#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:51:15 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179309 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/06/4320680.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_4320680
loop_
_publ_author_name
'Carlos Yélamos'
'Karl R. Gust'
'Anwar G. Baboul'
'Mary Jane Heeg'
'H. Bernhard Schlegel'
'Charles H. Winter'
_publ_section_title
;
 Early Transition Metal Complexes Containing 1,2,4-Triazolato and
 Tetrazolato Ligands: Synthesis, Structure, and Molecular Orbital Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6451
_journal_page_last               6462
_journal_paper_doi               10.1021/ic0109389
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C41 H69 N12 Nb'
_chemical_formula_weight         822.99
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           20
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c 2'
_symmetry_space_group_name_H-M   'C 2 2 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.2966(8)
_cell_length_b                   23.9396(14)
_cell_length_c                   14.7500(8)
_cell_measurement_reflns_used    5783
_cell_measurement_temperature    295(2)
_cell_volume                     5048.3(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    SHELXTL-Plus
_computing_publication_material  SHELX-97
_computing_structure_refinement  'SHELX-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELX-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_measurement_device       'Bruker P4/CCD'
_diffrn_measurement_method       'SMART CCD'
_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  0.054
_diffrn_reflns_av_sigmaI/netI    0.0736
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            24787
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    0.276
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.083
_exptl_crystal_description       multifaceted
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.361
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(4)
_refine_ls_extinction_coef       0.00013(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.024
_refine_ls_goodness_of_fit_obs   1.064
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         5389
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_restrained_S_obs      1.064
_refine_ls_R_factor_all          0.0743
_refine_ls_R_factor_obs          0.0492
_refine_ls_shift/esd_max         -0.237
_refine_ls_shift/esd_mean        0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0482P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0996
_refine_ls_wR_factor_obs         0.0910
_reflns_number_observed          4221
_reflns_number_total             5390
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0109389_4.cif
_cod_data_source_block           band(4)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to the built-in table from CIF Core dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0482P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0482P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4320680
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Nb1 Nb 0.0000 0.188647(15) 0.7500 0.02985(11) Uani 1 d S .
N1 N 0.0466(2) 0.10503(10) 0.7588(3) 0.0383(6) Uani 1 d . .
C1 C 0.0770(3) 0.05193(13) 0.7633(3) 0.0480(10) Uani 1 d . .
C2 C 0.0000 0.0179(2) 0.7500 0.0575(13) Uani 1 d S .
H2 H 0.0000 -0.0209(2) 0.7500 0.069 Uiso 1 calc SR .
C3 C 0.1781(3) 0.0368(2) 0.7806(3) 0.0650(14) Uani 1 d . .
C4 C 0.2233(4) 0.0744(3) 0.8462(5) 0.124(3) Uani 1 d . .
H4A H 0.2893(6) 0.0671(13) 0.8474(22) 0.149 Uiso 1 calc R .
H4B H 0.1975(21) 0.0680(13) 0.9054(7) 0.149 Uiso 1 calc R .
H4C H 0.2125(26) 0.1124(3) 0.8288(17) 0.149 Uiso 1 calc R .
C5 C 0.1839(5) -0.0236(2) 0.8128(6) 0.173(4) Uani 1 d . .
H5A H 0.2470(11) -0.0368(9) 0.8067(38) 0.208 Uiso 1 calc R .
H5B H 0.1431(33) -0.0464(5) 0.7766(27) 0.208 Uiso 1 calc R .
H5C H 0.1652(39) -0.0258(4) 0.8752(13) 0.208 Uiso 1 calc R .
C6 C 0.2288(5) 0.0393(4) 0.6901(5) 0.155(4) Uani 1 d . .
H6A H 0.1991(23) 0.0144(17) 0.6480(12) 0.186 Uiso 1 calc R .
H6B H 0.2928(11) 0.0283(22) 0.6983(9) 0.186 Uiso 1 calc R .
H6C H 0.2264(33) 0.0767(6) 0.6669(18) 0.186 Uiso 1 calc R .
N2 N 0.0228(2) 0.18959(12) 0.6112(2) 0.0364(7) Uani 1 d . .
N3 N 0.0257(2) 0.24411(11) 0.6431(2) 0.0345(7) Uani 1 d . .
C7 C 0.0528(2) 0.1899(2) 0.5242(2) 0.0407(8) Uani 1 d . .
C8 C 0.0737(2) 0.2436(2) 0.5005(2) 0.0430(9) Uani 1 d . .
H8 H 0.0944(2) 0.2557(2) 0.4440(2) 0.052 Uiso 1 calc R .
C9 C 0.0585(2) 0.2769(2) 0.5763(2) 0.0421(9) Uani 1 d . .
