#------------------------------------------------------------------------------
#$Date: 2024-05-05 05:52:41 +0300 (Sun, 05 May 2024) $
#$Revision: 291629 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/56/7715601.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_7715601
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         'C18 H28 N Nb O5'
_chemical_formula_sum            'C18 H28 N Nb O5'
_chemical_formula_weight         431.32
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 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                 98.4580(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   30.4282(3)
_cell_length_b                   8.11400(10)
_cell_length_c                   15.99700(10)
_cell_measurement_reflns_used    28134
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      67.9400
_cell_measurement_theta_min      2.9270
_cell_volume                     3906.61(7)
_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 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_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_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_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_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_description       block
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.219
_exptl_crystal_size_mid          0.078
_exptl_crystal_size_min          0.06
_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_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_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0286
_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
_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_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt00422a2.cif
_cod_data_source_block           I-1
_cod_depositor_comments
'Adding full bibliography for 7715601--7715608.cif.'
_cod_database_code               7715601
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C H N O Nb'
_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   0.744
_shelx_estimated_absorpt_t_min   0.391
_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:
 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)
;
_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
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'
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 . . .
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'
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
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) . . ?
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_
_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
