#------------------------------------------------------------------------------
#$Date: 2024-05-05 05:52:41 +0300 (Sun, 05 May 2024) $
#$Revision: 291629 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/56/7715604.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7715604
loop_
_publ_author_name
'Peprah, Frank'
'Tarantola, Grace E.'
'Plaman, Alyson S.'
'Vu, Emily L.'
'Huynh, Alyssa B.'
'Durr, Christopher B.'
_publ_section_title
;
 Synthesis and catalytic activity of single-site group V alkoxide
 complexes for the ring-opening polymerization of ε-caprolactone.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7073
_journal_page_last               7080
_journal_paper_doi               10.1039/d4dt00422a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C17 H25 Cl N Nb O5'
_chemical_formula_sum            'C17 H25 Cl N Nb O5'
_chemical_formula_weight         451.74
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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)
;
_audit_update_record
;
2024-02-05 deposited with the CCDC.	2024-03-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.0660(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.4876(2)
_cell_length_b                   13.0436(2)
_cell_length_c                   22.1841(3)
_cell_measurement_reflns_used    16623
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      67.9320
_cell_measurement_theta_min      3.8950
_cell_volume                     3892.96(10)
_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)'
_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_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_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_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_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_description       block
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.175
_exptl_crystal_size_mid          0.145
_exptl_crystal_size_min          0.056
_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_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0298
_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
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6137
_reflns_number_total             7048
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt00422a2.cif
_cod_data_source_block           I-3
_cod_depositor_comments
'Adding full bibliography for 7715601--7715608.cif.'
_cod_database_code               7715604
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C H Nb O N Cl'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.695
_shelx_estimated_absorpt_t_min   0.403
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.65
_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)
;
_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
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'
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 . . .
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'
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
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) . . ?
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_
_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
