    --   93.72  50.00 120.00  168
 70  ω   -160.00 -77.00   0.50    1.20    --  -94.03 -50.00-150.00  166
 71  ω    -57.00 -28.00   0.50    1.20    --  -94.03  50.00  30.00   58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at home/near, HyPix3000'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0137130000
_diffrn_orient_matrix_UB_12      0.1689148000
_diffrn_orient_matrix_UB_13      -0.0318219000
_diffrn_orient_matrix_UB_21      -0.0070049000
_diffrn_orient_matrix_UB_22      -0.0654212000
_diffrn_orient_matrix_UB_23      -0.0914034000
_diffrn_orient_matrix_UB_31      -0.0487958000
_diffrn_orient_matrix_UB_32      0.0569329000
_diffrn_orient_matrix_UB_33      -0.0108235000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.763
_reflns_Friedel_fraction_full    0.765
_reflns_Friedel_fraction_max     0.763
_reflns_number_gt                6106
_reflns_number_total             6259
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.65
_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 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.676
_refine_diff_density_min         -0.656
_refine_diff_density_rms         0.067
_refine_ls_abs_structure_details 
;
 Flack x determined using 2547 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.033(6)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         6259
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0286
_refine_ls_restrained_S_all      1.060
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0546P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0735
_refine_ls_wR_factor_ref         0.0741
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C15(H15A,H15B), C17(H17A,H17B), C31(H31A,H31B), C33(H33A,
 H33B), C35(H35A,H35B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C9(H9), C20(H20), C21(H21), C23(H23), C26(H26)
2.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,
 H14C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C28(H28A,H28B,H28C), C29(H29A,
 H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C),
 C36(H36A,H36B,H36C)
;
_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
Nb1 Nb 0.62573(2) 0.66112(4) 0.54365(2) 0.02343(11) Uani 1 1 d . . . . .
O1 O 0.67855(12) 0.7680(4) 0.5114(2) 0.0273(7) Uani 1 1 d . . . . .
O2 O 0.57104(13) 0.5132(4) 0.5257(2) 0.0281(8) Uani 1 1 d . . . . .
O3 O 0.58425(13) 0.8316(4) 0.5093(2) 0.0282(8) Uani 1 1 d . . . . .
O4 O 0.63530(13) 0.7443(4) 0.6571(2) 0.0302(8) Uani 1 1 d . . . . .
O5 O 0.65348(13) 0.4592(4) 0.5783(2) 0.0276(7) Uani 1 1 d . . . . .
N1 N 0.62547(14) 0.5985(5) 0.4038(2) 0.0225(8) Uani 1 1 d . . . . .
C1 C 0.69498(17) 0.7273(6) 0.4399(3) 0.0254(10) Uani 1 1 d . . . . .
C2 C 0.73738(17) 0.7730(6) 0.4273(3) 0.0274(10) Uani 1 1 d . . . . .
H2 H 0.755171 0.840018 0.467692 0.033 Uiso 1 1 calc R U . . .
C3 C 0.75362(17) 0.7201(6) 0.3554(3) 0.0279(10) Uani 1 1 d . . . . .
H3 H 0.782509 0.752976 0.346254 0.033 Uiso 1 1 calc R U . . .
C4 C 0.72822(18) 0.6194(6) 0.2960(3) 0.0279(10) Uani 1 1 d . . . . .
C5 C 0.68527(17) 0.5771(6) 0.3086(3) 0.0250(10) Uani 1 1 d . . . . .
H5 H 0.667672 0.508396 0.268834 0.030 Uiso 1 1 calc R U . . .
C6 C 0.66790(17) 0.6346(6) 0.3791(3) 0.0228(10) Uani 1 1 d . . . . .
C7 C 0.74787(19) 0.5535(7) 0.2214(3) 0.0337(11) Uani 1 1 d . . . . .
H7A H 0.754515 0.645448 0.185506 0.051 Uiso 1 1 calc R U . . .
H7B H 0.726561 0.479060 0.188598 0.051 Uiso 1 1 calc R U . . .
H7C H 0.775306 0.493294 0.241539 0.051 Uiso 1 1 calc R U . . .
C8 C 0.58975(17) 0.5651(6) 0.3500(3) 0.0242(10) Uani 1 1 d . . . . .
C9 C 0.54967(19) 0.5094(6) 0.3772(3) 0.0264(11) Uani 1 1 d . . . . .
H9 H 0.525038 0.492051 0.334245 0.032 Uiso 1 1 calc R U . . .
C10 C 0.54277(19) 0.4781(6) 0.4588(3) 0.0269(11) Uani 1 1 d . . . . .
C11 C 0.58708(17) 0.5818(7) 0.2552(3) 0.0283(11) Uani 1 1 d . . . . .
H11A H 0.606431 0.671913 0.242283 0.042 Uiso 1 1 calc R U . . .
H11B H 0.556362 0.605630 0.230283 0.042 Uiso 1 1 calc R U . . .
H11C H 0.596705 0.478627 0.231712 0.042 Uiso 1 1 calc R U . . .
C12 C 0.50113(18) 0.3960(7) 0.4771(3) 0.0328(11) Uani 1 1 d . . . . .
H12A H 0.508554 0.289319 0.504313 0.049 Uiso 1 1 calc R U . . .
H12B H 0.480960 0.378961 0.424169 0.049 Uiso 1 1 calc R U . . .
H12C H 0.486637 0.465968 0.514899 0.049 Uiso 1 1 calc R U . . .
C13 C 0.54022(19) 0.8875(7) 0.4919(3) 0.0313(11) Uani 1 1 d . . . . .
H13A H 0.534193 0.964627 0.536806 0.038 Uiso 1 1 calc R U . . .
H13B H 0.519692 0.792757 0.491617 0.038 Uiso 1 1 calc R U . . .
C14 C 0.5320(2) 0.9736(7) 0.4073(4) 0.0371(13) Uani 1 1 d . . . . .
H14A H 0.536846 0.895891 0.362633 0.056 Uiso 1 1 calc R U . . .
H14B H 0.552549 1.066655 0.407436 0.056 Uiso 1 1 calc R U . . .
H14C H 0.501351 1.013962 0.396990 0.056 Uiso 1 1 calc R U . . .
C15 C 0.6328(2) 0.9069(7) 0.6901(4) 0.0370(12) Uani 1 1 d . . . . .
H15A H 0.608884 0.969067 0.654955 0.044 Uiso 1 1 calc R U . . .
H15B H 0.661216 0.965142 0.688228 0.044 Uiso 1 1 calc R U . . .
C16 C 0.6236(2) 0.8997(8) 0.7785(4) 0.0372(13) Uani 1 1 d . . . . .
H16A H 0.594718 0.847148 0.779866 0.056 Uiso 1 1 calc R U . . .
H16B H 0.623131 1.011726 0.801299 0.056 Uiso 1 1 calc R U . . .
H16C H 0.646887 0.835543 0.812881 0.056 Uiso 1 1 calc R U . . .
C17 C 0.6477(2) 0.2851(6) 0.5801(3) 0.0304(11) Uani 1 1 d . . . . .
H17A H 0.617157 0.259272 0.590392 0.036 Uiso 1 1 calc R U . . .
H17B H 0.668752 0.237476 0.627031 0.036 Uiso 1 1 calc R U . . .
C18 C 0.6556(2) 0.2096(7) 0.4982(4) 0.0414(14) Uani 1 1 d . . . . .
H18A H 0.635055 0.257780 0.451715 0.062 Uiso 1 1 calc R U . . .
H18B H 0.650743 0.090325 0.499952 0.062 Uiso 1 1 calc R U . . .
H18C H 0.686284 0.231249 0.489223 0.062 Uiso 1 1 calc R U . . .
Nb2 Nb 0.36558(2) 0.50651(4) 0.48807(2) 0.02292(11) Uani 1 1 d . . . . .
O6 O 0.41310(13) 0.5206(4) 0.5879(2) 0.0276(8) Uani 1 1 d . . . . .
O7 O 0.31547(12) 0.5900(4) 0.4040(2) 0.0268(7) Uani 1 1 d . . . . .
O8 O 0.32382(12) 0.4665(4) 0.5632(2) 0.0278(7) Uani 1 1 d . . . . .
O9 O 0.37077(12) 0.2844(4) 0.4540(2) 0.0280(7) Uani 1 1 d . . . . .
O10 O 0.40556(12) 0.5892(4) 0.4177(2) 0.0258(7) Uani 1 1 d . . . . .
N2 N 0.36393(15) 0.7727(5) 0.5333(3) 0.0242(8) Uani 1 1 d . . . . .
C19 C 0.42974(18) 0.6700(6) 0.6132(3) 0.0264(11) Uani 1 1 d . . . . .
C20 C 0.4704(2) 0.6859(7) 0.6640(3) 0.0310(11) Uani 1 1 d . . . . .
H20 H 0.486702 0.590564 0.684353 0.037 Uiso 1 1 calc R U . . .
C21 C 0.4873(2) 0.8423(7) 0.6853(3) 0.0324(12) Uani 1 1 d . . . . .
H21 H 0.514810 0.852624 0.721685 0.039 Uiso 1 1 calc R U . . .
C22 C 0.4649(2) 0.9833(6) 0.6543(3) 0.0303(12) Uani 1 1 d . . . . .
C23 C 0.42364(19) 0.9657(6) 0.6042(3) 0.0271(10) Uani 1 1 d . . . . .
H23 H 0.407784 1.061211 0.582690 0.032 Uiso 1 1 calc R U . . .
C24 C 0.40526(18) 0.8105(6) 0.5851(3) 0.0245(10) Uani 1 1 d . . . . .
C25 C 0.32854(18) 0.8663(6) 0.5252(3) 0.0258(10) Uani 1 1 d . . . . .
C26 C 0.28972(19) 0.8284(6) 0.4659(4) 0.0288(11) Uani 1 1 d . . . . .
H26 H 0.264650 0.897867 0.466724 0.035 Uiso 1 1 calc R U . . .
C27 C 0.28512(18) 0.7030(6) 0.4086(3) 0.0279(11) Uani 1 1 d . . . . .
C28 C 0.4849(2) 1.1525(7) 0.6733(4) 0.0363(13) Uani 1 1 d . . . . .
H28A H 0.487521 1.174006 0.734120 0.054 Uiso 1 1 calc R U . . .
H28B H 0.465627 1.235966 0.642418 0.054 Uiso 1 1 calc R U . . .
H28C H 0.514340 1.156910 0.655678 0.054 Uiso 1 1 calc R U . . .
C29 C 0.32452(19) 1.0207(6) 0.5766(3) 0.0290(11) Uani 1 1 d . . . . .
H29A H 0.342094 1.007904 0.632672 0.043 Uiso 1 1 calc R U . . .
H29B H 0.293288 1.038717 0.582527 0.043 Uiso 1 1 calc R U . . .
H29C H 0.335590 1.115366 0.547864 0.043 Uiso 1 1 calc R U . . .
C30 C 0.24483(19) 0.6849(7) 0.3439(4) 0.0355(12) Uani 1 1 d . . . . .
H30A H 0.253603 0.684365 0.287322 0.053 Uiso 1 1 calc R U . . .
H30B H 0.224607 0.777394 0.348530 0.053 Uiso 1 1 calc R U . . .
H30C H 0.229794 0.581207 0.353212 0.053 Uiso 1 1 calc R U . . .
C31 C 0.3088(2) 0.5162(7) 0.6384(4) 0.0355(13) Uani 1 1 d . . . . .
H31A H 0.319383 0.629660 0.652642 0.043 Uiso 1 1 calc R U . . .
H31B H 0.321820 0.442817 0.685048 0.043 Uiso 1 1 calc R U . . .
C32 C 0.2591(2) 0.5119(7) 0.6316(4) 0.0398(14) Uani 1 1 d . . . . .
H32A H 0.246019 0.584011 0.585304 0.060 Uiso 1 1 calc R U . . .
H32B H 0.250152 0.550166 0.684709 0.060 Uiso 1 1 calc R U . . .
H32C H 0.248542 0.398861 0.620157 0.060 Uiso 1 1 calc R U . . .
C33 C 0.3881(2) 0.1714(6) 0.4000(3) 0.0318(12) Uani 1 1 d . . . . .
H33A H 0.371152 0.067186 0.398873 0.038 Uiso 1 1 calc R U . . .
H33B H 0.419400 0.146844 0.423430 0.038 Uiso 1 1 calc R U . . .
C34 C 0.3864(2) 0.2335(8) 0.3117(4) 0.0403(14) Uani 1 1 d . . . . .
H34A H 0.399096 0.150727 0.277634 0.060 Uiso 1 1 calc R U . . .
H34B H 0.403460 0.335957 0.312224 0.060 Uiso 1 1 calc R U . . .
H34C H 0.355414 0.254509 0.287384 0.060 Uiso 1 1 calc R U . . .
C35 C 0.42300(18) 0.7230(6) 0.3766(3) 0.0288(10) Uani 1 1 d . . . . .
H35A H 0.453732 0.696985 0.367531 0.035 Uiso 1 1 calc R U . . .
H35B H 0.424060 0.822019 0.413008 0.035 Uiso 1 1 calc R U . . .
C36 C 0.3950(2) 0.7585(8) 0.2930(4) 0.0406(13) Uani 1 1 d . . . . .
H36A H 0.396924 0.665547 0.254505 0.061 Uiso 1 1 calc R U . . .
H36B H 0.405914 0.858607 0.268538 0.061 Uiso 1 1 calc R U . . .
H36C H 0.364051 0.774368 0.301310 0.061 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
Nb1 O1 1.961(4) . ?
Nb1 O2 2.038(4) . ?
Nb1 O3 1.899(4) . ?
Nb1 O4 1.918(3) . ?
Nb1 O5 1.889(3) . ?
Nb1 N1 2.292(4) . ?
O1 C1 1.354(6) . ?
O2 C10 1.303(7) . ?
O3 C13 1.403(7) . ?
O4 C15 1.427(6) . ?
O5 C17 1.425(6) . ?
N1 C6 1.435(6) . ?
N1 C8 1.312(7) . ?
C1 C2 1.385(7) . ?
C1 C6 1.399(7) . ?
C2 C3 1.386(7) . ?
C3 C4 1.397(8) . ?
C4 C5 1.394(7) . ?
C4 C7 1.510(7) . ?
C5 C6 1.393(7) . ?
C8 C9 1.427(8) . ?
C8 C11 1.512(7) . ?
C9 C10 1.375(8) . ?
C10 C12 1.498(8) . ?
C13 C14 1.511(8) . ?
C15 C16 1.483(8) . ?
C17 C18 1.499(7) . ?
Nb2 O6 1.994(4) . ?
Nb2 O7 1.997(3) . ?
Nb2 O8 1.901(4) . ?
Nb2 O9 1.896(3) . ?
Nb2 O10 1.897(3) . ?
Nb2 N2 2.281(4) . ?
O6 C19 1.353(6) . ?
O7 C27 1.311(6) . ?
O8 C31 1.407(7) . ?
O9 C33 1.414(6) . ?
O10 C35 1.412(6) . ?
N2 C24 1.433(7) . ?
N2 C25 1.308(7) . ?
C19 C20 1.382(8) . ?
C19 C24 1.399(7) . ?
C20 C21 1.393(8) . ?
C21 C22 1.386(8) . ?
C22 C23 1.393(8) . ?
C22 C28 1.514(7) . ?
C23 C24 1.394(7) . ?
C25 C26 1.435(8) . ?
C25 C29 1.514(7) . ?
C26 C27 1.363(8) . ?
C27 C30 1.491(8) . ?
C31 C32 1.503(9) . ?
C33 C34 1.493(7) . ?
C35 C36 1.505(8) . ?

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 Nb1 O2 155.14(14) . . ?
O1 Nb1 N1 74.13(14) . . ?
O2 Nb1 N1 81.16(14) . . ?
O3 Nb1 O1 97.88(15) . . ?
O3 Nb1 O2 83.92(15) . . ?
O3 Nb1 O4 91.11(15) . . ?
O3 Nb1 N1 88.42(14) . . ?
O4 Nb1 O1 94.44(15) . . ?
O4 Nb1 O2 110.35(15) . . ?
O4 Nb1 N1 168.37(15) . . ?
O5 Nb1 O1 96.47(16) . . ?
O5 Nb1 O2 81.43(15) . . ?
O5 Nb1 O3 165.13(16) . . ?
O5 Nb1 O4 91.61(14) . . ?
O5 Nb1 N1 91.81(14) . . ?
C1 O1 Nb1 122.2(3) . . ?
C10 O2 Nb1 132.2(3) . . ?
C13 O3 Nb1 150.2(3) . . ?
C15 O4 Nb1 131.8(3) . . ?
C17 O5 Nb1 144.6(3) . . ?
C6 N1 Nb1 110.5(3) . . ?
C8 N1 Nb1 124.8(3) . . ?
C8 N1 C6 123.5(4) . . ?
O1 C1 C2 121.7(4) . . ?
O1 C1 C6 117.8(4) . . ?
C2 C1 C6 120.6(5) . . ?
C1 C2 C3 119.4(5) . . ?
C2 C3 C4 121.1(5) . . ?
C3 C4 C7 120.1(5) . . ?
C5 C4 C3 118.8(5) . . ?
C5 C4 C7 121.1(5) . . ?
C6 C5 C4 120.6(5) . . ?
C1 C6 N1 112.3(4) . . ?
C5 C6 N1 128.2(4) . . ?
C5 C6 C1 119.2(5) . . ?
N1 C8 C9 121.8(4) . . ?
N1 C8 C11 123.8(4) . . ?
C9 C8 C11 114.3(4) . . ?
C10 C9 C8 127.2(5) . . ?
O2 C10 C9 124.4(5) . . ?
O2 C10 C12 114.3(5) . . ?
C9 C10 C12 121.3(5) . . ?
O3 C13 C14 110.7(4) . . ?
O4 C15 C16 110.2(5) . . ?
O5 C17 C18 110.6(4) . . ?
O6 Nb2 O7 155.75(14) . . ?
O6 Nb2 N2 74.86(15) . . ?
O7 Nb2 N2 80.91(14) . . ?
O8 Nb2 O6 88.66(16) . . ?
O8 Nb2 O7 88.20(15) . . ?
O8 Nb2 N2 85.00(15) . . ?
O9 Nb2 O6 101.74(15) . . ?
O9 Nb2 O7 102.51(15) . . ?
O9 Nb2 O8 96.39(15) . . ?
O9 Nb2 O10 94.46(15) . . ?
O9 Nb2 N2 176.32(17) . . ?
O10 Nb2 O6 90.12(15) . . ?
O10 Nb2 O7 88.47(14) . . ?
O10 Nb2 O8 169.10(15) . . ?
O10 Nb2 N2 84.23(14) . . ?
C19 O6 Nb2 119.1(3) . . ?
C27 O7 Nb2 132.4(3) . . ?
C31 O8 Nb2 145.4(4) . . ?
C33 O9 Nb2 147.8(3) . . ?
C35 O10 Nb2 149.9(3) . . ?
C24 N2 Nb2 109.1(3) . . ?
C25 N2 Nb2 125.0(3) . . ?
C25 N2 C24 125.0(4) . . ?
O6 C19 C20 121.5(5) . . ?
O6 C19 C24 118.4(5) . . ?
C20 C19 C24 120.1(5) . . ?
C19 C20 C21 119.7(5) . . ?
C22 C21 C20 121.3(6) . . ?
C21 C22 C23 118.4(5) . . ?
C21 C22 C28 120.9(6) . . ?
C23 C22 C28 120.6(5) . . ?
C22 C23 C24 121.1(5) . . ?
C19 C24 N2 113.1(4) . . ?
C23 C24 N2 127.5(5) . . ?
C23 C24 C19 119.2(5) . . ?
N2 C25 C26 121.8(5) . . ?
N2 C25 C29 123.9(5) . . ?
C26 C25 C29 114.3(5) . . ?
C27 C26 C25 126.7(5) . . ?
O7 C27 C26 123.8(5) . . ?
O7 C27 C30 114.0(5) . . ?
C26 C27 C30 122.2(5) . . ?
O8 C31 C32 112.4(5) . . ?
O9 C33 C34 113.2(4) . . ?
O10 C35 C36 111.0(4) . . ?