C10 C 0.0639(3) 0.1365(2) 0.4685(3) 0.0578(11) Uani 1 d . .
C11 C 0.0195(6) 0.0879(2) 0.5131(3) 0.101(2) Uani 1 d . .
H11A H 0.0468(18) 0.0825(9) 0.5719(11) 0.122 Uiso 1 calc R .
H11B H 0.0294(22) 0.0551(3) 0.4769(13) 0.122 Uiso 1 calc R .
H11C H -0.0464(7) 0.0945(7) 0.5194(21) 0.122 Uiso 1 calc R .
C12 C 0.1666(5) 0.1265(3) 0.4575(5) 0.143(3) Uani 1 d . .
H12A H 0.1949(7) 0.1221(19) 0.5161(5) 0.171 Uiso 1 calc R .
H12B H 0.1945(7) 0.1577(9) 0.4269(27) 0.171 Uiso 1 calc R .
H12C H 0.1762(5) 0.0932(11) 0.4224(27) 0.171 Uiso 1 calc R .
C13 C 0.0189(8) 0.1459(2) 0.3755(3) 0.131(3) Uani 1 d . .
H13A H 0.0457(22) 0.1784(11) 0.3477(12) 0.157 Uiso 1 calc R .
H13B H -0.0472(9) 0.1512(17) 0.3827(4) 0.157 Uiso 1 calc R .
H13C H 0.0301(26) 0.1139(8) 0.3378(10) 0.157 Uiso 1 calc R .
C14 C 0.0756(4) 0.3389(2) 0.5894(3) 0.073(2) Uani 1 d . .
C15 C 0.1074(6) 0.3646(2) 0.4995(4) 0.151(4) Uani 1 d . .
H15A H 0.0696(22) 0.3503(15) 0.4511(6) 0.181 Uiso 1 calc R .
H15B H 0.1718(10) 0.3553(17) 0.4889(16) 0.181 Uiso 1 calc R .
H15C H 0.1008(33) 0.4045(3) 0.5024(13) 0.181 Uiso 1 calc R .
C16 C -0.0135(7) 0.3671(2) 0.6153(5) 0.140(3) Uani 1 d . .
H16A H -0.0544(14) 0.3685(17) 0.5638(9) 0.168 Uiso 1 calc R .
H16B H -0.0003(8) 0.4044(7) 0.6356(30) 0.168 Uiso 1 calc R .
H16C H -0.0431(17) 0.3465(11) 0.6633(21) 0.168 Uiso 1 calc R .
C17 C 0.1468(6) 0.3454(3) 0.6622(5) 0.138(3) Uani 1 d . .
H17A H 0.2068(8) 0.3338(17) 0.6398(10) 0.166 Uiso 1 calc R .
H17B H 0.1298(16) 0.3227(14) 0.7133(12) 0.166 Uiso 1 calc R .
H17C H 0.1499(22) 0.3839(4) 0.6804(21) 0.166 Uiso 1 calc R .
N4 N 0.1477(2) 0.20834(12) 0.7747(2) 0.0390(7) Uani 1 d . .
N5 N 0.2046(2) 0.1984(2) 0.6988(2) 0.0492(8) Uani 1 d . .
C18 C 0.2046(3) 0.2253(2) 0.8420(3) 0.0507(11) Uani 1 d . .
N6 N 0.2938(2) 0.2265(2) 0.8157(2) 0.0581(10) Uani 1 d . .
C19 C 0.2890(3) 0.2104(2) 0.7288(2) 0.0548(12) Uani 1 d . .
C20 C 0.1746(3) 0.2377(2) 0.9374(3) 0.078(2) Uani 1 d . .
H20A H 0.1514(19) 0.2041(3) 0.9651(7) 0.093 Uiso 1 calc R .
H20B H 0.1262(14) 0.2654(9) 0.9368(3) 0.093 Uiso 1 calc R .
H20C H 0.2271(6) 0.2513(12) 0.9714(6) 0.093 Uiso 1 calc R .
C21 C 0.3735(3) 0.2039(3) 0.6695(3) 0.094(2) Uani 1 d . .
H21A H 0.4263(6) 0.1934(14) 0.7059(4) 0.113 Uiso 1 calc R .
H21B H 0.3865(14) 0.2387(5) 0.6397(17) 0.113 Uiso 1 calc R .
H21C H 0.3619(9) 0.1756(10) 0.6249(15) 0.113 Uiso 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'
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
_geom_angle_publ_flag
N2 Nb1 N2 178.8(2) 3_556 . ?
N2 Nb1 N3 38.90(10) 3_556 3_556 ?
N2 Nb1 N3 139.86(11) . 3_556 ?
