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#$Date: 2025-08-21 00:01:10 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301838 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/75/4327562.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_4327562
loop_
_publ_author_name
'Maryam Tayebani'
'Khalil Feghali'
'Sandro Gambarotta'
'Glenn P. A. Yap'
_publ_section_title
;
 Insensitivity of the Nb-Nb Distance in a Paddle-Wheel Compound to Bond
 Multiplicity and Axial Ligation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1399
_journal_page_last               1401
_journal_paper_doi               10.1021/ic001110+
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C36 H36 N8 Nb2 O2'
_chemical_formula_weight         798.55
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                83.476(6)
_cell_angle_beta                 89.613(6)
_cell_angle_gamma                69.641(5)
_cell_formula_units_Z            1
_cell_length_a                   9.079(3)
_cell_length_b                   9.551(3)
_cell_length_c                   10.571(4)
_cell_measurement_reflns_used    'reflections from 60 data frames'
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      1.47
_cell_volume                     853.3(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.871
_diffrn_measured_fraction_theta_max 0.871
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0658
_diffrn_reflns_av_sigmaI/netI    0.1531
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            6608
_diffrn_reflns_theta_full        28.68
_diffrn_reflns_theta_max         28.68
_diffrn_reflns_theta_min         1.94
_diffrn_standards_decay_%        <1
_diffrn_standards_number         '50 standard frames at start and end'
_exptl_absorpt_coefficient_mu    0.717
_exptl_absorpt_correction_T_max  0.928074
_exptl_absorpt_correction_T_min  0.561012
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing,R., Acta Cryst. (1995) A51 33-38.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_description       block
_exptl_crystal_F_000             406
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.859
_refine_diff_density_min         -2.173
_refine_diff_density_rms         0.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         3830
_refine_ls_number_restraints     225
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.1081
_refine_ls_R_factor_gt           0.0679
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0600P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1447
_refine_ls_wR_factor_ref         0.1559
_reflns_number_gt                2287
_reflns_number_total             3830
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0011102B.cif
_cod_data_source_block           sg261a
_cod_database_code               4327562
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Nb Nb 0.47634(7) 0.10899(7) 0.43547(6) 0.0276(2) Uani 1 1 d U
N1 N 0.7442(6) -0.0915(6) 0.6511(5) 0.0331(12) Uani 1 1 d U
N2 N 0.6919(6) 0.1341(5) 0.5053(5) 0.0343(12) Uani 1 1 d U
C1 C 0.8435(7) -0.1810(7) 0.7436(6) 0.0379(16) Uani 1 1 d U
H1A H 0.8253 -0.2668 0.7821 0.045 Uiso 1 1 calc R
C2 C 0.9717(8) -0.1504(8) 0.7839(7) 0.0465(18) Uani 1 1 d U
H2A H 1.0395 -0.2182 0.8478 0.056 Uiso 1 1 calc R
C3 C 1.0053(8) -0.0277(9) 0.7363(8) 0.0525(19) Uani 1 1 d U
H3A H 1.0917 -0.0081 0.7682 0.063 Uiso 1 1 calc R
C4 C 0.9091(8) 0.0664(8) 0.6405(7) 0.0423(16) Uani 1 1 d U
C5 C 0.7797(7) 0.0305(7) 0.6012(6) 0.0317(14) Uani 1 1 d U
C6 C 0.8965(8) 0.2047(8) 0.5600(7) 0.0456(17) Uani 1 1 d U
H6A H 0.9648 0.2594 0.5603 0.055 Uiso 1 1 calc R