_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 1.430
_oxdiff_exptl_absorpt_empirical_full_min 0.720
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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_C-4
_database_code_depnum_ccdc_archive 'CCDC 2331124'
loop_
_audit_author_name
_audit_author_address
'Christopher Durr'
;Amherst College
United States of America
;
_audit_update_record             
;
2024-02-05 deposited with the CCDC.	2024-03-19 downloaded from the CCDC.
;
_audit_creation_date             2024-01-03
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C19 H19 Cl N O5 Ta'
_chemical_formula_sum            'C19 H19 Cl N O5 Ta'
_chemical_formula_weight         557.75
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Ta Cl N O C H'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ta Ta -5.7959 5.2718 '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           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   15.1854(2)
_cell_length_b                   7.69460(10)
_cell_length_c                   16.3573(2)
_cell_angle_alpha                90
_cell_angle_beta                 95.7850(10)
_cell_angle_gamma                90
_cell_volume                     1901.54(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    26826
_cell_measurement_temperature    110.5(9)
_cell_measurement_theta_max      67.9140
_cell_measurement_theta_min      3.7620
_shelx_estimated_absorpt_T_max   0.640
_shelx_estimated_absorpt_T_min   0.580
_exptl_absorpt_coefficient_mu    12.233
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85985
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.93a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.948
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1080
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-4 -3 8 0.0187
8 0 5 0.0356
9 2 -3 0.0271
-9 -1 -1 0.0019
2 -5 2 0.0175
3 -1 -10 0.0201
-2 5 -3 0.0175
-3 2 9 0.0195

_exptl_crystal_size_max          0.049
_exptl_crystal_size_mid          0.037
_exptl_crystal_size_min          0.036
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-4.3305 -2.8860 7.7232 0.1108 -0.3821 0.9175
8.1563 0.0088 5.0593 -0.2604 0.8706 0.4175
8.6973 2.2164 -2.5782 -0.2566 0.8669 -0.4273
-9.2994 -1.2372 -1.3350 0.2852 -0.9584 0.0091
2.0453 -4.8042 1.6583 0.7329 0.2202 0.6437
2.8382 -1.2870 -10.0490 0.7160 0.2109 -0.6655
-1.6278 4.6548 -3.2282 -0.6298 -0.1899 -0.7532
-3.1230 2.2393 9.1677 -0.8339 -0.2466 0.4937

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            36004
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.125
_diffrn_reflns_theta_min         3.786
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110.5(9)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -26.00  68.00   0.50    1.00    --   41.95 -79.00 117.00  188
  2  ω    -68.00  26.00   0.50    1.00    --  -42.26  79.00-117.00  188
  3  ω   -162.00 -78.00   0.50    3.00    --  -94.03 -79.00 117.00  168
  4  ω   -120.00 -26.00   0.50    3.00    --  -94.03  79.00-117.00  188
  5  ω     31.00 108.00   0.50    1.00    --   41.95  32.00 -30.00  154
  6  ω    -28.00  28.00   0.50    1.00    --   41.95 -21.00   0.00  112
  7  ω     19.00  99.00   0.50    1.00    --   41.95-138.00-120.00  160
  8  ω     31.00 108.00   0.50    1.00    --   41.95  32.00  60.00  154
  9  ω    -33.00  24.00   0.50    1.00    --   41.95 -11.00 -60.00  114
 10  ω    -28.00  28.00   0.50    1.00    --   41.95 -21.00-150.00  112
 11  ω    -28.00  28.00   0.50    1.00    --  -42.26  21.00  60.00  112
 12  ω    -37.00  24.00   0.50    1.00    --  -42.26  32.00 120.00  122
 13  ω    -78.00   4.00   0.50    1.00    --  -42.26 104.00  30.00  164
 14  ω   -109.00 -27.00   0.50    1.00    --  -42.26 -43.00   0.00  164
 15  ω    -24.00  32.00   0.50    1.00    --  -42.26  11.00-120.00  112
 16  ω   -109.00 -79.00   0.50    1.00    --  -42.26-138.00-120.00   60
 17  ω   -109.00 -79.00   0.50    1.00    --  -42.26-138.00-180.00   60
 18  ω    -28.00  28.00   0.50    1.00    --  -42.26  21.00 -90.00  112
 19  ω   -109.00 -27.00   0.50    1.00    --  -42.26 -43.00 -60.00  164
 20  ω   -109.00 -79.00   0.50    1.00    --  -42.26-138.00   0.00   60
 21  ω     97.00 162.00   0.50    3.00    --   93.72  68.00 120.00  130
 22  ω     76.00 160.00   0.50    3.00    --   93.72  50.00-180.00  168
 23  ω     25.00 105.00   0.50    3.00    --   93.72 -77.00  30.00  160
 24  ω     28.00  57.00   0.50    3.00    --   93.72 -50.00 120.00   58
 25  ω     83.00 160.00   0.50    3.00    --   93.72  33.00  30.00  154
 26  ω     97.00 162.00   0.50    3.00    --   93.72  68.00 -90.00  130
 27  ω     83.00 162.00   0.50    3.00    --   93.72  25.00  60.00  158
 28  ω     26.00  83.00   0.50    3.00    --   93.72 -68.00 -60.00  114
 29  ω     28.00  57.00   0.50    3.00    --   93.72 -50.00  60.00   58
 30  ω     26.00 120.00   0.50    3.00    --   93.72 -79.00 117.00  188
 31  ω     83.00 160.00   0.50    3.00    --   93.72  33.00 -30.00  154
 32  ω     78.00 162.00   0.50    3.00    --   93.72  79.00-117.00  168
 33  ω     76.00 160.00   0.50    3.00    --   93.72  50.00   0.00  168
 34  ω     97.00 162.00   0.50    3.00    --   93.72  68.00-180.00  130
 35  ω     76.00 160.00   0.50    3.00    --   93.72  50.00-120.00  168
 36  ω     28.00  57.00   0.50    3.00    --   93.72 -50.00 150.00   58
 37  ω     26.00  83.00   0.50    3.00    --   93.72 -68.00 -90.00  114
 38  ω   -127.00 -27.00   0.50    3.00    --  -94.03 145.00  90.00  200
 39  ω    -68.00 -27.00   0.50    3.00    --  -94.03  59.00-150.00   82
 40  ω    -57.00 -28.00   0.50    3.00    --  -94.03  50.00-150.00   58
 41  ω   -162.00-101.00   0.50    3.00    --  -94.03 -77.00  90.00  122
 42  ω    -57.00 -28.00   0.50    3.00    --  -94.03  50.00 -30.00   58
 43  ω   -163.00-101.00   0.50    3.00    --  -94.03 -87.00   0.00  124
 44  ω   -109.00 -32.00   0.50    3.00    --  -94.03 117.00-180.00  154
 45  ω   -163.00 -83.00   0.50    3.00    --  -94.03 -25.00-180.00  160
 46  ω   -160.00 -87.00   0.50    3.00    --  -94.03 -59.00  30.00  146
 47  ω   -161.00 -97.00   0.50    3.00    --  -94.03 -68.00-180.00  128
 48  ω    -57.00 -28.00   0.50    3.00    --  -94.03  50.00  30.00   58
 49  ω    -57.00 -28.00   0.50    3.00    --  -94.03  50.00   0.00   58
 50  ω   -106.00 -23.00   0.50    3.00    --  -94.03  96.00-180.00  166
 51  ω   -160.00 -77.00   0.50    3.00    --  -94.03 -50.00 -30.00  166
 52  ω   -109.00 -32.00   0.50    3.00    --  -94.03 117.00-120.00  154
 53  ω   -160.00 -87.00   0.50    3.00    --  -94.03 -59.00   0.00  146
 54  ω   -127.00 -27.00   0.50    3.00    --  -94.03 145.00   0.00  200
 55  ω    -15.00  72.00   0.50    1.00    --   41.95 -89.00 -30.00  174
 56  ω     23.00 108.00   0.50    1.00    --   41.95  54.00-150.00  170
 57  ω     23.00 108.00   0.50    1.00    --   41.95  54.00 -60.00  170
 58  ω     23.00 108.00   0.50    1.00    --   41.95  54.00 -90.00  170
 59  ω     23.00 108.00   0.50    1.00    --   41.95  54.00  90.00  170
 60  ω     23.00 108.00   0.50    1.00    --   41.95  54.00 120.00  170
 61  ω     23.00 108.00   0.50    1.00    --   41.95  54.00  60.00  170
 62  ω     23.00 108.00   0.50    1.00    --   41.95  54.00 150.00  170
 63  ω   -108.00 -24.00   0.50    1.00    --  -42.26 -54.00-180.00  168
 64  ω   -108.00 -24.00   0.50    1.00    --  -42.26 -54.00  60.00  168
 65  ω   -108.00 -24.00   0.50    1.00    --  -42.26 -54.00 -60.00  168
 66  ω   -108.00 -24.00   0.50    1.00    --  -42.26 -54.00  90.00  168
 67  ω   -108.00 -24.00   0.50    1.00    --  -42.26 -54.00 -30.00  168
 68  ω   -108.00 -24.00   0.50    1.00    --  -42.26 -54.00 -90.00  168
 69  ω   -108.00 -24.00   0.50    1.00    --  -42.26 -54.00 150.00  168
 70  ω   -108.00 -24.00   0.50    1.00    --  -42.26 -54.00-150.00  168
 71  ω   -108.00 -24.00   0.50    1.00    --  -42.26 -54.00 120.00  168
 72  ω   -108.00 -24.00   0.50    1.00    --  -42.26 -54.00-120.00  168
 73  ω     76.00 137.00   0.50    3.00    --   93.72  50.00  90.00  122
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at home/near, HyPix3000'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0008991000
_diffrn_orient_matrix_UB_12      -0.1701014000
_diffrn_orient_matrix_UB_13      -0.0497205000
_diffrn_orient_matrix_UB_21      0.1019175000
_diffrn_orient_matrix_UB_22      0.0002362000
_diffrn_orient_matrix_UB_23      0.0077655000
_diffrn_orient_matrix_UB_31      0.0015627000
_diffrn_orient_matrix_UB_32      -0.1056443000
_diffrn_orient_matrix_UB_33      0.0801927000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3215
_reflns_number_total             3459
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.65
_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 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.407
_refine_diff_density_min         -0.556
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       0.000082(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         3459
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0186
_refine_ls_R_factor_gt           0.0167
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0138P)²+2.2856P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0389
_refine_ls_wR_factor_ref         0.0395
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C8(H8), C13(H13), C14(H14), C15(H15), C16(H16)
2.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C19(H19A,H19B,H19C)
;
_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
Ta1 Ta 0.47271(2) 0.34431(2) 0.27750(2) 0.01480(5) Uani 1 1 d . . . . .
Cl1 Cl 0.13407(5) 0.17622(9) 0.51784(4) 0.02765(15) Uani 1 1 d . . . . .
O1 O 0.44811(11) 0.4486(2) 0.38329(11) 0.0205(4) Uani 1 1 d . . . . .
O2 O 0.43995(11) 0.2314(2) 0.17040(11) 0.0177(4) Uani 1 1 d . . . . .
O3 O 0.45217(11) 0.5735(2) 0.22010(11) 0.0170(4) Uani 1 1 d . . . . .
O4 O 0.59403(11) 0.4294(2) 0.26983(11) 0.0205(4) Uani 1 1 d . . . . .
O5 O 0.51660(12) 0.1397(2) 0.32553(11) 0.0207(4) Uani 1 1 d . . . . .
N1 N 0.32717(13) 0.3242(3) 0.28007(13) 0.0143(4) Uani 1 1 d . . . . .
C1 C 0.37389(17) 0.4002(3) 0.41696(16) 0.0187(5) Uani 1 1 d . . . . .
C2 C 0.36593(18) 0.4120(3) 0.50029(16) 0.0207(6) Uani 1 1 d . . . . .
H2 H 0.411580 0.464223 0.536060 0.025 Uiso 1 1 calc R U . . .
C3 C 0.29069(18) 0.3470(3) 0.53125(17) 0.0218(6) Uani 1 1 d . . . . .
H3 H 0.284151 0.354712 0.588282 0.026 Uiso 1 1 calc R U . . .
C4 C 0.22495(17) 0.2702(3) 0.47757(16) 0.0202(6) Uani 1 1 d . . . . .
C5 C 0.23066(16) 0.2603(3) 0.39363(16) 0.0170(5) Uani 1 1 d . . . . .
H5 H 0.185106 0.206996 0.358173 0.020 Uiso 1 1 calc R U . . .
C6 C 0.30509(16) 0.3308(3) 0.36270(15) 0.0151(5) Uani 1 1 d . . . . .
C7 C 0.26760(16) 0.3352(3) 0.21458(16) 0.0145(5) Uani 1 1 d . . . . .
C8 C 0.29095(17) 0.3018(3) 0.13406(16) 0.0178(5) Uani 1 1 d . . . . .
H8 H 0.246462 0.320333 0.089788 0.021 Uiso 1 1 calc R U . . .
C9 C 0.37118(17) 0.2456(3) 0.11463(15) 0.0182(5) Uani 1 1 d . . . . .
C10 C 0.17269(16) 0.3813(3) 0.22053(16) 0.0184(5) Uani 1 1 d . . . . .
H10A H 0.138025 0.274686 0.224441 0.028 Uiso 1 1 calc R U . . .
H10B H 0.149743 0.446531 0.171500 0.028 Uiso 1 1 calc R U . . .
H10C H 0.168151 0.452687 0.269527 0.028 Uiso 1 1 calc R U . . .
C11 C 0.38841(19) 0.1944(4) 0.02988(16) 0.0243(6) Uani 1 1 d . . . . .
H11A H 0.431011 0.275284 0.009459 0.036 Uiso 1 1 calc R U . . .
H11B H 0.332919 0.198040 -0.006289 0.036 Uiso 1 1 calc R U . . .
H11C H 0.412650 0.076350 0.030699 0.036 Uiso 1 1 calc R U . . .
C12 C 0.52457(16) 0.6682(3) 0.20607(16) 0.0165(5) Uani 1 1 d . . . . .
C13 C 0.52361(18) 0.8310(3) 0.17061(16) 0.0198(6) Uani 1 1 d . . . . .
H13 H 0.469168 0.887520 0.153819 0.024 Uiso 1 1 calc R U . . .
C14 C 0.60392(18) 0.9108(4) 0.15988(16) 0.0221(6) Uani 1 1 d . . . . .
H14 H 0.604555 1.023739 0.136494 0.027 Uiso 1 1 calc R U . . .
C15 C 0.68313(18) 0.8256(4) 0.18332(17) 0.0230(6) Uani 1 1 d . . . . .
H15 H 0.737438 0.879708 0.173912 0.028 Uiso 1 1 calc R U . . .
C16 C 0.68442(18) 0.6629(4) 0.22025(17) 0.0239(6) Uani 1 1 d . . . . .
H16 H 0.738793 0.605592 0.236533 0.029 Uiso 1 1 calc R U . . .
C17 C 0.60442(17) 0.5866(3) 0.23265(16) 0.0188(5) Uani 1 1 d . . . . .
C18 C 0.5737(2) 0.0203(4) 0.37069(17) 0.0297(7) Uani 1 1 d . . . . .
H18A H 0.623063 -0.010483 0.338283 0.036 Uiso 1 1 calc R U . . .
H18B H 0.540576 -0.087404 0.380343 0.036 Uiso 1 1 calc R U . . .
C19 C 0.6098(3) 0.0949(5) 0.4506(2) 0.0581(12) Uani 1 1 d . . . . .
H19A H 0.648914 0.192503 0.441125 0.087 Uiso 1 1 calc R U . . .
H19B H 0.643341 0.005533 0.483145 0.087 Uiso 1 1 calc R U . . .
H19C H 0.560978 0.135874 0.480494 0.087 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
Ta1 O1 1.9770(18) . ?
Ta1 O2 1.9737(17) . ?
Ta1 O3 2.0077(17) . ?
Ta1 O4 1.9711(17) . ?
Ta1 O5 1.8529(18) . ?
Ta1 N1 2.220(2) . ?
Cl1 C4 1.745(3) . ?
O1 C1 1.356(3) . ?
O2 C9 1.320(3) . ?
O3 C12 1.357(3) . ?
O4 C17 1.370(3) . ?
O5 C18 1.419(3) . ?
N1 C6 1.426(3) . ?
N1 C7 1.333(3) . ?
C1 C2 1.383(4) . ?
C1 C6 1.406(4) . ?
C2 C3 1.389(4) . ?
C3 C4 1.393(4) . ?
C4 C5 1.387(4) . ?
C5 C6 1.394(4) . ?
C7 C8 1.422(4) . ?
C7 C10 1.497(3) . ?
C8 C9 1.360(4) . ?
C9 C11 1.490(4) . ?
C12 C13 1.380(4) . ?
C12 C17 1.395(4) . ?
C13 C14 1.392(4) . ?
C14 C15 1.389(4) . ?
C15 C16 1.390(4) . ?
C16 C17 1.382(4) . ?
C18 C19 1.482(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 Ta1 O3 91.06(7) . . ?
O1 Ta1 N1 74.65(7) . . ?
O2 Ta1 O1 154.51(7) . . ?
O2 Ta1 O3 87.60(7) . . ?
O2 Ta1 N1 79.86(7) . . ?
O3 Ta1 N1 87.82(7) . . ?
O4 Ta1 O1 100.44(7) . . ?
O4 Ta1 O2 104.08(7) . . ?
O4 Ta1 O3 77.31(7) . . ?
O4 Ta1 N1 164.34(7) . . ?
O5 Ta1 O1 93.75(8) . . ?
O5 Ta1 O2 92.88(7) . . ?
O5 Ta1 O3 167.65(7) . . ?
O5 Ta1 O4 90.62(8) . . ?
O5 Ta1 N1 104.42(8) . . ?
C1 O1 Ta1 118.83(15) . . ?
C9 O2 Ta1 133.47(16) . . ?
C12 O3 Ta1 117.40(15) . . ?
C17 O4 Ta1 118.15(15) . . ?
C18 O5 Ta1 161.07(18) . . ?
C6 N1 Ta1 110.19(15) . . ?
C7 N1 Ta1 125.21(17) . . ?
C7 N1 C6 123.6(2) . . ?
O1 C1 C2 122.8(2) . . ?
O1 C1 C6 116.3(2) . . ?
C2 C1 C6 120.9(2) . . ?
C1 C2 C3 119.5(2) . . ?
C2 C3 C4 119.1(2) . . ?
C3 C4 Cl1 118.8(2) . . ?
C5 C4 Cl1 118.8(2) . . ?
C5 C4 C3 122.4(2) . . ?
C4 C5 C6 118.2(2) . . ?
C1 C6 N1 112.4(2) . . ?
C5 C6 N1 127.4(2) . . ?
C5 C6 C1 119.8(2) . . ?
N1 C7 C8 121.4(2) . . ?
N1 C7 C10 122.9(2) . . ?
C8 C7 C10 115.8(2) . . ?
C9 C8 C7 125.9(2) . . ?
O2 C9 C8 122.0(2) . . ?
O2 C9 C11 114.9(2) . . ?
C8 C9 C11 123.2(2) . . ?
O3 C12 C13 125.7(2) . . ?
O3 C12 C17 113.5(2) . . ?
C13 C12 C17 120.8(2) . . ?
C12 C13 C14 118.8(3) . . ?
C15 C14 C13 120.1(3) . . ?
C14 C15 C16 121.3(3) . . ?
C17 C16 C15 118.2(3) . . ?
O4 C17 C12 113.6(2) . . ?
O4 C17 C16 125.6(2) . . ?
C16 C17 C12 120.8(3) . . ?
O5 C18 C19 111.2(2) . . ?

_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 1.358
_oxdiff_exptl_absorpt_empirical_full_min 0.679


_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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_I-2
_database_code_depnum_ccdc_archive 'CCDC 2331118'
loop_
_audit_author_name
_audit_author_address
'Christopher Durr'
;Amherst College
United States of America
;
_audit_update_record             
;
2024-02-05 deposited with the CCDC.	2024-03-19 downloaded from the CCDC.
;
_audit_creation_date             2022-05-02
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C18 H28 N O5 Ta'
_chemical_formula_sum            'C18 H28 N O5 Ta'
_chemical_formula_weight         519.36
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Ta O N C H'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ta Ta -5.7959 5.2718 '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           9
_space_group_name_H-M_alt        'C 1 c 1'
_space_group_name_Hall           'C -2yc'
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'

_cell_length_a                   30.4758(4)
_cell_length_b                   8.11590(10)
_cell_length_c                   16.0060(3)
_cell_angle_alpha                90
_cell_angle_beta                 98.4290(10)
_cell_angle_gamma                90
_cell_volume                     3916.14(10)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    25075
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      67.8310
_cell_measurement_theta_min      2.9130
_shelx_estimated_absorpt_T_max   0.512
_shelx_estimated_absorpt_T_min   0.242
_exptl_absorpt_coefficient_mu    10.588
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50974
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.110a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.762
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2048
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
9 -2 8 0.0464
18 0 -5 0.0893
-1 2 -10 0.0212
-18 0 6 0.0766
4 2 9 0.0389
-1 -5 -2 0.0308
-5 0 -10 0.0401
-1 5 -2 0.0315

_exptl_crystal_size_max          0.187
_exptl_crystal_size_mid          0.096
_exptl_crystal_size_min          0.073
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
8.5778 -1.8589 7.8577 -0.2128 0.0022 0.9771
18.3827 -0.2967 -5.1697 -0.9953 0.0251 -0.0938
-1.3808 1.6950 -9.5962 -0.1699 0.0073 -0.9854
-17.9349 0.1786 5.7053 0.9872 -0.0251 0.1573
4.4932 2.0051 8.8538 0.0516 -0.6736 0.7373
-0.6628 -5.1914 -1.6963 -0.0790 0.9813 0.1753
-4.9451 0.1271 -9.5583 -0.0228 0.3209 -0.9468
-1.2311 5.1559 -1.9712 0.0691 -0.8433 -0.5330

