#------------------------------------------------------------------------------
#$Date: 2024-05-05 05:52:41 +0300 (Sun, 05 May 2024) $
#$Revision: 291629 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/56/7715607.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_7715607
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         'C20 H21 Cl N Nb O6'
_chemical_formula_sum            'C20 H21 Cl N Nb O6'
_chemical_formula_weight         499.74
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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)
;
_audit_update_record
;
2024-02-05 deposited with the CCDC.	2024-03-19 downloaded from the CCDC.
;
_cell_angle_alpha                115.7499(18)
_cell_angle_beta                 90.3226(17)
_cell_angle_gamma                91.8519(16)
_cell_formula_units_Z            2
_cell_length_a                   7.93594(17)
_cell_length_b                   11.4858(2)
_cell_length_c                   12.4086(2)
_cell_measurement_reflns_used    10697
_cell_measurement_temperature    120.00(16)
_cell_measurement_theta_max      67.9160
_cell_measurement_theta_min      3.9300
_cell_volume                     1017.96(4)
_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)'
_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_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_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_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_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_description       needle
_exptl_crystal_F_000             508
_exptl_crystal_size_max          0.156
_exptl_crystal_size_mid          0.053
_exptl_crystal_size_min          0.047
_refine_diff_density_max         0.952
_refine_diff_density_min         -0.974
_refine_diff_density_rms         0.106
_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_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0340
_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
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3393
_reflns_number_total             3682
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt00422a2.cif
_cod_data_source_block           C-3OMe
_cod_depositor_comments
'Adding full bibliography for 7715601--7715608.cif.'
_cod_original_cell_volume        1017.95(4)
_cod_database_code               7715607
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Nb Cl O N C H'
_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   0.754
_shelx_estimated_absorpt_t_min   0.437
_reflns_odcompleteness_completeness 99.94
_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:
 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)
;
_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
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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 . . .
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
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
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 . . ?
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_
_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