C7 C 0.7657(8) 0.2379(7) 0.4847(7) 0.0427(17) Uani 1 1 d U
H7A H 0.7290 0.3236 0.4242 0.051 Uiso 1 1 calc R
N3 N 0.5964(6) -0.0165(6) 0.2753(5) 0.0341(12) Uani 1 1 d U
N4 N 0.6768(6) -0.2380(5) 0.4247(5) 0.0339(12) Uani 1 1 d U
C8 C 0.6118(8) 0.0298(8) 0.1498(7) 0.0400(15) Uani 1 1 d U
H8A H 0.5587 0.1308 0.1175 0.048 Uiso 1 1 calc R
C9 C 0.7026(9) -0.0672(11) 0.0700(8) 0.060(2) Uani 1 1 d U
H9A H 0.7080 -0.0282 -0.0149 0.072 Uiso 1 1 calc R
C10 C 0.7802(12) -0.2067(13) 0.1026(11) 0.060(3) Uani 0.80(2) 1 d PU
H10A H 0.8411 -0.2685 0.0444 0.072 Uiso 1 1 calc R
C10' C 0.862(5) -0.377(6) 0.209(5) 0.060(3) Uani 0.20 1 d PU
C11 C 0.7709(9) -0.2578(10) 0.2185(8) 0.0539(18) Uani 1 1 d U
C12 C 0.6792(7) -0.1655(7) 0.3064(7) 0.0340(14) Uani 1 1 d U
C13 C 0.8417(9) -0.4199(9) 0.3071(10) 0.064(2) Uani 1 1 d U
H13A H 0.9106 -0.5121 0.2848 0.077 Uiso 1 1 calc R
C14 C 0.7748(8) -0.3875(7) 0.4233(8) 0.0445(17) Uani 1 1 d U
H14A H 0.7936 -0.4600 0.4950 0.053 Uiso 1 1 calc R
O1 O 0.3639(12) 0.4363(9) 0.1702(11) 0.148(4) Uani 1 1 d U
C15 C 0.2463(14) 0.5448(14) 0.1021(15) 0.132(5) Uani 1 1 d U
H15A H 0.1466 0.5539 0.1429 0.158 Uiso 1 1 calc R
H15B H 0.2401 0.5163 0.0166 0.158 Uiso 1 1 calc R
C16 C 0.2670(13) 0.6829(11) 0.0917(11) 0.093(3) Uani 1 1 d U
H16A H 0.1735 0.7598 0.1198 0.111 Uiso 1 1 calc R
H16B H 0.2846 0.7140 0.0031 0.111 Uiso 1 1 calc R
C17 C 0.4049(11) 0.6645(12) 0.1733(10) 0.088(3) Uani 1 1 d U
H17A H 0.3767 0.7328 0.2392 0.106 Uiso 1 1 calc R
H17B H 0.4885 0.6834 0.1229 0.106 Uiso 1 1 calc R
C18 C 0.4546(14) 0.5043(15) 0.2309(12) 0.114(4) Uani 1 1 d U
H18A H 0.5667 0.4526 0.2181 0.137 Uiso 1 1 calc R
H18B H 0.4371 0.4987 0.3226 0.137 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
N2 Nb N4 95.42(19) . 2_656
N2 Nb N3 93.40(19) . .
N4 Nb N3 170.76(17) 2_656 .
N2 Nb Nb 91.73(14) . 2_656
N4 Nb Nb 91.41(14) 2_656 2_656
N3 Nb Nb 91.08(14) . 2_656
N2 Nb N1 175.8(2) . 2_656
N4 Nb N1 86.77(18) 2_656 2_656
N3 Nb N1 84.26(18) . 2_656
Nb Nb N1 91.85(14) 2_656 2_656
C1 N1 C5 115.1(5) . .
C1 N1 Nb 130.3(4) . 2_656
C5 N1 Nb 114.7(4) . 2_656
C5 N2 C7 104.8(5) . .
C5 N2 Nb 118.3(4) . .
C7 N2 Nb 136.7(4) . .
N1 C1 C2 121.6(6) . .
C3 C2 C1 123.4(7) . .
C2 C3 C4 117.4(7) . .
C3 C4 C5 117.4(7) . .
C3 C4 C6 138.1(7) . .
C5 C4 C6 104.5(6) . .
N1 C5 N2 123.3(5) . .
N1 C5 C4 125.0(6) . .
N2 C5 C4 111.6(6) . .
C7 C6 C4 105.6(6) . .
C6 C7 N2 113.5(6) . .
C12 N3 C8 111.7(6) . .
C12 N3 Nb 116.0(4) . .
C8 N3 Nb 132.1(5) . .
C12 N4 C14 106.9(6) . .
C12 N4 Nb 117.8(4) . 2_656
C14 N4 Nb 135.2(5) . 2_656
N3 C8 C9 121.9(7) . .
C10 C9 C8 124.9(10) . .
C11 C10 C9 116.6(11) . .
C10 C11 C12 122.0(10) . .
C10 C11 C13 136.7(9) . .
C12 C11 C13 101.3(7) . .
N3 C12 N4 122.2(6) . .
N3 C12 C11 122.9(7) . .
N4 C12 C11 114.8(7) . .
C14 C13 C11 102.6(6) . .
C13 C14 N4 114.3(7) . .
C15 O1 C18 108.5(9) . .
O1 C15 C16 112.1(10) . .
C15 C16 C17 107.2(10) . .
C16 C17 C18 103.4(9) . .
O1 C18 C17 107.4(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Nb N2 2.195(5) .
Nb N4 2.198(5) 2_656
Nb N3 2.240(5) .
Nb Nb 2.2628(14) 2_656
Nb N1 2.273(5) 2_656
N1 C1 1.336(7) .
N1 C5 1.364(8) .
N1 Nb 2.273(5) 2_656
N2 C5 1.370(8) .
N2 C7 1.375(8) .
C1 C2 1.376(9) .
C2 C3 1.354(10) .
C3 C4 1.362(10) .
C4 C5 1.411(8) .
C4 C6 1.457(10) .
C6 C7 1.356(9) .
N3 C12 1.361(8) .
N3 C8 1.372(8) .
N4 C12 1.362(8) .
N4 C14 1.397(8) .
N4 Nb 2.198(5) 2_656
C8 C9 1.373(10) .
C9 C10 1.279(13) .
C10 C11 1.279(13) .
C11 C12 1.415(10) .
C11 C13 1.635(13) .
C13 C14 1.386(11) .
O1 C15 1.343(13) .
O1 C18 1.409(13) .
C15 C16 1.388(14) .
C16 C17 1.473(12) .
C17 C18 1.493(14) .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139136652