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0651
_diffrn_reflns_av_unetI/netI     0.0430
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            35982
_diffrn_reflns_point_group_measured_fraction_full 0.904
_diffrn_reflns_point_group_measured_fraction_max 0.893
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.387
_diffrn_reflns_theta_min         2.932
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -30.00  74.00   0.50    0.20    --   41.95 -96.00-140.00  208
  2  ω    -75.00  30.00   0.50    0.20    --  -42.26  96.00 -31.00  210
  3  ω     22.00 106.00   0.50    0.60    --   93.72 -96.00-140.00  168
  4  ω   -166.00 -83.00   0.50    0.60    --  -94.03 -96.00-140.00  166
  5  ω     22.00  56.00   0.50    0.20    --   41.95  58.00-137.86   68
  6  ω    -24.00  37.00   0.50    0.20    --   41.95 -32.00-180.00  122
  7  ω    -24.00  37.00   0.50    0.20    --   41.95 -32.00 -60.00  122
  8  ω    -28.00  28.00   0.50    0.20    --   41.95 -21.00-120.00  112
  9  ω    -23.00  48.00   0.50    0.20    --   41.95 -43.00-120.00  142
 10  ω     21.00  48.00   0.50    0.20    --   41.95  61.00 107.89   54
 11  ω     23.00  66.00   0.50    0.20    --   41.95  56.00  71.49   86
 12  ω    -28.00  28.00   0.50    0.20    --   41.95 -21.00   0.00  112
 13  ω     22.00  50.00   0.50    0.20    --   41.95  60.00 150.30   56
 14  ω    -48.00  24.00   0.50    0.20    --  -42.26  43.00  60.00  144
 15  ω   -100.00 -19.00   0.50    0.20    --  -42.26 138.00 120.00  162
 16  ω   -108.00 -24.00   0.50    0.20    --  -42.26 -54.00  30.00  168
 17  ω    -24.00  32.00   0.50    0.20    --  -42.26  11.00-180.00  112
 18  ω   -109.00 -79.00   0.50    0.20    --  -42.26-138.00   0.00   60
 19  ω    -60.00 -23.00   0.50    0.20    --  -42.26 -57.00  65.97   74
 20  ω    -53.00 -22.00   0.50    0.20    --  -42.26 -59.00-140.66   62
 21  ω   -109.00 -79.00   0.50    0.20    --  -42.26-138.00 -30.00   60
 22  ω    -53.00 -22.00   0.50    0.20    --  -42.26 -59.00 -94.14   62
 23  ω    -53.00 -22.00   0.50    0.20    --  -42.26 -59.00-170.19   62
 24  ω    -37.00  24.00   0.50    0.20    --  -42.26  32.00 120.00  122
 25  ω    -24.00  32.00   0.50    0.20    --  -42.26  11.00 -90.00  112
 26  ω     28.00  57.00   0.50    0.60    --   93.72 -50.00  90.00   58
 27  ω     28.00 109.00   0.50    0.60    --   93.72-117.00 -30.00  162
 28  ω     28.00 109.00   0.50    0.60    --   93.72-117.00  60.00  162
 29  ω     79.00 160.00   0.50    0.60    --   93.72  42.00 -60.00  162
 30  ω     92.00 159.00   0.50    0.60    --   93.72 117.00 -60.00  134
 31  ω     79.00 160.00   0.50    0.60    --   93.72  42.00 -90.00  162
 32  ω     28.00  57.00   0.50    0.60    --   93.72 -50.00-180.00   58
 33  ω     27.00 127.00   0.50    0.60    --   93.72-145.00 -90.00  200
 34  ω     26.00  83.00   0.50    0.60    --   93.72 -68.00-120.00  114
 35  ω     28.00 109.00   0.50    0.60    --   93.72-117.00  30.00  162
 36  ω     28.00 109.00   0.50    0.60    --   93.72-117.00-180.00  162
 37  ω     28.00  57.00   0.50    0.60    --   93.72 -50.00  60.00   58
 38  ω     84.00 166.00   0.50    0.60    --   93.72  96.00 -31.00  164
 39  ω     26.00  83.00   0.50    0.60    --   93.72 -68.00   0.00  114
 40  ω    -57.00 -28.00   0.50    0.60    --  -94.03  50.00-120.00   58
 41  ω   -160.00 -77.00   0.50    0.60    --  -94.03 -50.00 150.00  166
 42  ω   -162.00-101.00   0.50    0.60    --  -94.03 -77.00  30.00  122
 43  ω   -159.00 -92.00   0.50    0.60    --  -94.03-117.00 -90.00  134
 44  ω   -160.00 -83.00   0.50    0.60    --  -94.03 -33.00  90.00  154
 45  ω    -68.00 -27.00   0.50    0.60    --  -94.03  59.00 120.00   82
 46  ω   -160.00 -83.00   0.50    0.60    --  -94.03 -33.00  60.00  154
 47  ω   -109.00 -29.00   0.50    0.60    --  -94.03 117.00-150.00  160
 48  ω   -160.00 -77.00   0.50    0.60    --  -94.03 -50.00-120.00  166
 49  ω   -162.00-101.00   0.50    0.60    --  -94.03 -77.00-180.00  122
 50  ω   -160.00 -77.00   0.50    0.60    --  -94.03 -50.00 120.00  166
 51  ω    -57.00 -28.00   0.50    0.60    --  -94.03  50.00 -30.00   58
 52  ω    -83.00 -26.00   0.50    0.60    --  -94.03  68.00 -30.00  114
 53  ω   -161.00 -97.00   0.50    0.60    --  -94.03 -68.00  90.00  128
 54  ω   -105.00 -25.00   0.50    0.60    --  -94.03  77.00-120.00  160
 55  ω    -57.00 -28.00   0.50    0.60    --  -94.03  50.00 -60.00   58
 56  ω   -106.00 -22.00   0.50    0.60    --  -94.03  96.00 -31.00  168
 57  ω     21.00  48.00   0.50    0.20    --   41.95  61.00  28.62   54
 58  ω     22.00  56.00   0.50    0.20    --   41.95  58.00 174.84   68
 59  ω     21.00  48.00   0.50    0.20    --   41.95  61.00  83.34   54
 60  ω     27.00 108.00   0.50    0.20    --   41.95  43.00 120.00  162
 61  ω     22.00  50.00   0.50    0.20    --   41.95  60.00-171.12   56
 62  ω     21.00  48.00   0.50    0.20    --   41.95  61.00-132.68   54
 63  ω     31.00 108.00   0.50    0.20    --   41.95  32.00 -90.00  154
 64  ω     23.00  66.00   0.50    0.20    --   41.95  56.00-107.21   86
 65  ω    -56.00 -22.00   0.50    0.20    --  -42.26 -58.00 174.35   68
 66  ω    -48.00 -22.00   0.50    0.20    --  -42.26 -61.00 -34.90   52
 67  ω   -109.00 -31.00   0.50    0.20    --  -42.26 -32.00 -30.00  156
 68  ω    -48.00 -22.00   0.50    0.20    --  -42.26 -61.00 -76.14   52
 69  ω    -53.00 -22.00   0.50    0.20    --  -42.26 -59.00 -57.64   62
 70  ω    -60.00 -23.00   0.50    0.20    --  -42.26 -57.00-115.49   74
 71  ω   -109.00 -27.00   0.50    0.20    --  -42.26 -43.00 -60.00  164
 72  ω    -79.00   4.00   0.50    0.20    --  -42.26 104.00 120.00  166
 73  ω   -109.00 -24.00   0.50    0.20    --  -42.26 -53.00 164.36  170
 74  ω    -60.00 -23.00   0.50    0.20    --  -42.26 -57.00 108.18   74
 75  ω     76.00 160.00   0.50    0.60    --   93.72  50.00 -30.00  168
 76  ω     87.00 161.00   0.50    0.60    --   93.72  59.00-150.00  148
 77  ω   -160.00 -75.00   0.50    0.60    --  -94.03 -55.00  74.76  170
 78  ω   -160.00 -75.00   0.50    0.60    --  -94.03 -54.00  -0.46  170
 79  ω   -160.00 -75.00   0.50    0.60    --  -94.03 -56.00-172.41  170
 80  ω   -161.00 -75.00   0.50    0.60    --  -94.03-145.00 -30.00  172
 81  ω   -160.00 -77.00   0.50    0.60    --  -94.03 -50.00  30.00  166
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at home/near, HyPix3000'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0464630000
_diffrn_orient_matrix_UB_12      0.0124645000
_diffrn_orient_matrix_UB_13      0.0265898000
_diffrn_orient_matrix_UB_21      -0.0101350000
_diffrn_orient_matrix_UB_22      -0.1777100000
_diffrn_orient_matrix_UB_23      -0.0306941000
_diffrn_orient_matrix_UB_31      0.0187367000
_diffrn_orient_matrix_UB_32      -0.0650766000
_diffrn_orient_matrix_UB_33      0.0884997000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.805
_reflns_Friedel_fraction_full    0.808
_reflns_Friedel_fraction_max     0.797
_reflns_number_gt                6186
_reflns_number_total             6422
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.65
_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 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         1.226
_refine_diff_density_min         -0.721
_refine_diff_density_rms         0.117
_refine_ls_abs_structure_details 
;
 Flack x determined using 2592 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.047(11)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         6422
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0325
_refine_ls_restrained_S_all      1.107
_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)+(0.0436P)²+16.3483P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0831
_refine_ls_wR_factor_ref         0.0852
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C15(H15A,H15B), C17(H17A,H17B), C31(H31A,H31B), C33(H33A,
 H33B), C35(H35A,H35B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C9(H9), C20(H20), C21(H21), C23(H23), C27(H27)
2.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,
 H14C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C25(H25A,H25B,H25C), C29(H29A,
 H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C),
 C36(H36A,H36B,H36C)
;
_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
Ta1 Ta 0.36656(2) 0.49197(5) 0.48865(2) 0.02423(13) Uani 1 1 d . . . . .
O1 O 0.4137(2) 0.4794(8) 0.5884(5) 0.0286(17) Uani 1 1 d . . . . .
O2 O 0.3166(2) 0.4100(9) 0.4040(5) 0.0288(16) Uani 1 1 d . . . . .
O3 O 0.3243(2) 0.5369(9) 0.5632(5) 0.0304(17) Uani 1 1 d . . . . .
O4 O 0.3719(2) 0.7120(9) 0.4541(5) 0.0283(16) Uani 1 1 d . . . . .
O5 O 0.4072(2) 0.4105(9) 0.4187(5) 0.0277(16) Uani 1 1 d . . . . .
N1 N 0.3648(3) 0.2266(10) 0.5335(6) 0.0272(19) Uani 1 1 d . . . . .
C1 C 0.4305(4) 0.3299(12) 0.6149(7) 0.027(2) Uani 1 1 d . . . . .
C2 C 0.4711(4) 0.3140(15) 0.6650(8) 0.033(3) Uani 1 1 d . . . . .
H2 H 0.487362 0.409154 0.685502 0.040 Uiso 1 1 calc R U . . .
C3 C 0.4879(4) 0.1582(14) 0.6852(8) 0.035(3) Uani 1 1 d . . . . .
H3 H 0.515534 0.147534 0.721034 0.042 Uiso 1 1 calc R U . . .
C4 C 0.4656(4) 0.0185(13) 0.6544(8) 0.032(2) Uani 1 1 d . . . . .
C5 C 0.4244(4) 0.0354(14) 0.6040(7) 0.029(2) Uani 1 1 d . . . . .
H5 H 0.408744 -0.059668 0.581330 0.035 Uiso 1 1 calc R U . . .
C6 C 0.4063(4) 0.1901(13) 0.5869(7) 0.027(2) Uani 1 1 d . . . . .
C7 C 0.4854(4) -0.1516(14) 0.6734(8) 0.035(3) Uani 1 1 d . . . . .
H7A H 0.513611 -0.159905 0.651003 0.052 Uiso 1 1 calc R U . . .
H7B H 0.464837 -0.235469 0.646859 0.052 Uiso 1 1 calc R U . . .
H7C H 0.490680 -0.169069 0.734657 0.052 Uiso 1 1 calc R U . . .
C8 C 0.3293(4) 0.1341(13) 0.5266(7) 0.029(2) Uani 1 1 d . . . . .
C9 C 0.2910(4) 0.1713(13) 0.4668(8) 0.030(2) Uani 1 1 d . . . . .
H9 H 0.266105 0.100798 0.467214 0.036 Uiso 1 1 calc R U . . .
C10 C 0.2859(4) 0.2974(13) 0.4089(8) 0.028(2) Uani 1 1 d . . . . .
C11 C 0.3254(4) -0.0213(12) 0.5768(8) 0.029(2) Uani 1 1 d . . . . .
H11A H 0.336168 -0.115215 0.547141 0.043 Uiso 1 1 calc R U . . .
H11B H 0.294205 -0.039310 0.583062 0.043 Uiso 1 1 calc R U . . .
H11C H 0.343108 -0.010322 0.632727 0.043 Uiso 1 1 calc R U . . .
C12 C 0.2459(4) 0.3160(14) 0.3445(8) 0.035(3) Uani 1 1 d . . . . .
H12A H 0.233331 0.426228 0.348874 0.052 Uiso 1 1 calc R U . . .
H12B H 0.223891 0.232781 0.353943 0.052 Uiso 1 1 calc R U . . .
H12C H 0.254175 0.301368 0.288006 0.052 Uiso 1 1 calc R U . . .
C13 C 0.3100(4) 0.4920(17) 0.6392(8) 0.042(3) Uani 1 1 d . . . . .
H13A H 0.321884 0.571699 0.683618 0.050 Uiso 1 1 calc R U . . .
H13B H 0.322167 0.382023 0.656474 0.050 Uiso 1 1 calc R U . . .
C14 C 0.2607(4) 0.4868(16) 0.6329(9) 0.043(3) Uani 1 1 d . . . . .
H14A H 0.248722 0.406654 0.589653 0.065 Uiso 1 1 calc R U . . .
H14B H 0.248462 0.596098 0.617316 0.065 Uiso 1 1 calc R U . . .
H14C H 0.252471 0.454242 0.687470 0.065 Uiso 1 1 calc R U . . .
C15 C 0.3896(4) 0.8271(12) 0.4015(8) 0.033(3) Uani 1 1 d . . . . .
H15A H 0.420963 0.849020 0.424526 0.039 Uiso 1 1 calc R U . . .
H15B H 0.373068 0.932158 0.401682 0.039 Uiso 1 1 calc R U . . .
C16 C 0.3868(5) 0.7658(17) 0.3121(9) 0.046(3) Uani 1 1 d . . . . .
H16A H 0.401259 0.844969 0.278806 0.069 Uiso 1 1 calc R U . . .
H16B H 0.355588 0.753646 0.287349 0.069 Uiso 1 1 calc R U . . .
H16C H 0.401719 0.658864 0.311966 0.069 Uiso 1 1 calc R U . . .
C17 C 0.4242(4) 0.2758(13) 0.3772(7) 0.031(2) Uani 1 1 d . . . . .
H17A H 0.425130 0.176572 0.413348 0.037 Uiso 1 1 calc R U . . .
H17B H 0.454872 0.300649 0.367526 0.037 Uiso 1 1 calc R U . . .
C18 C 0.3957(4) 0.2421(17) 0.2938(9) 0.041(3) Uani 1 1 d . . . . .
H18A H 0.397200 0.336195 0.255923 0.061 Uiso 1 1 calc R U . . .
H18B H 0.364919 0.225287 0.302927 0.061 Uiso 1 1 calc R U . . .
H18C H 0.406447 0.142986 0.268286 0.061 Uiso 1 1 calc R U . . .
Ta2 Ta 0.62663(2) 0.33975(5) 0.54346(3) 0.02511(13) Uani 1 1 d . . . . .
O6 O 0.6794(2) 0.2315(9) 0.5119(5) 0.0274(16) Uani 1 1 d . . . . .
O7 O 0.5721(3) 0.4886(9) 0.5255(5) 0.0307(17) Uani 1 1 d . . . . .
O8 O 0.6552(2) 0.5414(9) 0.5783(5) 0.0305(16) Uani 1 1 d . . . . .
O9 O 0.6357(2) 0.2573(9) 0.6569(5) 0.0318(17) Uani 1 1 d . . . . .
O10 O 0.5855(3) 0.1673(9) 0.5093(5) 0.0312(17) Uani 1 1 d . . . . .
N2 N 0.6264(3) 0.4014(10) 0.4041(5) 0.0231(17) Uani 1 1 d . . . . .
C19 C 0.6961(3) 0.2727(13) 0.4410(7) 0.028(2) Uani 1 1 d . . . . .
C20 C 0.7382(3) 0.2285(12) 0.4284(7) 0.029(2) Uani 1 1 d . . . . .
H20 H 0.756006 0.161854 0.468706 0.034 Uiso 1 1 calc R U . . .
C21 C 0.7545(4) 0.2816(14) 0.3565(8) 0.033(2) Uani 1 1 d . . . . .
H21 H 0.783436 0.249039 0.347766 0.040 Uiso 1 1 calc R U . . .
C22 C 0.7293(4) 0.3819(13) 0.2967(7) 0.030(2) Uani 1 1 d . . . . .
C23 C 0.6864(3) 0.4240(12) 0.3091(7) 0.025(2) Uani 1 1 d . . . . .
H23 H 0.668706 0.491402 0.268831 0.030 Uiso 1 1 calc R U . . .
C24 C 0.6690(3) 0.3679(12) 0.3803(7) 0.023(2) Uani 1 1 d . . . . .
C25 C 0.7486(4) 0.4488(16) 0.2234(8) 0.036(3) Uani 1 1 d . . . . .
H25A H 0.775691 0.510528 0.243909 0.054 Uiso 1 1 calc R U . . .
H25B H 0.727083 0.522277 0.190598 0.054 Uiso 1 1 calc R U . . .
H25C H 0.755737 0.357725 0.187534 0.054 Uiso 1 1 calc R U . . .
C26 C 0.5906(3) 0.4345(11) 0.3501(6) 0.022(2) Uani 1 1 d . . . . .
C27 C 0.5508(4) 0.4896(12) 0.3776(8) 0.026(2) Uani 1 1 d . . . . .
H27 H 0.526377 0.507823 0.334493 0.032 Uiso 1 1 calc R U . . .
C28 C 0.5435(4) 0.5195(12) 0.4584(8) 0.027(2) Uani 1 1 d . . . . .
C29 C 0.5884(4) 0.4166(13) 0.2561(7) 0.027(2) Uani 1 1 d . . . . .
H29A H 0.597292 0.520335 0.232133 0.041 Uiso 1 1 calc R U . . .
H29B H 0.557919 0.389513 0.231009 0.041 Uiso 1 1 calc R U . . .
H29C H 0.608370 0.328228 0.243756 0.041 Uiso 1 1 calc R U . . .
C30 C 0.5020(3) 0.6024(14) 0.4775(8) 0.034(3) Uani 1 1 d . . . . .
H30A H 0.488332 0.534862 0.517366 0.050 Uiso 1 1 calc R U . . .
H30B H 0.481211 0.615476 0.425123 0.050 Uiso 1 1 calc R U . . .
H30C H 0.509494 0.710959 0.502408 0.050 Uiso 1 1 calc R U . . .
C31 C 0.6498(4) 0.7156(12) 0.5815(8) 0.033(2) Uani 1 1 d . . . . .
H31A H 0.671251 0.762053 0.627939 0.040 Uiso 1 1 calc R U . . .
H31B H 0.619470 0.742104 0.592747 0.040 Uiso 1 1 calc R U . . .
C32 C 0.6573(5) 0.7909(15) 0.4981(9) 0.043(3) Uani 1 1 d . . . . .
H32A H 0.636858 0.741109 0.452097 0.064 Uiso 1 1 calc R U . . .
H32B H 0.687957 0.770428 0.489007 0.064 Uiso 1 1 calc R U . . .
H32C H 0.652037 0.909956 0.499340 0.064 Uiso 1 1 calc R U . . .
C33 C 0.6338(4) 0.0945(13) 0.6911(7) 0.035(3) Uani 1 1 d . . . . .
H33A H 0.662517 0.037974 0.690203 0.042 Uiso 1 1 calc R U . . .
H33B H 0.610414 0.030066 0.655989 0.042 Uiso 1 1 calc R U . . .
C34 C 0.6241(4) 0.1028(18) 0.7787(9) 0.041(3) Uani 1 1 d . . . . .
H34A H 0.595363 0.156576 0.779303 0.061 Uiso 1 1 calc R U . . .
H34B H 0.647354 0.166212 0.813402 0.061 Uiso 1 1 calc R U . . .
H34C H 0.623148 -0.008992 0.801553 0.061 Uiso 1 1 calc R U . . .
C35 C 0.5415(4) 0.1105(14) 0.4917(8) 0.033(2) Uani 1 1 d . . . . .
H35A H 0.520985 0.205107 0.491250 0.040 Uiso 1 1 calc R U . . .
H35B H 0.535563 0.034065 0.536913 0.040 Uiso 1 1 calc R U . . .
C36 C 0.5328(4) 0.0236(15) 0.4083(9) 0.040(3) Uani 1 1 d . . . . .
H36A H 0.538335 0.099260 0.363234 0.060 Uiso 1 1 calc R U . . .
H36B H 0.501850 -0.013244 0.397999 0.060 Uiso 1 1 calc R U . . .
H36C H 0.552500 -0.071962 0.408989 0.060 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
Ta1 O1 1.988(8) . ?
Ta1 O2 1.997(8) . ?
Ta1 O3 1.915(8) . ?
Ta1 O4 1.883(7) . ?
Ta1 O5 1.906(7) . ?
Ta1 N1 2.273(8) . ?
O1 C1 1.361(12) . ?
O2 C10 1.320(13) . ?
O3 C13 1.399(15) . ?
O4 C15 1.416(13) . ?
O5 C17 1.417(12) . ?
N1 C6 1.448(14) . ?
N1 C8 1.309(14) . ?
C1 C2 1.376(17) . ?
C1 C6 1.393(15) . ?
C2 C3 1.386(17) . ?
C3 C4 1.376(17) . ?
C4 C5 1.398(17) . ?
C4 C7 1.519(15) . ?
C5 C6 1.383(15) . ?
C8 C9 1.431(17) . ?
C8 C11 1.509(14) . ?
C9 C10 1.374(17) . ?
C10 C12 1.484(17) . ?
C13 C14 1.492(18) . ?
C15 C16 1.506(18) . ?
C17 C18 1.507(17) . ?
Ta2 O6 1.963(7) . ?
Ta2 O7 2.040(7) . ?
Ta2 O8 1.898(8) . ?
Ta2 O9 1.917(8) . ?
Ta2 O10 1.905(8) . ?
Ta2 N2 2.284(8) . ?
O6 C19 1.352(13) . ?
O7 C28 1.305(14) . ?
O8 C31 1.425(12) . ?
O9 C33 1.435(13) . ?
O10 C35 1.406(13) . ?
N2 C24 1.432(12) . ?
N2 C26 1.316(13) . ?
C19 C20 1.373(14) . ?
C19 C24 1.411(15) . ?
C20 C21 1.387(16) . ?
C21 C22 1.398(16) . ?
C22 C23 1.394(15) . ?
C22 C25 1.489(16) . ?
C23 C24 1.401(14) . ?
C26 C27 1.421(14) . ?
C26 C29 1.503(15) . ?
C27 C28 1.367(17) . ?
C28 C30 1.502(15) . ?
C31 C32 1.516(17) . ?
C33 C34 1.476(17) . ?
C35 C36 1.499(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 Ta1 O2 156.5(3) . . ?
O1 Ta1 N1 75.2(3) . . ?
O2 Ta1 N1 81.3(3) . . ?
O3 Ta1 O1 89.0(3) . . ?
O3 Ta1 O2 88.3(3) . . ?
O3 Ta1 N1 86.3(3) . . ?
O4 Ta1 O1 101.6(3) . . ?
O4 Ta1 O2 101.9(3) . . ?
O4 Ta1 O3 95.6(3) . . ?
O4 Ta1 O5 93.7(3) . . ?
O4 Ta1 N1 176.4(3) . . ?
O5 Ta1 O1 89.9(3) . . ?
O5 Ta1 O2 89.0(3) . . ?
O5 Ta1 O3 170.7(3) . . ?
O5 Ta1 N1 84.5(3) . . ?
C1 O1 Ta1 119.4(7) . . ?
C10 O2 Ta1 131.8(7) . . ?
C13 O3 Ta1 144.6(8) . . ?
C15 O4 Ta1 148.9(7) . . ?
C17 O5 Ta1 149.0(7) . . ?
C6 N1 Ta1 108.8(6) . . ?
C8 N1 Ta1 125.0(7) . . ?
C8 N1 C6 124.8(9) . . ?
O1 C1 C2 122.1(10) . . ?
O1 C1 C6 117.9(10) . . ?
C2 C1 C6 120.0(10) . . ?
C1 C2 C3 119.5(11) . . ?
C4 C3 C2 121.4(12) . . ?
C3 C4 C5 118.8(11) . . ?
C3 C4 C7 121.0(12) . . ?
C5 C4 C7 120.2(10) . . ?
C6 C5 C4 120.2(10) . . ?
C1 C6 N1 113.6(9) . . ?
C5 C6 N1 126.2(10) . . ?
C5 C6 C1 119.9(10) . . ?
N1 C8 C9 121.3(10) . . ?
N1 C8 C11 124.4(10) . . ?
C9 C8 C11 114.3(10) . . ?
C10 C9 C8 127.5(10) . . ?
O2 C10 C9 123.1(11) . . ?
O2 C10 C12 113.9(10) . . ?
C9 C10 C12 123.0(10) . . ?
O3 C13 C14 112.8(11) . . ?
O4 C15 C16 112.0(9) . . ?
O5 C17 C18 110.7(9) . . ?
O6 Ta2 O7 155.5(3) . . ?
O6 Ta2 N2 74.5(3) . . ?
O7 Ta2 N2 81.2(3) . . ?
O8 Ta2 O6 96.0(3) . . ?
O8 Ta2 O7 81.9(3) . . ?
O8 Ta2 O9 91.5(3) . . ?
O8 Ta2 O10 166.3(3) . . ?
O8 Ta2 N2 91.9(3) . . ?
O9 Ta2 O6 94.4(3) . . ?
O9 Ta2 O7 110.0(3) . . ?
O9 Ta2 N2 168.7(3) . . ?
O10 Ta2 O6 97.3(3) . . ?
O10 Ta2 O7 84.6(3) . . ?
O10 Ta2 O9 90.7(3) . . ?
O10 Ta2 N2 88.5(3) . . ?
C19 O6 Ta2 121.9(6) . . ?
C28 O7 Ta2 131.5(7) . . ?
C31 O8 Ta2 144.6(7) . . ?
C33 O9 Ta2 132.4(7) . . ?
C35 O10 Ta2 150.1(7) . . ?
C24 N2 Ta2 110.2(6) . . ?
C26 N2 Ta2 124.7(6) . . ?
C26 N2 C24 124.0(9) . . ?
O6 C19 C20 122.3(10) . . ?
O6 C19 C24 117.3(9) . . ?
C20 C19 C24 120.4(10) . . ?
C19 C20 C21 119.8(10) . . ?
C20 C21 C22 121.4(10) . . ?
C21 C22 C25 120.7(10) . . ?
C23 C22 C21 118.5(10) . . ?
C23 C22 C25 120.7(10) . . ?
C22 C23 C24 120.7(10) . . ?
C19 C24 N2 112.5(9) . . ?
C23 C24 N2 128.3(9) . . ?
C23 C24 C19 119.0(9) . . ?
N2 C26 C27 121.5(10) . . ?
N2 C26 C29 123.4(9) . . ?
C27 C26 C29 115.1(9) . . ?
C28 C27 C26 127.9(11) . . ?
O7 C28 C27 124.2(10) . . ?
O7 C28 C30 113.6(10) . . ?
C27 C28 C30 122.1(11) . . ?
O8 C31 C32 109.6(9) . . ?
O9 C33 C34 110.2(10) . . ?
O10 C35 C36 111.9(9) . . ?

_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 1.911
_oxdiff_exptl_absorpt_empirical_full_min 0.577
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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_I-3
_database_code_depnum_ccdc_archive 'CCDC 2331119'
loop_
_audit_author_name
_audit_author_address
'Christopher Durr'
;Amherst College
United States of America
;
_audit_update_record             
;
2024-02-05 deposited with the CCDC.	2024-03-19 downloaded from the CCDC.
;
_audit_creation_date             2022-05-16
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C17 H25 Cl N Nb O5'
_chemical_formula_sum            'C17 H25 Cl N Nb O5'
_chemical_formula_weight         451.74
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H Nb O N Cl'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -0.1121 2.4826 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   13.4876(2)
_cell_length_b                   13.0436(2)
_cell_length_c                   22.1841(3)
_cell_angle_alpha                90
_cell_angle_beta                 94.0660(10)
_cell_angle_gamma                90
_cell_volume                     3892.96(10)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    16623
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      67.9320
_cell_measurement_theta_min      3.8950
_shelx_estimated_absorpt_T_max   0.695
_shelx_estimated_absorpt_T_min   0.403
_exptl_absorpt_coefficient_mu    6.530
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63420
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.110a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1856
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 8 -5 0.0374
0 -2 14 0.0057
0 0 -14 0.0464
1 8 2 0.0189
9 0 -4 0.0606
-1 -8 -2 0.1159
-8 2 4 0.0810

_exptl_crystal_size_max          0.175
_exptl_crystal_size_mid          0.145
_exptl_crystal_size_min          0.056
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.7391 7.9145 -5.0275 0.0372 -0.4977 0.8665
-0.2406 -1.5108 14.1661 -0.0797 0.9968 -0.0091
0.0895 -0.2125 -14.3783 0.0788 -0.9776 -0.1950
0.7642 8.3102 2.2954 -0.0077 -0.0056 1.0000
8.5759 -0.4618 -3.7836 -0.9584 -0.2852 -0.0090
-1.4623 -8.2447 -1.9786 0.0860 0.0289 -0.9959
-8.2815 2.0086 4.1463 0.9401 0.2791 0.1960

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_av_unetI/netI     0.0414
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            29938
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.350
_diffrn_reflns_theta_min         3.722
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     19.00 115.00   0.50    1.00    --   41.95  15.00-154.00  192
  2  ω    -31.00  24.00   0.50    1.00    --   41.95 -15.00  35.00  110
  3  ω     70.00 167.00   0.50    5.00    --   93.72  15.00-154.00  194
  4  ω   -167.00 -73.00   0.50    5.00    --  -94.03 -15.00  35.00  188
  5  ω    -28.00  28.00   0.50    1.00    --   41.95 -21.00-120.00  112
  6  ω     19.00  99.00   0.50    1.00    --   41.95-138.00 -30.00  160
  7  ω     23.00 108.00   0.50    1.00    --   41.95  54.00-150.00  170
  8  ω   -109.00 -79.00   0.50    1.00    --  -42.26-138.00 150.00   60
  9  ω    -28.00  28.00   0.50    1.00    --  -42.26  21.00   0.00  112
 10  ω   -109.00 -79.00   0.50    1.00    --  -42.26-138.00 -90.00   60
 11  ω   -109.00 -79.00   0.50    1.00    --  -42.26-138.00 -30.00   60
 12  ω    -24.00  31.00   0.50    1.00    --  -42.26  15.00-154.00  110
 13  ω   -109.00 -79.00   0.50    1.00    --  -42.26-138.00-120.00   60
 14  ω    -79.00   4.00   0.50    1.00    --  -42.26 104.00-180.00  166
 15  ω   -115.00 -21.00   0.50    1.00    --  -42.26 -15.00  35.00  188
 16  ω   -109.00 -79.00   0.50    1.00    --  -42.26-138.00-180.00   60
 17  ω     28.00  57.00   0.50    5.00    --   93.72 -50.00 -60.00   58
 18  ω     28.00  57.00   0.50    5.00    --   93.72 -50.00-120.00   58
 19  ω   -160.00 -87.00   0.50    5.00    --  -94.03 -59.00   0.00  146
 20  ω    -68.00 -27.00   0.50    5.00    --  -94.03  59.00   0.00   82
 21  ω    -57.00 -28.00   0.50    5.00    --  -94.03  50.00-180.00   58
 22  ω   -109.00 -29.00   0.50    5.00    --  -94.03 117.00 -90.00  160
 23  ω   -109.00 -29.00   0.50    5.00    --  -94.03 117.00-150.00  160
 24  ω   -161.00 -97.00   0.50    5.00    --  -94.03 -68.00 -30.00  128
 25  ω    -68.00 -27.00   0.50    5.00    --  -94.03  59.00-150.00   82
 26  ω   -161.00 -97.00   0.50    5.00    --  -94.03 -68.00 -60.00  128
 27  ω    -57.00 -28.00   0.50    5.00    --  -94.03  50.00  90.00   58
 28  ω    -57.00 -28.00   0.50    5.00    --  -94.03  50.00  30.00   58
 29  ω    -57.00 -28.00   0.50    5.00    --  -94.03  50.00-120.00   58
 30  ω    -68.00 -27.00   0.50    5.00    --  -94.03  59.00 120.00   82
 31  ω    -57.00 -28.00   0.50    5.00    --  -94.03  50.00 -30.00   58
 32  ω   -160.00 -83.00   0.50    5.00    --  -94.03 -33.00   0.00  154
 33  ω   -106.00 -22.00   0.50    5.00    --  -94.03  96.00  90.00  168
 34  ω   -161.00 -99.00   0.50    5.00    --  -94.03 -68.00  90.00  124
 35  ω   -102.00 -37.00   0.50    5.00    --  -94.03  96.00-150.00  130
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at home/near, HyPix3000'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1139528000
_diffrn_orient_matrix_UB_12      0.0113036000
_diffrn_orient_matrix_UB_13      -0.0063551000
_diffrn_orient_matrix_UB_21      -0.0041742000
_diffrn_orient_matrix_UB_22      -0.0191448000
_diffrn_orient_matrix_UB_23      0.0682508000
_diffrn_orient_matrix_UB_31      0.0104536000
_diffrn_orient_matrix_UB_32      0.1160769000
_diffrn_orient_matrix_UB_33      0.0119116000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6137
_reflns_number_total             7048
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.65
_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 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.639
_refine_diff_density_min         -0.911
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       0.00012(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         7048
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0298
_refine_ls_restrained_S_all      1.075
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0386P)²+0.9597P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0776
_refine_ls_wR_factor_ref         0.0804
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C14(H14A,H14B), C16(H16A,H16B), C29(H29A,H29B), C31(H31A,
 H31B), C33(H33A,H33B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C8(H8), C19(H19), C20(H20), C22(H22), C25(H25)
2.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C15(H15A,H15B,
 H15C), C17(H17A,H17B,H17C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C30(H30A,
 H30B,H30C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C)
;
_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
Nb1 Nb 0.67496(2) 0.60537(2) 0.64476(2) 0.01407(8) Uani 1 1 d . . . . .
Cl1 Cl 0.84220(5) 0.58239(6) 0.95103(3) 0.03137(16) Uani 1 1 d . . . . .
O1 O 0.60886(12) 0.62511(13) 0.72081(7) 0.0171(3) Uani 1 1 d . . . . .
O2 O 0.78177(12) 0.55443(13) 0.59258(7) 0.0189(4) Uani 1 1 d . . . . .
O3 O 0.76377(12) 0.71810(13) 0.65887(7) 0.0188(3) Uani 1 1 d . . . . .
O4 O 0.58590(12) 0.68852(12) 0.59576(8) 0.0194(4) Uani 1 1 d . . . . .
O5 O 0.61305(12) 0.47950(12) 0.62582(7) 0.0184(3) Uani 1 1 d . . . . .
N1 N 0.77576(14) 0.52672(15) 0.71831(9) 0.0160(4) Uani 1 1 d . . . . .
C1 C 0.65763(18) 0.60997(17) 0.77497(11) 0.0163(5) Uani 1 1 d . . . . .
C2 C 0.61972(18) 0.64439(19) 0.82780(11) 0.0200(5) Uani 1 1 d . . . . .
H2 H 0.555490 0.674550 0.826510 0.024 Uiso 1 1 calc R U . . .
C3 C 0.67543(19) 0.6349(2) 0.88265(11) 0.0215(5) Uani 1 1 d . . . . .
H3 H 0.650024 0.658310 0.919051 0.026 Uiso 1 1 calc R U . . .
C4 C 0.76900(19) 0.5904(2) 0.88314(11) 0.0217(5) Uani 1 1 d . . . . .
C5 C 0.80669(18) 0.55292(18) 0.83128(11) 0.0190(5) Uani 1 1 d . . . . .
H5 H 0.870825 0.522478 0.833198 0.023 Uiso 1 1 calc R U . . .
C6 C 0.75095(17) 0.55964(18) 0.77612(11) 0.0165(5) Uani 1 1 d . . . . .
C7 C 0.83993(17) 0.45205(18) 0.70929(11) 0.0163(5) Uani 1 1 d . . . . .
C8 C 0.86937(17) 0.42799(18) 0.65062(11) 0.0182(5) Uani 1 1 d . . . . .
H8 H 0.911835 0.370278 0.648062 0.022 Uiso 1 1 calc R U . . .
C9 C 0.84423(17) 0.47738(18) 0.59768(11) 0.0175(5) Uani 1 1 d . . . . .
C10 C 0.88603(19) 0.38549(19) 0.75897(11) 0.0206(5) Uani 1 1 d . . . . .
H10A H 0.946272 0.418556 0.777022 0.031 Uiso 1 1 calc R U . . .
H10B H 0.903244 0.318751 0.742312 0.031 Uiso 1 1 calc R U . . .
H10C H 0.838642 0.375746 0.789986 0.031 Uiso 1 1 calc R U . . .
C11 C 0.88688(19) 0.4470(2) 0.53957(11) 0.0236(5) Uani 1 1 d . . . . .
H11A H 0.837705 0.406824 0.514994 0.035 Uiso 1 1 calc R U . . .
H11B H 0.946796 0.405639 0.548446 0.035 Uiso 1 1 calc R U . . .
H11C H 0.903966 0.508713 0.517335 0.035 Uiso 1 1 calc R U . . .
C12 C 0.86677(18) 0.7381(2) 0.66030(14) 0.0278(6) Uani 1 1 d . . . . .
H12A H 0.894969 0.705493 0.625028 0.033 Uiso 1 1 calc R U . . .
H12B H 0.900186 0.708299 0.697430 0.033 Uiso 1 1 calc R U . . .
C13 C 0.8854(2) 0.8523(2) 0.65907(16) 0.0363(7) Uani 1 1 d . . . . .
H13A H 0.846710 0.882776 0.624556 0.054 Uiso 1 1 calc R U . . .
H13B H 0.956338 0.865042 0.655265 0.054 Uiso 1 1 calc R U . . .
H13C H 0.865397 0.883191 0.696605 0.054 Uiso 1 1 calc R U . . .
C14 C 0.58492(19) 0.79342(18) 0.57739(11) 0.0200(5) Uani 1 1 d . . . . .
H14A H 0.647288 0.827113 0.593046 0.024 Uiso 1 1 calc R U . . .
H14B H 0.528659 0.829264 0.594540 0.024 Uiso 1 1 calc R U . . .
C15 C 0.5749(2) 0.8013(2) 0.50981(12) 0.0300(6) Uani 1 1 d . . . . .
H15A H 0.630806 0.766060 0.492904 0.045 Uiso 1 1 calc R U . . .
H15B H 0.574879 0.873608 0.497906 0.045 Uiso 1 1 calc R U . . .
H15C H 0.512398 0.769213 0.494435 0.045 Uiso 1 1 calc R U . . .
C16 C 0.6091(2) 0.37333(19) 0.61303(12) 0.0249(6) Uani 1 1 d . . . . .
H16A H 0.669170 0.352973 0.592773 0.030 Uiso 1 1 calc R U . . .
H16B H 0.550246 0.358500 0.585185 0.030 Uiso 1 1 calc R U . . .
C17 C 0.6032(2) 0.3121(2) 0.67016(15) 0.0351(7) Uani 1 1 d . . . . .
H17A H 0.591392 0.239787 0.659929 0.053 Uiso 1 1 calc R U . . .
H17B H 0.548522 0.337932 0.692693 0.053 Uiso 1 1 calc R U . . .
H17C H 0.665896 0.318554 0.695041 0.053 Uiso 1 1 calc R U . . .
Nb2 Nb 0.17479(2) 0.30967(2) 0.64008(2) 0.01546(8) Uani 1 1 d . . . . .
Cl2 Cl 0.34698(5) 0.30764(5) 0.94571(3) 0.02991(16) Uani 1 1 d . . . . .
O6 O 0.10936(12) 0.28436(13) 0.71595(7) 0.0181(3) Uani 1 1 d . . . . .
O7 O 0.28154(12) 0.36376(13) 0.58909(7) 0.0191(4) Uani 1 1 d . . . . .
O8 O 0.26118(12) 0.19422(12) 0.65087(8) 0.0189(4) Uani 1 1 d . . . . .
O9 O 0.08399(12) 0.23322(14) 0.58837(8) 0.0242(4) Uani 1 1 d . . . . .
O10 O 0.11424(12) 0.43824(13) 0.62728(7) 0.0193(4) Uani 1 1 d . . . . .
N2 N 0.27746(14) 0.38197(15) 0.71555(9) 0.0156(4) Uani 1 1 d . . . . .
C18 C 0.15764(18) 0.29736(17) 0.77061(11) 0.0171(5) Uani 1 1 d . . . . .
C19 C 0.11899(19) 0.26232(19) 0.82331(12) 0.0212(5) Uani 1 1 d . . . . .
H19 H 0.053703 0.234663 0.821829 0.025 Uiso 1 1 calc R U . . .
C20 C 0.17553(19) 0.26757(19) 0.87827(11) 0.0213(5) Uani 1 1 d . . . . .
H20 H 0.149619 0.243964 0.914491 0.026 Uiso 1 1 calc R U . . .
C21 C 0.2706(2) 0.30811(19) 0.87871(12) 0.0219(5) Uani 1 1 d . . . . .
C22 C 0.30895(18) 0.34801(19) 0.82754(11) 0.0195(5) Uani 1 1 d . . . . .
H22 H 0.373951 0.376439 0.829698 0.023 Uiso 1 1 calc R U . . .
C23 C 0.25148(17) 0.34623(18) 0.77266(11) 0.0168(5) Uani 1 1 d . . . . .
C24 C 0.34079(17) 0.45788(18) 0.70843(11) 0.0172(5) Uani 1 1 d . . . . .
C25 C 0.36855(17) 0.48707(18) 0.64998(11) 0.0182(5) Uani 1 1 d . . . . .
H25 H 0.410820 0.545184 0.648754 0.022 Uiso 1 1 calc R U . . .
C26 C 0.34233(17) 0.44250(18) 0.59590(11) 0.0174(5) Uani 1 1 d . . . . .
C27 C 0.38546(18) 0.52265(19) 0.75979(11) 0.0199(5) Uani 1 1 d . . . . .
H27A H 0.338236 0.528132 0.791231 0.030 Uiso 1 1 calc R U . . .
H27B H 0.400153 0.591235 0.744733 0.030 Uiso 1 1 calc R U . . .
H27C H 0.447003 0.490659 0.776748 0.030 Uiso 1 1 calc R U . . .
C28 C 0.38126(18) 0.4812(2) 0.53826(11) 0.0213(5) Uani 1 1 d . . . . .
H28A H 0.410815 0.424176 0.517005 0.032 Uiso 1 1 calc R U . . .
H28B H 0.431836 0.533805 0.547687 0.032 Uiso 1 1 calc R U . . .
H28C H 0.326494 0.510704 0.512515 0.032 Uiso 1 1 calc R U . . .
C29 C 0.36320(18) 0.1689(2) 0.65087(12) 0.0210(5) Uani 1 1 d . . . . .
H29A H 0.395999 0.180937 0.691596 0.025 Uiso 1 1 calc R U . . .
H29B H 0.395430 0.213516 0.621908 0.025 Uiso 1 1 calc R U . . .
C30 C 0.3758(2) 0.0578(2) 0.63342(13) 0.0296(6) Uani 1 1 d . . . . .
H30A H 0.340049 0.045019 0.594142 0.044 Uiso 1 1 calc R U . . .
H30B H 0.349065 0.013536 0.664039 0.044 Uiso 1 1 calc R U . . .
H30C H 0.446620 0.042921 0.630758 0.044 Uiso 1 1 calc R U . . .
C31 C 0.0846(2) 0.1299(2) 0.56632(14) 0.0306(6) Uani 1 1 d . . . . .
H31A H 0.016591 0.101193 0.565537 0.037 Uiso 1 1 calc R U . . .
H31B H 0.128408 0.087360 0.593896 0.037 Uiso 1 1 calc R U . . .
C32 C 0.1206(3) 0.1264(3) 0.50421(15) 0.0450(8) Uani 1 1 d . . . . .
H32A H 0.077397 0.168726 0.476961 0.067 Uiso 1 1 calc R U . . .
H32B H 0.119365 0.055432 0.489671 0.067 Uiso 1 1 calc R U . . .
H32C H 0.188791 0.152730 0.505254 0.067 Uiso 1 1 calc R U . . .
C33 C 0.10914(19) 0.54647(19) 0.62664(11) 0.0212(5) Uani 1 1 d . . . . .
H33A H 0.050027 0.568620 0.600928 0.025 Uiso 1 1 calc R U . . .
H33B H 0.168900 0.574611 0.609108 0.025 Uiso 1 1 calc R U . . .
C34 C 0.1027(2) 0.5880(2) 0.69006(12) 0.0246(6) Uani 1 1 d . . . . .
H34A H 0.091975 0.662244 0.688264 0.037 Uiso 1 1 calc R U . . .
H34B H 0.164847 0.573311 0.714137 0.037 Uiso 1 1 calc R U . . .
H34C H 0.047201 0.555183 0.708788 0.037 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
Nb1 O1 1.9802(16) . ?
Nb1 O2 2.0232(16) . ?
Nb1 O3 1.9082(17) . ?
Nb1 O4 1.9014(17) . ?
Nb1 O5 1.8761(16) . ?
Nb1 N1 2.2909(19) . ?
Cl1 C4 1.744(3) . ?
O1 C1 1.343(3) . ?
O2 C9 1.311(3) . ?
O3 C12 1.412(3) . ?
O4 C14 1.427(3) . ?
O5 C16 1.414(3) . ?
N1 C6 1.415(3) . ?
N1 C7 1.328(3) . ?
C1 C2 1.386(3) . ?
C1 C6 1.418(3) . ?
C2 C3 1.390(4) . ?
C3 C4 1.388(4) . ?
C4 C5 1.380(3) . ?
C5 C6 1.393(3) . ?
C7 C8 1.422(3) . ?
C7 C10 1.503(3) . ?
C8 C9 1.361(4) . ?
C9 C11 1.502(3) . ?
C12 C13 1.511(4) . ?
C14 C15 1.499(4) . ?
C16 C17 1.505(4) . ?
Nb2 O6 1.9828(16) . ?
Nb2 O7 2.0202(16) . ?
Nb2 O8 1.9087(16) . ?
Nb2 O9 1.9002(17) . ?
Nb2 O10 1.8781(17) . ?
Nb2 N2 2.298(2) . ?
Cl2 C21 1.748(3) . ?
O6 C18 1.346(3) . ?
O7 C26 1.316(3) . ?
O8 C29 1.415(3) . ?
O9 C31 1.434(3) . ?
O10 C33 1.413(3) . ?
N2 C23 1.417(3) . ?
N2 C24 1.324(3) . ?
C18 C19 1.391(3) . ?
C18 C23 1.415(3) . ?
C19 C20 1.393(4) . ?
C20 C21 1.386(4) . ?
C21 C22 1.382(4) . ?
C22 C23 1.396(3) . ?
C24 C25 1.427(3) . ?
C24 C27 1.509(3) . ?
C25 C26 1.357(4) . ?
C26 C28 1.503(3) . ?
C29 C30 1.512(4) . ?
C31 C32 1.494(4) . ?
C33 C34 1.516(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 Nb1 O2 155.79(7) . . ?
O1 Nb1 N1 74.44(7) . . ?
O2 Nb1 N1 81.36(7) . . ?
O3 Nb1 O1 94.32(7) . . ?
O3 Nb1 O2 83.27(7) . . ?
O3 Nb1 N1 83.93(7) . . ?
O4 Nb1 O1 96.23(7) . . ?
O4 Nb1 O2 107.87(7) . . ?
O4 Nb1 O3 91.03(7) . . ?
O4 Nb1 N1 168.96(7) . . ?
O5 Nb1 O1 94.84(7) . . ?
O5 Nb1 O2 84.73(7) . . ?
O5 Nb1 O3 167.23(7) . . ?
O5 Nb1 O4 96.78(7) . . ?
O5 Nb1 N1 89.99(7) . . ?
C1 O1 Nb1 121.44(14) . . ?
C9 O2 Nb1 132.97(15) . . ?
C12 O3 Nb1 138.71(15) . . ?
C14 O4 Nb1 134.64(15) . . ?
C16 O5 Nb1 155.77(16) . . ?
C6 N1 Nb1 110.07(14) . . ?
C7 N1 Nb1 125.56(16) . . ?
C7 N1 C6 123.9(2) . . ?
O1 C1 C2 121.5(2) . . ?
O1 C1 C6 117.5(2) . . ?
C2 C1 C6 121.0(2) . . ?
C1 C2 C3 120.2(2) . . ?
C4 C3 C2 118.6(2) . . ?
C3 C4 Cl1 119.36(19) . . ?
C5 C4 Cl1 118.6(2) . . ?
C5 C4 C3 122.0(2) . . ?
C4 C5 C6 120.2(2) . . ?
N1 C6 C1 113.0(2) . . ?
C5 C6 N1 129.0(2) . . ?
C5 C6 C1 117.9(2) . . ?
N1 C7 C8 121.8(2) . . ?
N1 C7 C10 123.6(2) . . ?
C8 C7 C10 114.6(2) . . ?
C9 C8 C7 128.1(2) . . ?
O2 C9 C8 123.8(2) . . ?
O2 C9 C11 114.3(2) . . ?
C8 C9 C11 121.9(2) . . ?
O3 C12 C13 110.3(2) . . ?
O4 C14 C15 110.4(2) . . ?
O5 C16 C17 110.8(2) . . ?
O6 Nb2 O7 155.67(7) . . ?
O6 Nb2 N2 74.42(7) . . ?
O7 Nb2 N2 81.25(7) . . ?
O8 Nb2 O6 93.82(7) . . ?
O8 Nb2 O7 83.84(7) . . ?
O8 Nb2 N2 84.34(7) . . ?
O9 Nb2 O6 96.80(7) . . ?
O9 Nb2 O7 107.44(7) . . ?
O9 Nb2 O8 91.34(7) . . ?
O9 Nb2 N2 169.87(7) . . ?
O10 Nb2 O6 93.56(7) . . ?
O10 Nb2 O7 85.59(7) . . ?
O10 Nb2 O8 168.10(7) . . ?
O10 Nb2 O9 97.04(7) . . ?
O10 Nb2 N2 88.67(7) . . ?
C18 O6 Nb2 121.85(14) . . ?
C26 O7 Nb2 132.17(15) . . ?
C29 O8 Nb2 140.28(15) . . ?
C31 O9 Nb2 132.85(17) . . ?
C33 O10 Nb2 156.03(16) . . ?
C23 N2 Nb2 109.99(14) . . ?
C24 N2 Nb2 125.48(16) . . ?
C24 N2 C23 123.7(2) . . ?
O6 C18 C19 122.0(2) . . ?
O6 C18 C23 117.4(2) . . ?
C19 C18 C23 120.6(2) . . ?
C18 C19 C20 120.3(2) . . ?
C21 C20 C19 118.3(2) . . ?
C20 C21 Cl2 119.6(2) . . ?
C22 C21 Cl2 117.8(2) . . ?
C22 C21 C20 122.5(2) . . ?
C21 C22 C23 119.5(2) . . ?
C18 C23 N2 113.4(2) . . ?
C22 C23 N2 128.1(2) . . ?
C22 C23 C18 118.4(2) . . ?
N2 C24 C25 121.4(2) . . ?
N2 C24 C27 123.7(2) . . ?
C25 C24 C27 114.9(2) . . ?
C26 C25 C24 128.3(2) . . ?
O7 C26 C25 123.8(2) . . ?
O7 C26 C28 114.6(2) . . ?
C25 C26 C28 121.6(2) . . ?
O8 C29 C30 110.5(2) . . ?
O9 C31 C32 110.7(3) . . ?
O10 C33 C34 110.7(2) . . ?

_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 2.858
_oxdiff_exptl_absorpt_empirical_full_min 0.315
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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_C-1tBu
_database_code_depnum_ccdc_archive 'CCDC 2331121'
loop_
_audit_author_name
_audit_author_address
'Christopher Durr'
;Amherst College
United States of America
;
_audit_update_record             
;
2024-02-05 deposited with the CCDC.	2024-03-19 downloaded from the CCDC.
;
_audit_creation_date             2023-12-07
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H30 N Nb O5'
_chemical_formula_sum            'C24 H30 N Nb O5'
_chemical_formula_weight         505.40
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Ta Cl O N C H'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -0.1121 2.4826 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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        'I 1 2/a 1'
_space_group_name_Hall           '-I 2ya'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   20.5797(4)
_cell_length_b                   7.4688(2)
_cell_length_c                   31.9583(9)
_cell_angle_alpha                90
_cell_angle_beta                 108.275(3)
_cell_angle_gamma                90
_cell_volume                     4664.4(2)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    5427
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      67.8100
_cell_measurement_theta_min      2.8920
_shelx_estimated_absorpt_T_max   0.797
_shelx_estimated_absorpt_T_min   0.648
_exptl_absorpt_coefficient_mu    4.488
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87081
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.93a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2096
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-5 4 0 0.0230
-6 -4 -1 0.0027
0 1 -20 0.0120
13 2 -5 0.0581
-12 -1 -2 0.0019
3 1 -20 0.0134
-11 -2 13 0.0027
4 0 17 0.0474

_exptl_crystal_size_max          0.106
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.053
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-5.2482 4.3994 -0.3348 0.9710 0.1817 0.1552
-6.0710 -4.2103 -0.9497 -0.6890 -0.1263 0.7136
0.3228 0.5679 -19.7103 0.0228 0.9513 0.3075
12.6031 1.5955 -5.1132 0.0108 0.3172 -0.9483
-11.8518 -1.3285 -1.5747 -0.0028 0.0092 1.0000
2.5716 0.8431 -20.2707 0.0243 0.9909 0.1324
-11.4146 -1.6759 13.2066 -0.0196 -0.7003 0.7135
3.6784 -0.0361 17.1461 -0.0183 -0.8053 -0.5926

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0609
_diffrn_reflns_av_unetI/netI     0.0602
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            15375
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.982
_diffrn_reflns_theta_min         2.912
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -4.00  79.00   0.50   10.00    --   41.95-104.00 -39.00  166
  2  ω    -79.00   4.00   0.50   10.00    --  -42.26 104.00  61.00  166
  3  ω     24.00 108.00   0.50   30.00    --   93.72-104.00 -39.00  168
  4  ω     83.00 163.00   0.50   30.00    --   93.72 104.00  61.00  160
  5  ω   -164.00 -83.00   0.50   30.00    --  -94.03-104.00 -39.00  162
  6  ω   -107.00 -24.00   0.50   30.00    --  -94.03 104.00  61.00  166
  7  ω    -24.00  37.00   0.50   10.00    --   41.95 -32.00 -90.00  122
  8  ω    -28.00  28.00   0.50   10.00    --   41.95 -21.00 -30.00  112
  9  ω    -33.00  24.00   0.50   10.00    --   41.95 -11.00  30.00  114
 10  ω    -48.00  24.00   0.50   10.00    --  -42.26  43.00 120.00  144
 11  ω   -109.00 -79.00   0.50   10.00    --  -42.26-138.00  90.00   60
 12  ω   -109.00 -79.00   0.50   10.00    --  -42.26-138.00 -60.00   60
 13  ω   -109.00 -79.00   0.50   10.00    --  -42.26-138.00  60.00   60
 14  ω    -28.00  28.00   0.50   10.00    --  -42.26  21.00-180.00  112
 15  ω    -48.00  24.00   0.50   10.00    --  -42.26  43.00 -60.00  144
 16  ω    -28.00  28.00   0.50   10.00    --  -42.26  21.00  60.00  112
 17  ω     28.00  57.00   0.50   30.00    --   93.72 -50.00 -30.00   58
 18  ω    101.00 162.00   0.50   30.00    --   93.72  77.00  30.00  122
 19  ω    101.00 162.00   0.50   30.00    --   93.72  77.00 -60.00  122
 20  ω     28.00  57.00   0.50   30.00    --   93.72 -50.00   0.00   58
 21  ω     28.00  57.00   0.50   30.00    --   93.72 -50.00 -60.00   58
 22  ω     26.00  83.00   0.50   30.00    --   93.72 -68.00 -60.00  114
 23  ω   -159.00 -92.00   0.50   30.00    --  -94.03-117.00 -60.00  134
 24  ω    -83.00 -26.00   0.50   30.00    --  -94.03  68.00  60.00  114
 25  ω   -109.00 -29.00   0.50   30.00    --  -94.03 117.00 -30.00  160
 26  ω   -153.00 -99.00   0.50   30.00    --  -94.03 -96.00 -60.00  108
 27  ω   -153.00-102.00   0.50   30.00    --  -94.03 -68.00-150.00  102
 28  ω   -129.00 -97.00   0.50   30.00    --  -94.03-117.00-150.00   64
 29  ω   -162.00-102.00   0.50   30.00    --  -94.03 -77.00  30.00  120
 30  ω   -108.00 -34.00   0.50   30.00    --  -94.03 117.00  90.00  148
 31  ω    -57.00 -28.00   0.50   30.00    --  -94.03  50.00 -60.00   58
 32  ω   -123.00 -84.00   0.50   30.00    --  -94.03 -25.00   0.00   78
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at home/near, HyPix3000'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0221262000
_diffrn_orient_matrix_UB_12      0.1946331000
_diffrn_orient_matrix_UB_13      0.0040902000
_diffrn_orient_matrix_UB_21      0.0011054000
_diffrn_orient_matrix_UB_22      0.0390420000
_diffrn_orient_matrix_UB_23      -0.0471194000
_diffrn_orient_matrix_UB_31      -0.0756061000
_diffrn_orient_matrix_UB_32      -0.0563145000
_diffrn_orient_matrix_UB_33      -0.0184633000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3329
_reflns_number_total             4223
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.65
_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 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         3.166
_refine_diff_density_min         -1.037
_refine_diff_density_rms         0.137
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         4223
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0799
_refine_ls_R_factor_gt           0.0631
_refine_ls_restrained_S_all      1.010
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1241P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1602
_refine_ls_wR_factor_ref         0.1723
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C9(H9), C14(H14), C16(H16), C17(H17)
2.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C20(H20A,H20B,
 H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C)
;
_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
Nb1 Nb 0.57573(2) 0.08892(6) 0.66930(2) 0.02761(19) Uani 1 1 d . . . . .
O1 O 0.64396(16) 0.2057(5) 0.71959(12) 0.0315(8) Uani 1 1 d . . . . .
O2 O 0.48554(17) -0.0214(5) 0.63895(13) 0.0329(8) Uani 1 1 d . . . . .
O3 O 0.61372(18) 0.1749(6) 0.62281(13) 0.0365(9) Uani 1 1 d . . . . .
O4 O 0.52821(17) 0.3246(5) 0.65191(13) 0.0344(8) Uani 1 1 d . . . . .
O5 O 0.62359(17) -0.1228(5) 0.67430(13) 0.0328(9) Uani 1 1 d . . . . .
N1 N 0.5336(2) 0.0659(6) 0.72563(14) 0.0252(9) Uani 1 1 d . . . . .
C1 C 0.6476(2) 0.1564(7) 0.76103(19) 0.0300(11) Uani 1 1 d . . . . .
C2 C 0.7061(3) 0.1754(7) 0.79649(19) 0.0312(12) Uani 1 1 d . . . . .
H2 H 0.745446 0.232240 0.793055 0.037 Uiso 1 1 calc R U . . .
C3 C 0.7068(3) 0.1099(8) 0.8374(2) 0.0345(13) Uani 1 1 d . . . . .
H3 H 0.746899 0.124285 0.861926 0.041 Uiso 1 1 calc R U . . .
C4 C 0.6505(3) 0.0241(8) 0.84327(19) 0.0309(12) Uani 1 1 d . . . . .
C5 C 0.5908(2) 0.0086(7) 0.80733(18) 0.0288(11) Uani 1 1 d . . . . .
H5 H 0.551841 -0.049987 0.810874 0.035 Uiso 1 1 calc R U . . .
C6 C 0.5880(2) 0.0785(7) 0.76641(17) 0.0252(10) Uani 1 1 d . . . . .
C7 C 0.6542(3) -0.0595(8) 0.88682(19) 0.0346(12) Uani 1 1 d . . . . .
H7A H 0.607765 -0.083201 0.887657 0.052 Uiso 1 1 calc R U . . .
H7B H 0.677434 0.022568 0.910766 0.052 Uiso 1 1 calc R U . . .
H7C H 0.679722 -0.172167 0.890386 0.052 Uiso 1 1 calc R U . . .
C8 C 0.4680(2) 0.0671(7) 0.72336(18) 0.0254(11) Uani 1 1 d . . . . .
C9 C 0.4154(2) 0.0309(8) 0.68298(19) 0.0316(12) Uani 1 1 d . . . . .
H9 H 0.369543 0.040509 0.683293 0.038 Uiso 1 1 calc R U . . .
C10 C 0.4243(2) -0.0155(7) 0.64455(19) 0.0306(12) Uani 1 1 d . . . . .
C11 C 0.4440(3) 0.1063(8) 0.76227(19) 0.0309(12) Uani 1 1 d . . . . .
H11A H 0.437621 -0.006474 0.776183 0.046 Uiso 1 1 calc R U . . .
H11B H 0.400456 0.171255 0.752373 0.046 Uiso 1 1 calc R U . . .
H11C H 0.478243 0.179547 0.783616 0.046 Uiso 1 1 calc R U . . .
C12 C 0.3674(3) -0.0648(8) 0.6039(2) 0.0379(13) Uani 1 1 d . . . . .
H12A H 0.363909 0.025187 0.580963 0.057 Uiso 1 1 calc R U . . .
H12B H 0.324177 -0.069540 0.610719 0.057 Uiso 1 1 calc R U . . .
H12C H 0.376700 -0.182248 0.593356 0.057 Uiso 1 1 calc R U . . .
C13 C 0.5929(3) 0.3425(8) 0.60542(19) 0.0328(12) Uani 1 1 d . . . . .
C14 C 0.6161(3) 0.4241(8) 0.5736(2) 0.0377(13) Uani 1 1 d . . . . .
H14 H 0.648443 0.365184 0.562725 0.045 Uiso 1 1 calc R U . . .
C15 C 0.5917(3) 0.5922(8) 0.55795(19) 0.0346(13) Uani 1 1 d . . . . .
C16 C 0.5439(3) 0.6754(8) 0.5755(2) 0.0403(14) Uani 1 1 d . . . . .
H16 H 0.527434 0.791738 0.565542 0.048 Uiso 1 1 calc R U . . .
C17 C 0.5206(3) 0.5911(8) 0.6067(2) 0.0361(13) Uani 1 1 d . . . . .
H17 H 0.487678 0.647889 0.617384 0.043 Uiso 1 1 calc R U . . .
C18 C 0.5459(3) 0.4226(8) 0.62225(19) 0.0347(12) Uani 1 1 d . . . . .
C19 C 0.6154(3) 0.6948(9) 0.5239(2) 0.0434(15) Uani 1 1 d . . . . .
C20 C 0.6600(4) 0.5778(11) 0.5048(3) 0.061(2) Uani 1 1 d . . . . .
H20A H 0.701861 0.544695 0.528211 0.092 Uiso 1 1 calc R U . . .
H20B H 0.671909 0.644419 0.481802 0.092 Uiso 1 1 calc R U . . .
H20C H 0.634717 0.469280 0.492041 0.092 Uiso 1 1 calc R U . . .
C21 C 0.6588(4) 0.8576(11) 0.5464(3) 0.061(2) Uani 1 1 d . . . . .
H21A H 0.630435 0.939882 0.557025 0.092 Uiso 1 1 calc R U . . .
H21B H 0.676239 0.919599 0.525036 0.092 Uiso 1 1 calc R U . . .
H21C H 0.697383 0.816520 0.571259 0.092 Uiso 1 1 calc R U . . .
C22 C 0.5543(4) 0.7598(12) 0.4857(2) 0.063(2) Uani 1 1 d . . . . .
H22A H 0.528665 0.656343 0.470012 0.094 Uiso 1 1 calc R U . . .
H22B H 0.570709 0.831429 0.465374 0.094 Uiso 1 1 calc R U . . .
H22C H 0.524290 0.833255 0.497253 0.094 Uiso 1 1 calc R U . . .
C23 C 0.6760(3) -0.2464(8) 0.6735(2) 0.0389(14) Uani 1 1 d . . . . .
H23A H 0.669058 -0.285953 0.642854 0.047 Uiso 1 1 calc R U . . .
H23B H 0.673501 -0.353130 0.691307 0.047 Uiso 1 1 calc R U . . .
C24 C 0.7440(3) -0.1626(11) 0.6913(4) 0.074(3) Uani 1 1 d . . . . .
H24A H 0.747532 -0.061539 0.672606 0.111 Uiso 1 1 calc R U . . .
H24B H 0.779545 -0.250918 0.691936 0.111 Uiso 1 1 calc R U . . .
H24C H 0.750252 -0.119694 0.721323 0.111 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
Nb1 O1 1.975(4) . ?
Nb1 O2 1.984(4) . ?
Nb1 O3 1.990(4) . ?
Nb1 O4 2.006(4) . ?
Nb1 O5 1.843(4) . ?
Nb1 N1 2.236(4) . ?
O1 C1 1.354(7) . ?
O2 C10 1.327(6) . ?
O3 C13 1.382(7) . ?
O4 C18 1.336(7) . ?
O5 C23 1.426(6) . ?
N1 C6 1.430(7) . ?
N1 C8 1.330(6) . ?
C1 C2 1.379(8) . ?
C1 C6 1.415(7) . ?
C2 H2 0.9500 . ?
C2 C3 1.391(8) . ?
C3 H3 0.9500 . ?
C3 C4 1.388(8) . ?
C4 C5 1.399(8) . ?
C4 C7 1.505(8) . ?
C5 H5 0.9500 . ?
C5 C6 1.393(7) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.426(7) . ?
C8 C11 1.503(7) . ?
C9 H9 0.9500 . ?
C9 C10 1.343(8) . ?
C10 C12 1.498(8) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.392(8) . ?
C13 C18 1.381(7) . ?
C14 H14 0.9500 . ?
C14 C15 1.386(9) . ?
C15 C16 1.418(8) . ?
C15 C19 1.530(8) . ?
C16 H16 0.9500 . ?
C16 C17 1.386(8) . ?
C17 H17 0.9500 . ?
C17 C18 1.393(9) . ?
C19 C20 1.527(10) . ?
C19 C21 1.546(10) . ?
C19 C22 1.533(9) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.475(8) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?

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 Nb1 O2 154.00(14) . . ?
O1 Nb1 O3 96.87(15) . . ?
O1 Nb1 O4 89.91(15) . . ?
O1 Nb1 N1 74.64(14) . . ?
O2 Nb1 O3 107.18(16) . . ?
O2 Nb1 O4 85.93(15) . . ?
O2 Nb1 N1 79.75(15) . . ?
O3 Nb1 O4 77.38(15) . . ?
O3 Nb1 N1 165.51(16) . . ?
O4 Nb1 N1 90.70(15) . . ?
O5 Nb1 O1 94.83(16) . . ?
O5 Nb1 O2 94.50(16) . . ?
O5 Nb1 O3 90.99(17) . . ?
O5 Nb1 O4 167.90(17) . . ?
O5 Nb1 N1 101.29(16) . . ?
C1 O1 Nb1 118.9(3) . . ?
C10 O2 Nb1 134.6(4) . . ?
C13 O3 Nb1 116.6(3) . . ?
C18 O4 Nb1 117.4(3) . . ?
C23 O5 Nb1 160.1(4) . . ?
C6 N1 Nb1 109.8(3) . . ?
C8 N1 Nb1 126.8(4) . . ?
C8 N1 C6 122.7(4) . . ?
O1 C1 C2 122.8(5) . . ?
O1 C1 C6 116.5(5) . . ?
C2 C1 C6 120.7(5) . . ?
C1 C2 H2 120.5 . . ?
C1 C2 C3 119.0(5) . . ?
C3 C2 H2 120.5 . . ?
C2 C3 H3 119.1 . . ?
C4 C3 C2 121.8(5) . . ?
C4 C3 H3 119.1 . . ?
C3 C4 C5 118.9(5) . . ?
C3 C4 C7 121.0(5) . . ?
C5 C4 C7 120.1(5) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 C4 120.4(5) . . ?
C6 C5 H5 119.8 . . ?
C1 C6 N1 112.1(4) . . ?
C5 C6 N1 128.4(4) . . ?
C5 C6 C1 119.1(5) . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N1 C8 C9 121.1(5) . . ?
N1 C8 C11 123.2(5) . . ?
C9 C8 C11 115.7(4) . . ?
C8 C9 H9 116.8 . . ?
C10 C9 C8 126.5(5) . . ?
C10 C9 H9 116.8 . . ?
O2 C10 C9 122.7(5) . . ?
O2 C10 C12 113.1(5) . . ?
C9 C10 C12 124.2(5) . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O3 C13 C14 123.8(5) . . ?
C18 C13 O3 113.7(5) . . ?
C18 C13 C14 122.5(6) . . ?
C13 C14 H14 120.3 . . ?
C15 C14 C13 119.4(5) . . ?
C15 C14 H14 120.3 . . ?
C14 C15 C16 118.2(5) . . ?
C14 C15 C19 123.3(5) . . ?
C16 C15 C19 118.4(5) . . ?
C15 C16 H16 119.2 . . ?
C17 C16 C15 121.6(6) . . ?
C17 C16 H16 119.2 . . ?
C16 C17 H17 120.2 . . ?
C16 C17 C18 119.5(5) . . ?
C18 C17 H17 120.2 . . ?
O4 C18 C13 114.8(5) . . ?
O4 C18 C17 126.4(5) . . ?
C13 C18 C17 118.8(5) . . ?
C15 C19 C21 109.4(5) . . ?
C15 C19 C22 111.1(5) . . ?
C20 C19 C15 111.3(6) . . ?
C20 C19 C21 107.7(5) . . ?
C20 C19 C22 107.9(6) . . ?
C22 C19 C21 109.4(6) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O5 C23 H23A 109.5 . . ?
O5 C23 H23B 109.5 . . ?
O5 C23 C24 110.5(5) . . ?
H23A C23 H23B 108.1 . . ?
C24 C23 H23A 109.5 . . ?
C24 C23 H23B 109.5 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?

_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 1.912
_oxdiff_exptl_absorpt_empirical_full_min 0.351

# start Validation Reply Form
_vrf_PLAT971_C-1tBu              
;
PROBLEM: Check Calcd Resid. Dens.  1.19Ang From O4              4.76 eA-3  
RESPONSE: Density is not located in any chemically relevant position. 
This residual electron density is likely due to low data quality 
stemming from the nature of the crystal. (i.e. not single crystalline)
;
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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_C-2
_database_code_depnum_ccdc_archive 'CCDC 2331122'
loop_
_audit_author_name
_audit_author_address
'Christopher Durr'
;Amherst College
United States of America
;
_audit_update_record             
;
2024-02-05 deposited with the CCDC.	2024-03-19 downloaded from the CCDC.
;
_audit_creation_date             2022-07-08
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C20 H22 N O5 Ta'
_chemical_formula_sum            'C20 H22 N O5 Ta'
_chemical_formula_weight         537.33
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Ta N O C H'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ta Ta -5.7959 5.2718 '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           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   15.1648(2)
_cell_length_b                   7.73010(10)
_cell_length_c                   16.3269(2)
_cell_angle_alpha                90
_cell_angle_beta                 95.7830(10)
_cell_angle_gamma                90
_cell_volume                     1904.19(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    14791
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      67.8430
_cell_measurement_theta_min      2.7070
_shelx_estimated_absorpt_T_max   0.515
_shelx_estimated_absorpt_T_min   0.208
_exptl_absorpt_coefficient_mu    10.924
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40137
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.110a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.874
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1048
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-5 -2 -8 0.0863
-8 0 7 0.0230
7 2 6 0.0872
7 0 -8 0.0360
-7 0 -7 0.0947
-3 -5 -3 0.0469
7 0 7 0.0672
-2 5 -2 0.0854

_exptl_crystal_size_max          0.215
_exptl_crystal_size_mid          0.167
_exptl_crystal_size_min          0.073
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-5.1803 -1.7207 -7.6453 -0.0066 -0.1445 0.9895
-8.2762 0.1680 6.5922 0.0241 0.9876 0.1554
6.6945 1.6505 6.1846 0.0017 -0.0526 -0.9986
7.3266 -0.4489 -7.7712 -0.0249 -0.9996 0.0092
-6.7539 -0.0290 -6.9406 -0.3282 0.0458 0.9435
-2.5818 -4.6132 -2.8102 0.7275 -0.0927 0.6798
6.7545 -0.1125 6.9365 0.3545 -0.0492 -0.9338
-1.9838 4.8129 -1.8742 -0.9900 0.1289 -0.0572

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19529
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.932
_diffrn_reflns_theta_min         3.792
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     23.00 108.00   0.50    0.20    --   41.95  54.00  30.00  170
  2  ω     23.00 108.00   0.50    0.20    --   41.95  54.00 120.00  170
  3  ω     23.00 108.00   0.50    0.20    --   41.95  54.00  60.00  170
  4  ω     23.00 108.00   0.50    0.20    --   41.95  54.00 -60.00  170
  5  ω     23.00 108.00   0.50    0.20    --   41.95  54.00-180.00  170
  6  ω     23.00 108.00   0.50    0.20    --   41.95  54.00-150.00  170
  7  ω     23.00 108.00   0.50    0.20    --   41.95  54.00-120.00  170
  8  ω     23.00 108.00   0.50    0.20    --   41.95  54.00 -30.00  170
  9  ω     23.00 108.00   0.50    0.20    --   41.95  54.00 150.00  170
 10  ω    -33.00  24.00   0.50    0.20    --   41.95 -11.00   0.00  114
 11  ω    -33.00  24.00   0.50    0.20    --   41.95 -11.00 120.00  114
 12  ω    -23.00  48.00   0.50    0.20    --   41.95 -43.00-180.00  142
 13  ω     77.00 152.00   0.50    0.40    --   93.72  17.00  30.00  150
 14  ω     84.00 165.00   0.50    0.40    --   93.72  97.00-133.00  162
 15  ω     97.00 162.00   0.50    0.40    --   93.72  68.00 -90.00  130
 16  ω     19.00  99.00   0.50    0.20    --   41.95-138.00-150.00  160
 17  ω     19.00  99.00   0.50    0.20    --   41.95-138.00  60.00  160
 18  ω    -28.00  75.00   0.50    0.20    --   41.95 -97.00 119.00  206
 19  ω     21.00 107.00   0.50    0.40    --   93.72 -97.00 119.00  172
 20  ω     26.00  83.00   0.50    0.40    --   93.72 -68.00 120.00  114
 21  ω     28.00  57.00   0.50    0.40    --   93.72 -50.00 150.00   58
 22  ω     28.00  57.00   0.50    0.40    --   93.72 -50.00 120.00   58
 23  ω     28.00  57.00   0.50    0.40    --   93.72 -50.00 -90.00   58
 24  ω     28.00  57.00   0.50    0.40    --   93.72 -50.00-120.00   58
 25  ω    -24.00  32.00   0.50    0.20    --  -42.26  11.00-150.00  112
 26  ω    -83.00 -26.00   0.50    0.40    --  -94.03  68.00-120.00  114
 27  ω    -83.00 -26.00   0.50    0.40    --  -94.03  68.00-150.00  114
 28  ω    -83.00 -26.00   0.50    0.40    --  -94.03  68.00-180.00  114
 29  ω    -48.00  24.00   0.50    0.20    --  -42.26  43.00-120.00  144
 30  ω    -57.00 -28.00   0.50    0.40    --  -94.03  50.00-180.00   58
 31  ω    -57.00 -28.00   0.50    0.40    --  -94.03  50.00-120.00   58
 32  ω    -68.00 -27.00   0.50    0.40    --  -94.03  59.00 -30.00   82
 33  ω    -57.00 -28.00   0.50    0.40    --  -94.03  50.00  30.00   58
 34  ω    -24.00  32.00   0.50    0.20    --  -42.26  11.00 150.00  112
 35  ω    -68.00 -27.00   0.50    0.40    --  -94.03  59.00  90.00   82
 36  ω   -160.00 -77.00   0.50    0.40    --  -94.03 -50.00 -60.00  166
 37  ω   -161.00 -97.00   0.50    0.40    --  -94.03 -68.00-150.00  128
 38  ω   -160.00 -87.00   0.50    0.40    --  -94.03 -59.00-180.00  146
 39  ω    -75.00  29.00   0.50    0.20    --  -42.26  97.00-133.00  208
 40  ω   -106.00 -22.00   0.50    0.40    --  -94.03  97.00-133.00  168
 41  ω   -161.00 -97.00   0.50    0.40    --  -94.03 -68.00 150.00  128
 42  ω   -167.00 -84.00   0.50    0.40    --  -94.03 -97.00 119.00  166
 43  ω   -109.00 -79.00   0.50    0.20    --  -42.26-138.00 -30.00   60
 44  ω   -109.00 -79.00   0.50    0.20    --  -42.26-138.00 -90.00   60
 45  ω   -109.00 -79.00   0.50    0.20    --  -42.26-138.00-150.00   60
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at home/near, HyPix3000'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0177952000
_diffrn_orient_matrix_UB_12      -0.1863880000
_diffrn_orient_matrix_UB_13      0.0307529000
_diffrn_orient_matrix_UB_21      -0.0699741000
_diffrn_orient_matrix_UB_22      0.0218446000
_diffrn_orient_matrix_UB_23      0.0614018000
_diffrn_orient_matrix_UB_31      -0.0722154000
_diffrn_orient_matrix_UB_32      -0.0671224000
_diffrn_orient_matrix_UB_33      -0.0653845000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3278
_reflns_number_total             3443
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.65
_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 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.721
_refine_diff_density_min         -0.873
_refine_diff_density_rms         0.089
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         3443
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0220
_refine_ls_R_factor_gt           0.0206
_refine_ls_restrained_S_all      1.060
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0211P)²+2.8587P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0491
_refine_ls_wR_factor_ref         0.0499
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C9(H9), C14(H14), C15(H15), C16(H16), C17(H17)
2.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C20(H20A,H20B,H20C)
;
_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
Ta1 Ta 0.52655(2) 0.33241(2) 0.72185(2) 0.01602(6) Uani 1 1 d . . . . .
O1 O 0.55115(13) 0.4379(3) 0.61684(12) 0.0207(5) Uani 1 1 d . . . . .
O2 O 0.55890(13) 0.2193(3) 0.82928(12) 0.0192(4) Uani 1 1 d . . . . .
O3 O 0.54713(13) 0.5611(3) 0.77932(12) 0.0192(4) Uani 1 1 d . . . . .
O4 O 0.40474(13) 0.4150(3) 0.73153(13) 0.0221(5) Uani 1 1 d . . . . .
O5 O 0.48311(13) 0.1295(3) 0.67347(13) 0.0209(5) Uani 1 1 d . . . . .
N1 N 0.67219(16) 0.3120(3) 0.71990(15) 0.0157(5) Uani 1 1 d . . . . .
C1 C 0.62630(19) 0.3906(4) 0.58276(18) 0.0190(6) Uani 1 1 d . . . . .
C2 C 0.6352(2) 0.4053(4) 0.49980(18) 0.0207(6) Uani 1 1 d . . . . .
H2 H 0.590383 0.459415 0.463750 0.025 Uiso 1 1 calc R U . . .
C3 C 0.7110(2) 0.3392(4) 0.4700(2) 0.0234(7) Uani 1 1 d . . . . .
H3 H 0.717808 0.350371 0.413017 0.028 Uiso 1 1 calc R U . . .
C4 C 0.7772(2) 0.2574(4) 0.52099(18) 0.0198(6) Uani 1 1 d . . . . .
C5 C 0.7687(2) 0.2495(4) 0.60571(18) 0.0185(6) Uani 1 1 d . . . . .
H5 H 0.813645 0.196198 0.641938 0.022 Uiso 1 1 calc R U . . .
C6 C 0.6943(2) 0.3200(3) 0.63649(18) 0.0158(6) Uani 1 1 d . . . . .
C7 C 0.8559(2) 0.1742(4) 0.4869(2) 0.0270(8) Uani 1 1 d . . . . .
H7A H 0.835479 0.079408 0.449892 0.041 Uiso 1 1 calc R U . . .
H7B H 0.896477 0.128695 0.532319 0.041 Uiso 1 1 calc R U . . .
H7C H 0.886787 0.260566 0.456384 0.041 Uiso 1 1 calc R U . . .
C8 C 0.7316(2) 0.3215(4) 0.78509(18) 0.0161(6) Uani 1 1 d . . . . .
C9 C 0.7083(2) 0.2867(4) 0.86574(18) 0.0192(6) Uani 1 1 d . . . . .
H9 H 0.752980 0.303549 0.910145 0.023 Uiso 1 1 calc R U . . .
C10 C 0.6281(2) 0.2315(4) 0.88478(18) 0.0184(6) Uani 1 1 d . . . . .
C11 C 0.8268(2) 0.3681(4) 0.77983(19) 0.0207(6) Uani 1 1 d . . . . .
H11A H 0.861667 0.262250 0.775512 0.031 Uiso 1 1 calc R U . . .
H11B H 0.849498 0.431947 0.829382 0.031 Uiso 1 1 calc R U . . .
H11C H 0.831604 0.440367 0.731176 0.031 Uiso 1 1 calc R U . . .
C12 C 0.6105(2) 0.1774(4) 0.96934(19) 0.0264(7) Uani 1 1 d . . . . .
H12A H 0.568269 0.257737 0.990539 0.040 Uiso 1 1 calc R U . . .
H12B H 0.666087 0.178659 1.005608 0.040 Uiso 1 1 calc R U . . .
H12C H 0.585631 0.060297 0.967430 0.040 Uiso 1 1 calc R U . . .
C13 C 0.47452(19) 0.6549(4) 0.79284(18) 0.0178(6) Uani 1 1 d . . . . .
C14 C 0.4751(2) 0.8188(4) 0.82656(19) 0.0206(7) Uani 1 1 d . . . . .
H14 H 0.529427 0.876705 0.842206 0.025 Uiso 1 1 calc R U . . .
C15 C 0.3942(2) 0.8977(4) 0.83719(19) 0.0248(7) Uani 1 1 d . . . . .
H15 H 0.393254 1.011595 0.859002 0.030 Uiso 1 1 calc R U . . .
C16 C 0.3157(2) 0.8114(4) 0.8162(2) 0.0261(7) Uani 1 1 d . . . . .
H16 H 0.261335 0.864825 0.826148 0.031 Uiso 1 1 calc R U . . .
C17 C 0.3143(2) 0.6480(4) 0.7809(2) 0.0267(7) Uani 1 1 d . . . . .
H17 H 0.259841 0.590077 0.766061 0.032 Uiso 1 1 calc R U . . .
C18 C 0.3943(2) 0.5714(4) 0.76787(18) 0.0199(6) Uani 1 1 d . . . . .
C19 C 0.4268(2) 0.0124(4) 0.62546(19) 0.0266(7) Uani 1 1 d . . . . .
H19A H 0.376790 -0.021641 0.656556 0.032 Uiso 1 1 calc R U . . .
H19B H 0.460448 -0.093303 0.614286 0.032 Uiso 1 1 calc R U . . .
C20 C 0.3916(3) 0.0946(5) 0.5456(2) 0.0427(10) Uani 1 1 d . . . . .
H20A H 0.357596 0.009071 0.511136 0.064 Uiso 1 1 calc R U . . .
H20B H 0.441108 0.136631 0.516840 0.064 Uiso 1 1 calc R U . . .
H20C H 0.353006 0.191900 0.556495 0.064 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
Ta1 O1 1.968(2) . ?
Ta1 O2 1.977(2) . ?
Ta1 O3 2.011(2) . ?
Ta1 O4 1.976(2) . ?
Ta1 O5 1.848(2) . ?
Ta1 N1 2.218(2) . ?
O1 C1 1.367(4) . ?
O2 C10 1.319(4) . ?
O3 C13 1.355(3) . ?
O4 C18 1.363(4) . ?
O5 C19 1.424(4) . ?
N1 C6 1.436(4) . ?
N1 C8 1.325(4) . ?
C1 C2 1.379(4) . ?
C1 C6 1.396(4) . ?
C2 C3 1.390(5) . ?
C3 C4 1.390(4) . ?
C4 C5 1.403(4) . ?
C4 C7 1.510(4) . ?
C5 C6 1.392(4) . ?
C8 C9 1.423(4) . ?
C8 C11 1.499(4) . ?
C9 C10 1.355(4) . ?
C10 C12 1.492(4) . ?
C13 C14 1.381(4) . ?
C13 C18 1.401(4) . ?
C14 C15 1.397(4) . ?
C15 C16 1.377(5) . ?
C16 C17 1.388(5) . ?
C17 C18 1.385(4) . ?
C19 C20 1.500(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
O1 Ta1 O2 154.74(8) . . ?
O1 Ta1 O3 90.46(9) . . ?
O1 Ta1 O4 101.33(8) . . ?
O1 Ta1 N1 74.96(8) . . ?
O2 Ta1 O3 87.82(8) . . ?
O2 Ta1 N1 79.79(8) . . ?
O3 Ta1 N1 87.78(8) . . ?
O4 Ta1 O2 102.85(8) . . ?
O4 Ta1 O3 77.34(8) . . ?
O4 Ta1 N1 164.71(9) . . ?
O5 Ta1 O1 94.02(9) . . ?
O5 Ta1 O2 92.85(9) . . ?
O5 Ta1 O3 167.88(8) . . ?
O5 Ta1 O4 90.73(9) . . ?
O5 Ta1 N1 104.26(9) . . ?
C1 O1 Ta1 118.86(17) . . ?
C10 O2 Ta1 133.40(19) . . ?
C13 O3 Ta1 117.13(18) . . ?
C18 O4 Ta1 118.18(18) . . ?
C19 O5 Ta1 160.6(2) . . ?
C6 N1 Ta1 109.79(18) . . ?
C8 N1 Ta1 125.6(2) . . ?
C8 N1 C6 123.7(3) . . ?
O1 C1 C2 123.1(3) . . ?
O1 C1 C6 116.2(3) . . ?
C2 C1 C6 120.7(3) . . ?
C1 C2 C3 118.7(3) . . ?
C2 C3 C4 122.0(3) . . ?
C3 C4 C5 118.6(3) . . ?
C3 C4 C7 121.5(3) . . ?
C5 C4 C7 119.9(3) . . ?
C6 C5 C4 119.8(3) . . ?
C1 C6 N1 112.6(3) . . ?
C5 C6 N1 126.9(3) . . ?
C5 C6 C1 120.0(3) . . ?
N1 C8 C9 121.4(3) . . ?
N1 C8 C11 123.2(3) . . ?
C9 C8 C11 115.4(3) . . ?
C10 C9 C8 125.8(3) . . ?
O2 C10 C9 122.4(3) . . ?
O2 C10 C12 114.3(3) . . ?
C9 C10 C12 123.3(3) . . ?
O3 C13 C14 125.7(3) . . ?
O3 C13 C18 113.7(3) . . ?
C14 C13 C18 120.6(3) . . ?
C13 C14 C15 118.7(3) . . ?
C16 C15 C14 120.4(3) . . ?
C15 C16 C17 121.3(3) . . ?
C18 C17 C16 118.5(3) . . ?
O4 C18 C13 113.6(3) . . ?
O4 C18 C17 126.1(3) . . ?
C17 C18 C13 120.4(3) . . ?
O5 C19 C20 110.5(3) . . ?

_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 2.142
_oxdiff_exptl_absorpt_empirical_full_min 0.623
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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_C-3OMe
_database_code_depnum_ccdc_archive 'CCDC 2331123'
loop_
_audit_author_name
_audit_author_address
'Christopher Durr'
;Amherst College
United States of America
;
_audit_update_record             
;
2024-02-05 deposited with the CCDC.	2024-03-19 downloaded from the CCDC.
;
_audit_creation_date             2023-11-17
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C20 H21 Cl N Nb O6'
_chemical_formula_sum            'C20 H21 Cl N Nb O6'
_chemical_formula_weight         499.74
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Nb Cl O N C H'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -0.1121 2.4826 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.93594(17)
_cell_length_b                   11.4858(2)
_cell_length_c                   12.4086(2)
_cell_angle_alpha                115.7499(18)
_cell_angle_beta                 90.3226(17)
_cell_angle_gamma                91.8519(16)
_cell_volume                     1017.95(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    10697
_cell_measurement_temperature    120.00(16)
_cell_measurement_theta_max      67.9160
_cell_measurement_theta_min      3.9300
_shelx_estimated_absorpt_T_max   0.754
_shelx_estimated_absorpt_T_min   0.437
_exptl_absorpt_coefficient_mu    6.356
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.860
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.93a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             508
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
4 4 -1 0.0287
0 -4 8 0.0381
-4 -4 1 0.0952
0 3 -8 0.0114
5 1 0 0.0424
0 7 -1 0.0137
-5 0 0 0.1017
0 -7 1 0.0311

_exptl_crystal_size_max          0.156
_exptl_crystal_size_mid          0.053
_exptl_crystal_size_min          0.047
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
4.1916 4.0792 -1.3682 0.0068 -0.1229 0.9924
-0.1362 -3.7516 8.0278 -0.0789 0.9909 -0.1086
-4.2173 -3.9820 1.1068 -0.0042 0.0904 -0.9959
-0.2898 3.4041 -8.0369 0.0797 -0.9968 0.0091
5.0979 0.7610 -0.1408 -0.4387 0.0138 0.8985
-0.1020 6.9145 -0.5352 0.8370 -0.0191 0.5469
-5.1243 -0.4742 0.1190 0.4757 -0.0146 -0.8795
-0.2466 -6.8920 0.5390 -0.7981 0.0180 -0.6023

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0555
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19633
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.084
_diffrn_reflns_theta_min         3.956
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(16)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      2.00  80.00   0.50    2.00    --   41.95-111.00-156.00  156
  2  ω    -80.00  -2.00   0.50    2.00    --  -42.26 111.00 -62.00  156
  3  ω     30.00 109.00   0.50    8.00    --   93.72-111.00-156.00  158
  4  ω     81.00 158.00   0.50    8.00    --   93.72 111.00 -62.00  154
  5  ω   -158.00 -81.00   0.50    8.00    --  -94.03-111.00-156.00  154
  6  ω   -109.00 -30.00   0.50    8.00    --  -94.03 111.00 -62.00  158
  7  ω    -28.00  28.00   0.50    2.00    --   41.95 -21.00 -30.00  112
  8  ω    -24.00  37.00   0.50    2.00    --   41.95 -32.00   0.00  122
  9  ω    -23.00  48.00   0.50    2.00    --   41.95 -43.00-120.00  142
 10  ω    -28.00  28.00   0.50    2.00    --   41.95 -21.00-150.00  112
 11  ω    -15.00  72.00   0.50    2.00    --   41.95 -89.00  30.00  174
 12  ω    -33.00  24.00   0.50    2.00    --   41.95 -11.00 -90.00  114
 13  ω    -64.00  25.00   0.50    2.00    --  -42.26  65.00-120.00  178
 14  ω   -112.00 -29.00   0.50    2.00    --  -42.26 -21.00-150.00  166
 15  ω    -24.00  32.00   0.50    2.00    --  -42.26  11.00-120.00  112
 16  ω   -109.00 -79.00   0.50    2.00    --  -42.26-138.00 -90.00   60
 17  ω    -78.00   4.00   0.50    2.00    --  -42.26 104.00  90.00  164
 18  ω   -112.00 -29.00   0.50    2.00    --  -42.26 -21.00 -90.00  166
 19  ω    -28.00  28.00   0.50    2.00    --  -42.26  21.00-180.00  112
 20  ω     28.00  57.00   0.50    8.00    --   93.72 -50.00 -90.00   58
 21  ω     28.00  57.00   0.50    8.00    --   93.72 -50.00  30.00   58
 22  ω     28.00  57.00   0.50    8.00    --   93.72 -50.00-180.00   58
 23  ω     87.00 161.00   0.50    8.00    --   93.72  59.00  30.00  148
 24  ω     28.00  57.00   0.50    8.00    --   93.72 -50.00-120.00   58
 25  ω     27.00 127.00   0.50    8.00    --   93.72-145.00  90.00  200
 26  ω     99.00 165.00   0.50    8.00    --   93.72  96.00 -30.00  132
 27  ω     28.00  57.00   0.50    8.00    --   93.72 -50.00 -30.00   58
 28  ω     23.00 106.00   0.50    8.00    --   93.72 -96.00-150.00  166
 29  ω     79.00 160.00   0.50    8.00    --   93.72  42.00  60.00  162
 30  ω     27.00 127.00   0.50    8.00    --   93.72-145.00-150.00  200
 31  ω     26.00  83.00   0.50    8.00    --   93.72 -68.00-180.00  114
 32  ω    101.00 162.00   0.50    8.00    --   93.72  77.00  60.00  122
 33  ω     28.00  57.00   0.50    8.00    --   93.72 -50.00-150.00   58
 34  ω   -159.00 -79.00   0.50    8.00    --  -94.03 -42.00-150.00  160
 35  ω   -105.00 -25.00   0.50    8.00    --  -94.03  77.00 -60.00  160
 36  ω   -106.00 -23.00   0.50    8.00    --  -94.03  96.00  60.00  166
 37  ω   -161.00 -97.00   0.50    8.00    --  -94.03 -68.00 -60.00  128
 38  ω    -83.00 -26.00   0.50    8.00    --  -94.03  68.00  60.00  114
 39  ω   -105.00 -25.00   0.50    8.00    --  -94.03  77.00   0.00  160
 40  ω   -163.00-101.00   0.50    8.00    --  -94.03 -87.00   0.00  124
 41  ω    -83.00 -26.00   0.50    8.00    --  -94.03  68.00 -60.00  114
 42  ω   -109.00 -32.00   0.50    8.00    --  -94.03 117.00  60.00  154
 43  ω   -106.00 -23.00   0.50    8.00    --  -94.03  96.00 120.00  166
 44  ω   -161.00 -97.00   0.50    8.00    --  -94.03 -68.00 -30.00  128
 45  ω    -83.00 -26.00   0.50    8.00    --  -94.03  68.00 120.00  114
 46  ω     23.00 108.00   0.50    2.00    --   41.95  54.00   0.00  170
 47  ω     23.00 108.00   0.50    2.00    --   41.95  54.00  60.00  170
 48  ω     23.00 108.00   0.50    2.00    --   41.95  54.00  90.00  170
 49  ω     23.00 108.00   0.50    2.00    --   41.95  54.00 150.00  170
 50  ω     27.00 108.00   0.50    2.00    --   41.95  43.00 -30.00  162
 51  ω     23.00 108.00   0.50    2.00    --   41.95  54.00-150.00  170
 52  ω     23.00 108.00   0.50    2.00    --   41.95  54.00  30.00  170
 53  ω     23.00 108.00   0.50    2.00    --   41.95  54.00 120.00  170
 54  ω   -108.00 -24.00   0.50    2.00    --  -42.26 -54.00-180.00  168
 55  ω   -108.00 -24.00   0.50    2.00    --  -42.26 -54.00   0.00  168
 56  ω   -108.00 -24.00   0.50    2.00    --  -42.26 -54.00 120.00  168
 57  ω   -108.00 -24.00   0.50    2.00    --  -42.26 -54.00-120.00  168
 58  ω   -108.00 -24.00   0.50    2.00    --  -42.26 -54.00-150.00  168
 59  ω     79.00 160.00   0.50    8.00    --   93.72  42.00 120.00  162
 60  ω     76.00 133.00   0.50    8.00    --   93.72  50.00  30.00  114
 61  ω     76.00 160.00   0.50    8.00    --   93.72  50.00 -30.00  168
 62  ω     76.00 160.00   0.50    8.00    --   93.72  50.00 150.00  168
 63  ω     76.00 160.00   0.50    8.00    --   93.72  50.00  90.00  168
 64  ω     76.00 160.00   0.50    8.00    --   93.72  50.00   0.00  168
 65  ω   -161.00 -97.00   0.50    8.00    --  -94.03 -68.00 -90.00  128
 66  ω   -160.00 -77.00   0.50    8.00    --  -94.03 -50.00-120.00  166
 67  ω   -160.00 -77.00   0.50    8.00    --  -94.03 -50.00 -90.00  166
 68  ω   -160.00 -77.00   0.50    8.00    --  -94.03 -50.00-180.00  166
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at home/near, HyPix3000'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1031547000
_diffrn_orient_matrix_UB_12      0.1230768000
_diffrn_orient_matrix_UB_13      0.0459348000
_diffrn_orient_matrix_UB_21      0.0051392000
_diffrn_orient_matrix_UB_22      0.0071283000
_diffrn_orient_matrix_UB_23      0.1268584000
_diffrn_orient_matrix_UB_31      0.1645433000
_diffrn_orient_matrix_UB_32      0.0837270000
_diffrn_orient_matrix_UB_33      0.0283920000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3393
_reflns_number_total             3682
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.65
_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 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.952
_refine_diff_density_min         -0.974
_refine_diff_density_rms         0.106
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         3682
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0340
_refine_ls_restrained_S_all      1.054
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0531P)²+1.1394P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0909
_refine_ls_wR_factor_ref         0.0928
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C8(H8), C14(H14), C15(H15), C16(H16)
2.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C18(H18A,H18B,H18C), C20(H20A,H20B,
 H20C)
;
_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
Nb1 Nb 0.68152(3) 0.55324(2) 0.26934(2) 0.02104(11) Uani 1 1 d . . . . .
Cl1 Cl 0.62416(11) 0.91197(8) 0.88129(7) 0.0340(2) Uani 1 1 d . . . . .
O1 O 0.7676(3) 0.5192(2) 0.4025(2) 0.0244(5) Uani 1 1 d . . . . .
O2 O 0.4679(3) 0.4588(2) 0.1925(2) 0.0258(5) Uani 1 1 d . . . . .
O3 O 0.8555(3) 0.6972(2) 0.32856(19) 0.0230(5) Uani 1 1 d . . . . .
O4 O 0.6086(3) 0.6682(2) 0.19583(19) 0.0243(5) Uani 1 1 d . . . . .
O5 O 0.7939(3) 0.4155(2) 0.1539(2) 0.0286(5) Uani 1 1 d . . . . .
O6 O 1.0963(3) 0.8983(2) 0.3886(2) 0.0300(5) Uani 1 1 d . . . . .
N1 N 0.5047(3) 0.6477(2) 0.4193(2) 0.0206(5) Uani 1 1 d . . . . .
C1 C 0.7355(4) 0.6061(3) 0.5148(3) 0.0242(7) Uani 1 1 d . . . . .
C2 C 0.8417(4) 0.6258(3) 0.6108(3) 0.0268(7) Uani 1 1 d . . . . .
H2 H 0.938246 0.575226 0.598992 0.032 Uiso 1 1 calc R U . . .
C3 C 0.8065(4) 0.7192(3) 0.7235(3) 0.0286(7) Uani 1 1 d . . . . .
H3 H 0.878129 0.733402 0.790017 0.034 Uiso 1 1 calc R U . . .
C4 C 0.6649(4) 0.7922(3) 0.7382(3) 0.0255(7) Uani 1 1 d . . . . .
C5 C 0.5570(4) 0.7751(3) 0.6445(3) 0.0235(7) Uani 1 1 d . . . . .
H5 H 0.461535 0.826981 0.657491 0.028 Uiso 1 1 calc R U . . .
C6 C 0.5905(4) 0.6802(3) 0.5301(3) 0.0216(6) Uani 1 1 d . . . . .
C7 C 0.3409(4) 0.6619(3) 0.4070(3) 0.0219(6) Uani 1 1 d . . . . .
C8 C 0.2610(4) 0.6066(3) 0.2922(3) 0.0239(7) Uani 1 1 d . . . . .
H8 H 0.159066 0.643150 0.283479 0.029 Uiso 1 1 calc R U . . .
C9 C 0.3180(4) 0.5055(3) 0.1933(3) 0.0249(7) Uani 1 1 d . . . . .
C10 C 0.2276(4) 0.7276(3) 0.5106(3) 0.0276(7) Uani 1 1 d . . . . .
H10A H 0.246724 0.695048 0.570513 0.041 Uiso 1 1 calc R U . . .
H10B H 0.109699 0.709734 0.482539 0.041 Uiso 1 1 calc R U . . .
H10C H 0.252219 0.821178 0.546477 0.041 Uiso 1 1 calc R U . . .
C11 C 0.2167(4) 0.4372(3) 0.0808(3) 0.0316(8) Uani 1 1 d . . . . .
H11A H 0.271572 0.450290 0.016071 0.047 Uiso 1 1 calc R U . . .
H11B H 0.103511 0.471761 0.092011 0.047 Uiso 1 1 calc R U . . .
H11C H 0.208272 0.344558 0.059923 0.047 Uiso 1 1 calc R U . . .
C12 C 0.8434(4) 0.7918(3) 0.2907(3) 0.0225(6) Uani 1 1 d . . . . .
C13 C 0.9609(4) 0.8938(3) 0.3175(3) 0.0244(7) Uani 1 1 d . . . . .
C14 C 0.9317(4) 0.9819(3) 0.2701(3) 0.0293(7) Uani 1 1 d . . . . .
H14 H 1.009641 1.052424 0.286553 0.035 Uiso 1 1 calc R U . . .
C15 C 0.7887(5) 0.9667(3) 0.1989(3) 0.0314(8) Uani 1 1 d . . . . .
H15 H 0.770650 1.027737 0.167848 0.038 Uiso 1 1 calc R U . . .
C16 C 0.6718(4) 0.8647(3) 0.1721(3) 0.0291(7) Uani 1 1 d . . . . .
H16 H 0.574160 0.855427 0.123932 0.035 Uiso 1 1 calc R U . . .
C17 C 0.7032(4) 0.7770(3) 0.2184(3) 0.0231(6) Uani 1 1 d . . . . .
C18 C 1.2253(5) 0.9955(4) 0.4074(3) 0.0355(8) Uani 1 1 d . . . . .
H18A H 1.271300 0.983113 0.330150 0.053 Uiso 1 1 calc R U . . .
H18B H 1.315487 0.988816 0.458390 0.053 Uiso 1 1 calc R U . . .
H18C H 1.177342 1.081230 0.446415 0.053 Uiso 1 1 calc R U . . .
C19 C 0.7722(5) 0.2814(3) 0.0730(3) 0.0337(8) Uani 1 1 d . . . . .
H19A H 0.659657 0.248696 0.083827 0.040 Uiso 1 1 calc R U . . .
H19B H 0.858376 0.231662 0.091150 0.040 Uiso 1 1 calc R U . . .
C20 C 0.7878(6) 0.2614(4) -0.0534(4) 0.0478(10) Uani 1 1 d . . . . .
H20A H 0.773163 0.168982 -0.107087 0.072 Uiso 1 1 calc R U . . .
H20B H 0.899604 0.292946 -0.064398 0.072 Uiso 1 1 calc R U . . .
H20C H 0.700945 0.309088 -0.071970 0.072 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
Nb1 O1 1.979(2) . ?
Nb1 O2 1.981(2) . ?
Nb1 O3 1.992(2) . ?
Nb1 O4 2.000(2) . ?
Nb1 O5 1.867(2) . ?
Nb1 N1 2.232(2) . ?
Cl1 C4 1.750(3) . ?
O1 C1 1.348(4) . ?
O2 C9 1.319(4) . ?
O3 C12 1.363(4) . ?
O4 C17 1.355(4) . ?
O5 C19 1.431(4) . ?
O6 C13 1.372(4) . ?
O6 C18 1.430(4) . ?
N1 C6 1.422(4) . ?
N1 C7 1.332(4) . ?
C1 C2 1.386(5) . ?
C1 C6 1.418(4) . ?
C2 H2 0.9500 . ?
C2 C3 1.380(5) . ?
C3 H3 0.9500 . ?
C3 C4 1.389(5) . ?
C4 C5 1.380(5) . ?
C5 H5 0.9500 . ?
C5 C6 1.396(4) . ?
C7 C8 1.418(4) . ?
C7 C10 1.498(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.365(5) . ?
C9 C11 1.485(5) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.393(5) . ?
C12 C17 1.384(5) . ?
C13 C14 1.398(5) . ?
C14 H14 0.9500 . ?
C14 C15 1.393(5) . ?
C15 H15 0.9500 . ?
C15 C16 1.390(5) . ?
C16 H16 0.9500 . ?
C16 C17 1.387(5) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.490(6) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?

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 Nb1 O2 115.20(9) . . ?
O1 Nb1 O3 83.98(9) . . ?
O1 Nb1 O4 153.74(9) . . ?
O1 Nb1 N1 74.32(9) . . ?
O2 Nb1 O3 157.73(9) . . ?
O2 Nb1 O4 81.67(9) . . ?
O2 Nb1 N1 79.90(9) . . ?
O3 Nb1 O4 76.49(9) . . ?
O3 Nb1 N1 95.70(9) . . ?
O4 Nb1 N1 90.15(9) . . ?
O5 Nb1 O1 93.13(10) . . ?
O5 Nb1 O2 87.30(10) . . ?
O5 Nb1 O3 103.57(9) . . ?
O5 Nb1 O4 108.30(10) . . ?
O5 Nb1 N1 155.83(10) . . ?
C1 O1 Nb1 117.45(18) . . ?
C9 O2 Nb1 128.7(2) . . ?
C12 O3 Nb1 117.86(19) . . ?
C17 O4 Nb1 118.46(19) . . ?
C19 O5 Nb1 142.2(2) . . ?
C13 O6 C18 116.8(3) . . ?
C6 N1 Nb1 109.43(19) . . ?
C7 N1 Nb1 125.4(2) . . ?
C7 N1 C6 124.9(3) . . ?
O1 C1 C2 121.9(3) . . ?
O1 C1 C6 116.9(3) . . ?
C2 C1 C6 121.2(3) . . ?
C1 C2 H2 120.1 . . ?
C3 C2 C1 119.7(3) . . ?
C3 C2 H2 120.1 . . ?
C2 C3 H3 120.5 . . ?
C2 C3 C4 119.0(3) . . ?
C4 C3 H3 120.5 . . ?
C3 C4 Cl1 118.4(3) . . ?
C5 C4 Cl1 119.0(3) . . ?
C5 C4 C3 122.6(3) . . ?
C4 C5 H5 120.5 . . ?
C4 C5 C6 118.9(3) . . ?
C6 C5 H5 120.5 . . ?
C1 C6 N1 111.6(3) . . ?
C5 C6 N1 129.8(3) . . ?
C5 C6 C1 118.5(3) . . ?
N1 C7 C8 120.6(3) . . ?
N1 C7 C10 123.5(3) . . ?
C8 C7 C10 115.8(3) . . ?
C7 C8 H8 117.2 . . ?
C9 C8 C7 125.6(3) . . ?
C9 C8 H8 117.2 . . ?
O2 C9 C8 121.6(3) . . ?
O2 C9 C11 114.9(3) . . ?
C8 C9 C11 123.5(3) . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O3 C12 C13 124.7(3) . . ?
O3 C12 C17 114.0(3) . . ?
C17 C12 C13 121.2(3) . . ?
O6 C13 C12 116.5(3) . . ?
O6 C13 C14 125.7(3) . . ?
C12 C13 C14 117.8(3) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 C13 120.2(3) . . ?
C15 C14 H14 119.9 . . ?
C14 C15 H15 119.0 . . ?
C16 C15 C14 121.9(3) . . ?
C16 C15 H15 119.0 . . ?
C15 C16 H16 121.3 . . ?
C17 C16 C15 117.4(3) . . ?
C17 C16 H16 121.3 . . ?
O4 C17 C12 113.1(3) . . ?
O4 C17 C16 125.4(3) . . ?
C12 C17 C16 121.5(3) . . ?
O6 C18 H18A 109.5 . . ?
O6 C18 H18B 109.5 . . ?
O6 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O5 C19 H19A 109.5 . . ?
O5 C19 H19B 109.5 . . ?
O5 C19 C20 110.9(3) . . ?
H19A C19 H19B 108.0 . . ?
C20 C19 H19A 109.5 . . ?
C20 C19 H19B 109.5 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?

_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 1.730
_oxdiff_exptl_absorpt_empirical_full_min 0.408
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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_I-4
_database_code_depnum_ccdc_archive 'CCDC 2331120'
loop_
_audit_author_name
_audit_author_address
'Christopher Durr'
;Amherst College
United States of America
;
_audit_update_record             
;
2024-02-05 deposited with the CCDC.	2024-03-19 downloaded from the CCDC.
;
_audit_creation_date             2022-05-02
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C17 H25 Cl N O5 Ta'
_chemical_formula_sum            'C17 H25 Cl N O5 Ta'
_chemical_formula_weight         539.78
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Ta N O C H Cl'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ta Ta -5.7959 5.2718 '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           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   13.50190(10)
_cell_length_b                   13.0675(2)
_cell_length_c                   22.1817(2)
_cell_angle_alpha                90
_cell_angle_beta                 94.0280(10)
_cell_angle_gamma                90
_cell_volume                     3903.99(8)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    42002
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      68.0430
_cell_measurement_theta_min      3.8780
_shelx_estimated_absorpt_T_max   0.654
_shelx_estimated_absorpt_T_min   0.271
_exptl_absorpt_coefficient_mu    11.881
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.28072
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.110a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.837
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2112
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -8 -4 0.0306
0 2 -14 0.0180
0 6 10 0.0175
0 -3 14 0.0204
0 -8 1 0.0341
-9 0 -1 0.0739
0 8 -1 0.0189
9 0 1 0.0701

_exptl_crystal_size_max          0.149
_exptl_crystal_size_mid          0.051
_exptl_crystal_size_min          0.039
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.1651 -8.0857 -4.3709 0.0067 0.3798 0.9250
0.0955 2.0964 -13.9306 0.0245 0.9454 -0.3249
-0.1861 5.9726 10.2191 -0.0171 -0.7650 -0.6438
-0.0860 -2.5757 13.6976 -0.0242 -0.9247 0.3799
0.0162 -8.4618 1.1109 0.0090 0.0039 1.0000
-8.6945 -0.1007 -0.7200 0.9968 0.0797 -0.0093
-0.0162 8.4618 -1.1109 -0.0090 -0.0039 -1.0000
8.6918 -0.1279 0.7497 -0.9962 -0.0796 0.0363

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_av_unetI/netI     0.0226
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            64517
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.343
_diffrn_reflns_theta_min         3.720
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -35.00  31.00   0.50    1.00    --   41.95  -6.00 171.00  132
  2  ω   -119.00  15.00   0.50    1.00    --  -42.26  -6.00 171.00  268
  3  ω    -31.00  34.00   0.50    1.00    --  -42.26   6.00 -12.00  130
  4  ω     25.00 170.00   0.50    4.00    --   93.72   6.00 -12.00  290
  5  ω   -171.00 -37.00   0.50    4.00    --  -94.03  -6.00 171.00  268
  6  ω    -27.00 119.00   0.50    1.00    --   41.95   6.00 -12.00  292
  7  ω     22.00  50.00   0.50    1.00    --   41.95  60.00-164.76   56
  8  ω     22.00  53.00   0.50    1.00    --   41.95  59.00 124.55   62
  9  ω     21.00  48.00   0.50    1.00    --   41.95  61.00 130.72   54
 10  ω     22.00  50.00   0.50    1.00    --   41.95  60.00  45.43   56
 11  ω     21.00  48.00   0.50    1.00    --   41.95  61.00  75.53   54
 12  ω     22.00  53.00   0.50    1.00    --   41.95  59.00-173.76   62
 13  ω    -24.00  37.00   0.50    1.00    --   41.95 -32.00 -60.00  122
 14  ω     22.00  50.00   0.50    1.00    --   41.95  60.00 115.84   56
 15  ω     31.00 108.00   0.50    1.00    --   41.95  32.00  60.00  154
 16  ω     19.00  99.00   0.50    1.00    --   41.95-138.00  90.00  160
 17  ω     22.00  50.00   0.50    1.00    --   41.95  60.00  95.89   56
 18  ω     21.00  48.00   0.50    1.00    --   41.95  61.00 104.72   54
 19  ω     21.00  48.00   0.50    1.00    --   41.95  61.00 -17.61   54
 20  ω     21.00  48.00   0.50    1.00    --   41.95  61.00-175.99   54
 21  ω     22.00  53.00   0.50    1.00    --   41.95  59.00 177.15   62
 22  ω     22.00  56.00   0.50    1.00    --   41.95  58.00  65.16   68
 23  ω    -23.00  48.00   0.50    1.00    --   41.95 -43.00 -60.00  142
 24  ω     21.00  48.00   0.50    1.00    --   41.95  61.00  -9.54   54
 25  ω     22.00  50.00   0.50    1.00    --   41.95  60.00-152.37   56
 26  ω     21.00  48.00   0.50    1.00    --   41.95  61.00 102.48   54
 27  ω     23.00 108.00   0.50    1.00    --   41.95  54.00-120.00  170
 28  ω     22.00  53.00   0.50    1.00    --   41.95  59.00 160.14   62
 29  ω     21.00  48.00   0.50    1.00    --   41.95  61.00-143.70   54
 30  ω    -28.00  28.00   0.50    1.00    --   41.95 -21.00-120.00  112
 31  ω     22.00  53.00   0.50    1.00    --   41.95  59.00  79.44   62
 32  ω    -79.00   4.00   0.50    1.00    --  -42.26 104.00 -30.00  166
 33  ω    -50.00 -25.00   0.50    1.00    --  -42.26 -60.00 113.12   50
 34  ω    -50.00 -25.00   0.50    1.00    --  -42.26 -60.00 135.77   50
 35  ω    -47.00  13.00   0.50    1.00    --  -42.26  43.00 120.00  120
 36  ω   -109.00 -81.00   0.50    1.00    --  -42.26-138.00 -30.00   56
 37  ω    -49.00  15.00   0.50    1.00    --  -42.26  -6.00 171.00  128
 38  ω    -50.00 -24.00   0.50    1.00    --  -42.26 -57.00  -1.05   52
 39  ω    -64.00 -29.00   0.50    1.00    --  -42.26 -21.00 120.00   70
 40  ω    -98.00 -73.00   0.50    1.00    --  -42.26 -21.00 120.00   50
 41  ω    -47.00 -22.00   0.50    1.00    --  -42.26 -61.00  51.64   50
 42  ω    -48.00 -22.00   0.50    1.00    --  -42.26 -60.00  63.74   52
 43  ω     28.00  57.00   0.50    4.00    --   93.72 -50.00-150.00   58
 44  ω     77.00 103.00   0.50    4.00    --   93.72  50.00 120.00   52
 45  ω     77.00 103.00   0.50    4.00    --   93.72  50.00  90.00   52
 46  ω     26.00  83.00   0.50    4.00    --   93.72 -68.00 150.00  114
 47  ω     76.00 102.00   0.50    4.00    --   93.72  53.00 135.95   52
 48  ω     76.00 102.00   0.50    4.00    --   93.72  50.00  60.00   52
 49  ω     28.00  57.00   0.50    4.00    --   93.72 -50.00-120.00   58
 50  ω     28.00 105.00   0.50    4.00    --   93.72 -77.00 -60.00  154
 51  ω    -53.00 -28.00   0.50    4.00    --  -94.03  59.00  60.00   50
 52  ω   -154.00-110.00   0.50    4.00    --  -94.03 -54.00  68.52   88
 53  ω   -102.00 -76.00   0.50    4.00    --  -94.03 -53.00  79.44   52
 54  ω    -83.00 -37.00   0.50    4.00    --  -94.03  68.00  90.00   92
 55  ω   -104.00 -75.00   0.50    4.00    --  -94.03 -54.00  12.81   58
 56  ω   -157.00-131.00   0.50    4.00    --  -94.03 -53.00  79.44   52
 57  ω   -159.00-133.00   0.50    4.00    --  -94.03 -54.00  12.81   52
 58  ω   -103.00 -75.00   0.50    4.00    --  -94.03 -54.00 117.80   56
 59  ω   -101.00 -75.00   0.50    4.00    --  -94.03 -55.00  21.88   52
 60  ω   -102.00 -76.00   0.50    4.00    --  -94.03 -55.00  41.90   52
 61  ω   -100.00 -75.00   0.50    4.00    --  -94.03 -54.00  68.52   50
 62  ω   -102.00 -76.00   0.50    4.00    --  -94.03 -56.00 -24.20   52
 63  ω   -102.00 -76.00   0.50    4.00    --  -94.03 -53.00  13.82   52
 64  ω   -100.00 -75.00   0.50    4.00    --  -94.03 -55.00  35.02   50
 65  ω   -153.00-127.00   0.50    4.00    --  -94.03 -55.00  41.90   52
 66  ω   -155.00 -77.00   0.50    4.00    --  -94.03 -50.00  60.00  156
 67  ω    -82.00 -33.00   0.50    4.00    --  -94.03 117.00-120.00   98
 68  ω   -101.00 -75.00   0.50    4.00    --  -94.03 -55.00 138.52   52
 69  ω    -61.00 -29.00   0.50    4.00    --  -94.03 117.00  90.00   64
 70  ω   -100.00 -75.00   0.50    4.00    --  -94.03 -54.00 125.27   50
 71  ω   -108.00 -70.00   0.50    4.00    --  -94.03 117.00  90.00   76
 72  ω   -102.00 -76.00   0.50    4.00    --  -94.03 -52.00  86.17   52
 73  ω   -160.00-135.00   0.50    4.00    --  -94.03 -54.00 125.27   50
 74  ω   -160.00 -75.00   0.50    4.00    --  -94.03 -55.00 105.24  170
 75  ω   -157.00-118.00   0.50    4.00    --  -94.03 -52.00  86.17   78
 76  ω   -114.00 -76.00   0.50    4.00    --  -94.03 -51.00 148.09   76
 77  ω   -160.00 -75.00   0.50    4.00    --  -94.03 -55.00  54.04  170
 78  ω   -159.00-133.00   0.50    4.00    --  -94.03 -51.00 148.09   52
 79  ω   -113.00 -76.00   0.50    4.00    --  -94.03 -56.00  -8.34   74
 80  ω    -57.00 -32.00   0.50    4.00    --  -94.03  50.00  30.00   50
 81  ω   -102.00 -76.00   0.50    4.00    --  -94.03 -54.00   2.21   52
 82  ω   -157.00-131.00   0.50    4.00    --  -94.03 -54.00   2.21   52
 83  ω   -156.00-116.00   0.50    4.00    --  -94.03 -56.00  -8.34   80
 84  ω    -62.00 -26.00   0.50    4.00    --  -94.03  96.00  90.00   72
 85  ω   -106.00 -66.00   0.50    4.00    --  -94.03  96.00  90.00   80
 86  ω    -58.00 -29.00   0.50    4.00    --  -94.03 117.00 -30.00   58
 87  ω   -103.00 -77.00   0.50    4.00    --  -94.03 -53.00   5.12   52
 88  ω   -134.00 -75.00   0.50    4.00    --  -94.03 -54.00 141.32  118
 89  ω   -160.00 -77.00   0.50    4.00    --  -94.03 -54.00 133.25  166
 90  ω   -101.00 -75.00   0.50    4.00    --  -94.03 -55.00  -3.18   52
 91  ω   -103.00 -77.00   0.50    4.00    --  -94.03 -56.00  50.74   52
 92  ω   -101.00 -75.00   0.50    4.00    --  -94.03 117.00 -30.00   52
 93  ω   -115.00 -77.00   0.50    4.00    --  -94.03 -49.00  51.09   76
 94  ω   -103.00 -77.00   0.50    4.00    --  -94.03 -50.00  90.00   52
 95  ω   -102.00 -76.00   0.50    4.00    --  -94.03 -52.00  80.06   52
 96  ω   -103.00 -77.00   0.50    4.00    --  -94.03 -53.00 113.40   52
 97  ω   -103.00 -77.00   0.50    4.00    --  -94.03 -51.00  83.39   52
 98  ω   -103.00 -77.00   0.50    4.00    --  -94.03 -53.00 109.29   52
 99  ω   -100.00 -75.00   0.50    4.00    --  -94.03 -55.00  26.65   50
100  ω   -159.00 -75.00   0.50    4.00    --  -94.03 -54.00 -19.82  168
101  ω   -160.00-107.00   0.50    4.00    --  -94.03 -55.00  21.88  106
102  ω    -56.00 -30.00   0.50    4.00    --  -94.03  50.00 -90.00   52
103  ω   -101.00 -75.00   0.50    4.00    --  -94.03 -55.00  23.92   52
104  ω   -100.00 -75.00   0.50    4.00    --  -94.03 -55.00  -7.88   50
105  ω   -101.00 -75.00   0.50    4.00    --  -94.03 -55.00 146.35   52
106  ω    -55.00 -28.00   0.50    4.00    --  -94.03  50.00-120.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at home/near, HyPix3000'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1143935000
_diffrn_orient_matrix_UB_12      -0.0016511000
_diffrn_orient_matrix_UB_13      -0.0027940000
_diffrn_orient_matrix_UB_21      -0.0033139000
_diffrn_orient_matrix_UB_22      -0.0095651000
_diffrn_orient_matrix_UB_23      -0.0693292000
_diffrn_orient_matrix_UB_31      0.0019597000
_diffrn_orient_matrix_UB_32      -0.1174257000
_diffrn_orient_matrix_UB_33      0.0056649000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6356
_reflns_number_total             7080
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.65
_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 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         1.067
_refine_diff_density_min         -1.018
_refine_diff_density_rms         0.094
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         7080
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0252
_refine_ls_R_factor_gt           0.0213
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0285P)²+3.3652P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0525
_refine_ls_wR_factor_ref         0.0541
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C29(H29A,H29B), C12(H12A,H12B), C33(H33A,H33B), C31(H31A,
 H31B), C16(H16A,H16B)
2.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C25(H25), C5(H5), C20(H20), C19(H19), C2(H2), C22(H22), C3(H3)
2.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C30(H30A,H30B,H30C), C10(H10A,H10B,H10C), C28(H28A,H28B,
 H28C), C11(H11A,H11B,H11C), C34(H34A,H34B,H34C), C15(H15A,H15B,H15C), C13(H13A,
 H13B,H13C), C17(H17A,H17B,H17C), C32(H32A,H32B,H32C)
;
_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
Ta1 Ta 0.32339(2) 0.39492(2) 0.35466(2) 0.01342(5) Uani 1 1 d . . . . .
Ta2 Ta 0.82405(2) 0.68811(2) 0.35975(2) 0.01486(5) Uani 1 1 d . . . . .
Cl2 Cl 0.65305(6) 0.69193(7) 0.05414(3) 0.03008(18) Uani 1 1 d . . . . .
Cl1 Cl 0.15674(6) 0.41885(7) 0.04857(3) 0.03180(18) Uani 1 1 d . . . . .
O1 O 0.39017(13) 0.37518(16) 0.27894(8) 0.0165(4) Uani 1 1 d . . . . .
O7 O 0.71794(13) 0.63468(16) 0.41059(8) 0.0177(4) Uani 1 1 d . . . . .
O6 O 0.89037(13) 0.71432(16) 0.28431(8) 0.0179(4) Uani 1 1 d . . . . .
O4 O 0.41254(14) 0.31248(16) 0.40403(8) 0.0192(4) Uani 1 1 d . . . . .
O3 O 0.23554(13) 0.28083(16) 0.34005(8) 0.0181(4) Uani 1 1 d . . . . .
O2 O 0.21721(13) 0.44465(16) 0.40706(8) 0.0177(4) Uani 1 1 d . . . . .
O8 O 0.88531(13) 0.55969(16) 0.37247(8) 0.0187(4) Uani 1 1 d . . . . .
O10 O 0.73895(14) 0.80515(16) 0.34923(8) 0.0189(4) Uani 1 1 d . . . . .
O5 O 0.38619(14) 0.52068(16) 0.37398(8) 0.0189(4) Uani 1 1 d . . . . .
O9 O 0.91504(14) 0.76298(17) 0.41219(9) 0.0238(5) Uani 1 1 d . . . . .
N1 N 0.22345(16) 0.47312(19) 0.28159(10) 0.0151(5) Uani 1 1 d . . . . .
N2 N 0.72248(16) 0.61686(18) 0.28458(10) 0.0147(5) Uani 1 1 d . . . . .
C6 C 0.24831(19) 0.4405(2) 0.22331(12) 0.0157(6) Uani 1 1 d . . . . .
C8 C 0.13039(19) 0.5720(2) 0.34970(12) 0.0178(6) Uani 1 1 d . . . . .
H8 H 0.088379 0.629951 0.352304 0.021 Uiso 1 1 calc R U . . .
C14 C 0.4145(2) 0.2078(2) 0.42234(12) 0.0185(6) Uani 1 1 d . . . . .
H14A H 0.470713 0.172402 0.404875 0.022 Uiso 1 1 calc R U . . .
H14B H 0.352279 0.173645 0.407106 0.022 Uiso 1 1 calc R U . . .
C18 C 0.8417(2) 0.7019(2) 0.22948(12) 0.0168(6) Uani 1 1 d . . . . .
C9 C 0.15529(18) 0.5223(2) 0.40258(12) 0.0164(6) Uani 1 1 d . . . . .
C25 C 0.63080(19) 0.5114(2) 0.34997(12) 0.0172(6) Uani 1 1 d . . . . .
H25 H 0.588093 0.453799 0.351032 0.021 Uiso 1 1 calc R U . . .
C1 C 0.3407(2) 0.3900(2) 0.22456(12) 0.0175(6) Uani 1 1 d . . . . .
C23 C 0.7482(2) 0.6528(2) 0.22723(12) 0.0157(6) Uani 1 1 d . . . . .
C26 C 0.65743(19) 0.5559(2) 0.40414(12) 0.0166(6) Uani 1 1 d . . . . .
C7 C 0.15985(19) 0.5475(2) 0.29077(12) 0.0154(6) Uani 1 1 d . . . . .
C24 C 0.65935(18) 0.5411(2) 0.29159(12) 0.0142(5) Uani 1 1 d . . . . .
C4 C 0.2303(2) 0.4101(2) 0.11649(12) 0.0217(6) Uani 1 1 d . . . . .
C5 C 0.1920(2) 0.4473(2) 0.16855(12) 0.0189(6) Uani 1 1 d . . . . .
H5 H 0.127791 0.477323 0.166815 0.023 Uiso 1 1 calc R U . . .
C27 C 0.6147(2) 0.4766(2) 0.24007(12) 0.0186(6) Uani 1 1 d . . . . .
H27A H 0.553242 0.508492 0.223187 0.028 Uiso 1 1 calc R U . . .
H27B H 0.600139 0.408002 0.255020 0.028 Uiso 1 1 calc R U . . .
H27C H 0.661926 0.471297 0.208598 0.028 Uiso 1 1 calc R U . . .
C20 C 0.8245(2) 0.7320(2) 0.12192(13) 0.0221(6) Uani 1 1 d . . . . .
H20 H 0.850739 0.755619 0.085805 0.027 Uiso 1 1 calc R U . . .
C19 C 0.8804(2) 0.7373(2) 0.17725(13) 0.0203(6) Uani 1 1 d . . . . .
H19 H 0.945496 0.765323 0.179027 0.024 Uiso 1 1 calc R U . . .
C21 C 0.7296(2) 0.6913(2) 0.12121(13) 0.0218(6) Uani 1 1 d . . . . .
C29 C 0.8915(2) 0.4523(2) 0.37317(13) 0.0216(6) Uani 1 1 d . . . . .
H29A H 0.832224 0.423664 0.390943 0.026 Uiso 1 1 calc R U . . .
H29B H 0.950896 0.430936 0.398763 0.026 Uiso 1 1 calc R U . . .
C2 C 0.3790(2) 0.3558(2) 0.17201(12) 0.0195(6) Uani 1 1 d . . . . .
H2 H 0.443211 0.325836 0.173413 0.023 Uiso 1 1 calc R U . . .
C30 C 0.8979(2) 0.4106(3) 0.31006(13) 0.0236(7) Uani 1 1 d . . . . .
H30A H 0.836669 0.427090 0.285595 0.035 Uiso 1 1 calc R U . . .
H30B H 0.906407 0.336196 0.311918 0.035 Uiso 1 1 calc R U . . .
H30C H 0.954645 0.441544 0.291720 0.035 Uiso 1 1 calc R U . . .
C22 C 0.6907(2) 0.6517(2) 0.17263(12) 0.0183(6) Uani 1 1 d . . . . .
H22 H 0.625449 0.624098 0.170554 0.022 Uiso 1 1 calc R U . . .
C10 C 0.1141(2) 0.6150(2) 0.24107(12) 0.0197(6) Uani 1 1 d . . . . .
H10A H 0.162515 0.627069 0.210938 0.029 Uiso 1 1 calc R U . . .
H10B H 0.094792 0.680583 0.258246 0.029 Uiso 1 1 calc R U . . .
H10C H 0.055271 0.581310 0.221785 0.029 Uiso 1 1 calc R U . . .
C3 C 0.3233(2) 0.3653(3) 0.11699(13) 0.0220(6) Uani 1 1 d . . . . .
H3 H 0.348643 0.341558 0.080619 0.026 Uiso 1 1 calc R U . . .
C12 C 0.1323(2) 0.2608(3) 0.33847(15) 0.0274(7) Uani 1 1 d . . . . .
H12A H 0.098992 0.290286 0.301272 0.033 Uiso 1 1 calc R U . . .
H12B H 0.103849 0.293193 0.373702 0.033 Uiso 1 1 calc R U . . .
C28 C 0.6189(2) 0.5173(3) 0.46164(12) 0.0215(6) Uani 1 1 d . . . . .
H28A H 0.672796 0.483820 0.486118 0.032 Uiso 1 1 calc R U . . .
H28B H 0.565335 0.468086 0.452168 0.032 Uiso 1 1 calc R U . . .
H28C H 0.593416 0.574911 0.484256 0.032 Uiso 1 1 calc R U . . .
C33 C 0.6374(2) 0.8312(2) 0.34928(13) 0.0204(6) Uani 1 1 d . . . . .
H33A H 0.604900 0.786467 0.378025 0.024 Uiso 1 1 calc R U . . .
H33B H 0.604752 0.819684 0.308483 0.024 Uiso 1 1 calc R U . . .
C31 C 0.9171(2) 0.8653(3) 0.43519(15) 0.0305(7) Uani 1 1 d . . . . .
H31A H 0.876681 0.910188 0.407176 0.037 Uiso 1 1 calc R U . . .
H31B H 0.986207 0.891132 0.437763 0.037 Uiso 1 1 calc R U . . .
C11 C 0.1130(2) 0.5523(3) 0.46063(12) 0.0238(7) Uani 1 1 d . . . . .
H11A H 0.097431 0.490607 0.483234 0.036 Uiso 1 1 calc R U . . .
H11B H 0.052251 0.592256 0.451864 0.036 Uiso 1 1 calc R U . . .
H11C H 0.161578 0.593673 0.484783 0.036 Uiso 1 1 calc R U . . .
C16 C 0.3919(2) 0.6258(2) 0.38716(14) 0.0241(7) Uani 1 1 d . . . . .
H16A H 0.451581 0.639194 0.414555 0.029 Uiso 1 1 calc R U . . .
H16B H 0.332890 0.646499 0.408262 0.029 Uiso 1 1 calc R U . . .
C34 C 0.6250(2) 0.9411(3) 0.36698(15) 0.0294(7) Uani 1 1 d . . . . .
H34A H 0.651859 0.985568 0.336520 0.044 Uiso 1 1 calc R U . . .
H34B H 0.660682 0.953453 0.406312 0.044 Uiso 1 1 calc R U . . .
H34C H 0.554299 0.955996 0.369664 0.044 Uiso 1 1 calc R U . . .
C15 C 0.4257(3) 0.2005(3) 0.49025(13) 0.0304(8) Uani 1 1 d . . . . .
H15A H 0.427471 0.128358 0.502346 0.046 Uiso 1 1 calc R U . . .
H15B H 0.369411 0.234442 0.507390 0.046 Uiso 1 1 calc R U . . .
H15C H 0.487628 0.233968 0.505192 0.046 Uiso 1 1 calc R U . . .
C13 C 0.1146(2) 0.1467(3) 0.33975(19) 0.0384(9) Uani 1 1 d . . . . .
H13A H 0.136096 0.115860 0.302556 0.058 Uiso 1 1 calc R U . . .
H13B H 0.043742 0.133331 0.342818 0.058 Uiso 1 1 calc R U . . .
H13C H 0.152597 0.116811 0.374707 0.058 Uiso 1 1 calc R U . . .
C17 C 0.3972(3) 0.6887(3) 0.33052(17) 0.0354(8) Uani 1 1 d . . . . .
H17A H 0.450149 0.662284 0.306826 0.053 Uiso 1 1 calc R U . . .
H17B H 0.411136 0.760197 0.341446 0.053 Uiso 1 1 calc R U . . .
H17C H 0.333565 0.684594 0.306458 0.053 Uiso 1 1 calc R U . . .
C32 C 0.8775(3) 0.8689(4) 0.49608(17) 0.0460(10) Uani 1 1 d . . . . .
H32A H 0.808946 0.843905 0.493441 0.069 Uiso 1 1 calc R U . . .
H32B H 0.879196 0.939574 0.510910 0.069 Uiso 1 1 calc R U . . .
H32C H 0.918429 0.825611 0.524001 0.069 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
Ta1 O1 1.9782(18) . ?
Ta1 O4 1.9035(19) . ?
Ta1 O3 1.919(2) . ?
Ta1 O2 2.0157(18) . ?
Ta1 O5 1.885(2) . ?
Ta1 N1 2.277(2) . ?
Ta2 O7 2.0097(18) . ?
Ta2 O6 1.9824(18) . ?
Ta2 O8 1.883(2) . ?
Ta2 O10 1.917(2) . ?
Ta2 O9 1.902(2) . ?
Ta2 N2 2.282(2) . ?
Cl2 C21 1.751(3) . ?
Cl1 C4 1.749(3) . ?
O1 C1 1.351(3) . ?
O7 C26 1.316(4) . ?
O6 C18 1.351(3) . ?
O4 C14 1.427(4) . ?
O3 C12 1.416(3) . ?
O2 C9 1.314(3) . ?
O8 C29 1.406(4) . ?
O10 C33 1.412(3) . ?
O5 C16 1.405(4) . ?
O9 C31 1.431(4) . ?
N1 C6 1.424(3) . ?
N1 C7 1.322(4) . ?
N2 C23 1.422(3) . ?
N2 C24 1.323(4) . ?
C6 C1 1.410(4) . ?
C6 C5 1.390(4) . ?
C8 C9 1.362(4) . ?
C8 C7 1.429(4) . ?
C14 C15 1.506(4) . ?
C18 C23 1.414(4) . ?
C18 C19 1.384(4) . ?
C9 C11 1.497(4) . ?
C25 C26 1.360(4) . ?
C25 C24 1.430(4) . ?
C1 C2 1.382(4) . ?
C23 C22 1.392(4) . ?
C26 C28 1.498(4) . ?
C7 C10 1.510(4) . ?
C24 C27 1.511(4) . ?
C4 C5 1.386(4) . ?
C4 C3 1.386(4) . ?
C20 C19 1.397(4) . ?
C20 C21 1.386(4) . ?
C21 C22 1.389(4) . ?
C29 C30 1.510(4) . ?
C2 C3 1.393(4) . ?
C12 C13 1.510(5) . ?
C33 C34 1.502(5) . ?
C31 C32 1.488(5) . ?
C16 C17 1.507(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
O1 Ta1 O2 156.45(8) . . ?
O1 Ta1 N1 74.74(8) . . ?
O4 Ta1 O1 96.15(8) . . ?
O4 Ta1 O3 90.91(8) . . ?
O4 Ta1 O2 107.30(8) . . ?
O4 Ta1 N1 169.31(8) . . ?
O3 Ta1 O1 93.93(8) . . ?
O3 Ta1 O2 83.77(8) . . ?
O3 Ta1 N1 84.26(8) . . ?
O2 Ta1 N1 81.71(7) . . ?
O5 Ta1 O1 94.72(8) . . ?
O5 Ta1 O4 96.11(8) . . ?
O5 Ta1 O3 168.22(8) . . ?
O5 Ta1 O2 85.10(8) . . ?
O5 Ta1 N1 90.30(8) . . ?
O7 Ta2 N2 81.53(8) . . ?
O6 Ta2 O7 156.31(8) . . ?
O6 Ta2 N2 74.79(8) . . ?
O8 Ta2 O7 85.94(8) . . ?
O8 Ta2 O6 93.48(8) . . ?
O8 Ta2 O10 169.15(8) . . ?
O8 Ta2 O9 96.24(9) . . ?
O8 Ta2 N2 88.91(8) . . ?
O10 Ta2 O7 84.30(8) . . ?
O10 Ta2 O6 93.54(8) . . ?
O10 Ta2 N2 84.96(8) . . ?
O9 Ta2 O7 106.91(8) . . ?
O9 Ta2 O6 96.71(8) . . ?
O9 Ta2 O10 91.14(9) . . ?
O9 Ta2 N2 170.36(9) . . ?
C1 O1 Ta1 120.87(16) . . ?
C26 O7 Ta2 132.26(17) . . ?
C18 O6 Ta2 121.28(16) . . ?
C14 O4 Ta1 134.83(17) . . ?
C12 O3 Ta1 138.05(19) . . ?
C9 O2 Ta1 132.83(17) . . ?
C29 O8 Ta2 156.37(18) . . ?
C33 O10 Ta2 139.93(19) . . ?
C16 O5 Ta1 156.47(18) . . ?
C31 O9 Ta2 133.97(19) . . ?
C6 N1 Ta1 110.25(17) . . ?
C7 N1 Ta1 125.39(17) . . ?
C7 N1 C6 123.9(2) . . ?
C23 N2 Ta2 110.32(17) . . ?
C24 N2 Ta2 125.37(18) . . ?
C24 N2 C23 123.5(2) . . ?
C1 C6 N1 112.8(2) . . ?
C5 C6 N1 128.7(2) . . ?
C5 C6 C1 118.4(3) . . ?
C9 C8 C7 127.8(3) . . ?
O4 C14 C15 110.1(2) . . ?
O6 C18 C23 117.6(2) . . ?
O6 C18 C19 121.7(3) . . ?
C19 C18 C23 120.7(3) . . ?
O2 C9 C8 123.4(2) . . ?
O2 C9 C11 114.6(2) . . ?
C8 C9 C11 122.0(3) . . ?
C26 C25 C24 127.8(3) . . ?
O1 C1 C6 117.8(2) . . ?
O1 C1 C2 121.1(2) . . ?
C2 C1 C6 121.2(3) . . ?
C18 C23 N2 113.1(2) . . ?
C22 C23 N2 128.3(2) . . ?
C22 C23 C18 118.5(3) . . ?
O7 C26 C25 123.6(2) . . ?
O7 C26 C28 114.9(2) . . ?
C25 C26 C28 121.5(3) . . ?
N1 C7 C8 122.1(3) . . ?
N1 C7 C10 123.6(2) . . ?
C8 C7 C10 114.3(2) . . ?
N2 C24 C25 121.7(2) . . ?
N2 C24 C27 123.7(2) . . ?
C25 C24 C27 114.5(2) . . ?
C5 C4 Cl1 118.2(2) . . ?
C5 C4 C3 122.2(3) . . ?
C3 C4 Cl1 119.6(2) . . ?
C4 C5 C6 119.5(3) . . ?
C21 C20 C19 118.1(3) . . ?
C18 C19 C20 120.4(3) . . ?
C20 C21 Cl2 119.9(2) . . ?
C20 C21 C22 122.4(3) . . ?
C22 C21 Cl2 117.7(2) . . ?
O8 C29 C30 110.9(2) . . ?
C1 C2 C3 120.0(3) . . ?
C21 C22 C23 119.4(3) . . ?
C4 C3 C2 118.5(3) . . ?
O3 C12 C13 109.8(3) . . ?
O10 C33 C34 110.9(2) . . ?
O9 C31 C32 110.7(3) . . ?
O5 C16 C17 111.4(3) . . ?

_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 3.260
_oxdiff_exptl_absorpt_empirical_full_min 0.626
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