N2 Nb1 N3 139.86(11) 3_556 . ?
N2 Nb1 N3 38.90(10) . . ?
N3 Nb1 N3 101.32(14) 3_556 . ?
N2 Nb1 N1 91.23(13) 3_556 3_556 ?
N2 Nb1 N1 89.95(13) . 3_556 ?
N3 Nb1 N1 126.24(12) 3_556 3_556 ?
N3 Nb1 N1 127.55(12) . 3_556 ?
N2 Nb1 N1 89.95(13) 3_556 . ?
N2 Nb1 N1 91.23(13) . . ?
N3 Nb1 N1 127.55(12) 3_556 . ?
N3 Nb1 N1 126.24(13) . . ?
N1 Nb1 N1 37.47(13) 3_556 . ?
N2 Nb1 N4 89.15(9) 3_556 . ?
N2 Nb1 N4 90.58(9) . . ?
N3 Nb1 N4 84.73(10) 3_556 . ?
N3 Nb1 N4 79.60(10) . . ?
N1 Nb1 N4 121.14(10) 3_556 . ?
N1 Nb1 N4 83.68(10) . . ?
N2 Nb1 N4 90.58(9) 3_556 3_556 ?
N2 Nb1 N4 89.15(9) . 3_556 ?
N3 Nb1 N4 79.60(10) 3_556 3_556 ?
N3 Nb1 N4 84.73(10) . 3_556 ?
N1 Nb1 N4 83.68(10) 3_556 3_556 ?
N1 Nb1 N4 121.14(10) . 3_556 ?
N4 Nb1 N4 155.18(15) . 3_556 ?
C1 N1 N1 109.1(2) . 3_556 ?
C1 N1 Nb1 179.2(3) . . ?
N1 N1 Nb1 71.26(7) 3_556 . ?
N1 C1 C2 107.0(3) . . ?
N1 C1 C3 122.9(3) . . ?
C2 C1 C3 130.1(3) . . ?
C1 C2 C1 107.9(4) . 3_556 ?
C4 C3 C1 112.6(4) . . ?
C4 C3 C6 110.2(6) . . ?
C1 C3 C6 107.4(4) . . ?
C4 C3 C5 110.5(5) . . ?
C1 C3 C5 109.3(4) . . ?
C6 C3 C5 106.6(6) . . ?
C7 N2 N3 107.9(3) . . ?
C7 N2 Nb1 170.5(2) . . ?
N3 N2 Nb1 71.40(14) . . ?
C9 N3 N2 108.2(3) . . ?
C9 N3 Nb1 169.6(2) . . ?
N2 N3 Nb1 69.71(15) . . ?
N2 C7 C8 108.5(3) . . ?
N2 C7 C10 122.6(3) . . ?
C8 C7 C10 128.8(3) . . ?
C7 C8 C9 107.4(3) . . ?
N3 C9 C8 108.0(3) . . ?
N3 C9 C14 122.3(3) . . ?
C8 C9 C14 129.6(3) . . ?
C11 C10 C12 110.0(5) . . ?
C11 C10 C13 109.4(5) . . ?
C12 C10 C13 109.7(5) . . ?
C11 C10 C7 112.0(3) . . ?
C12 C10 C7 107.2(4) . . ?
C13 C10 C7 108.4(4) . . ?
C16 C14 C17 110.6(5) . . ?
C16 C14 C9 109.8(5) . . ?
C17 C14 C9 107.7(4) . . ?
C16 C14 C15 107.1(5) . . ?
C17 C14 C15 112.2(6) . . ?
C9 C14 C15 109.4(4) . . ?
C18 N4 N5 106.9(3) . . ?
C18 N4 Nb1 140.2(2) . . ?
N5 N4 Nb1 112.9(2) . . ?
C19 N5 N4 103.1(3) . . ?
N6 C18 N4 111.6(3) . . ?
N6 C18 C20 122.8(3) . . ?
N4 C18 C20 125.4(4) . . ?
C18 N6 C19 102.9(3) . . ?
N5 C19 N6 115.6(3) . . ?
N5 C19 C21 121.3(3) . . ?
N6 C19 C21 123.1(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 N2 2.073(2) 3_556 ?
Nb1 N2 2.073(2) . ?
Nb1 N3 2.094(3) 3_556 ?
Nb1 N3 2.094(3) . ?
Nb1 N1 2.114(2) 3_556 ?
Nb1 N1 2.114(2) . ?
Nb1 N4 2.194(3) . ?
Nb1 N4 2.194(3) 3_556 ?
N1 C1 1.345(4) . ?
N1 N1 1.358(5) 3_556 ?
C1 C2 1.384(4) . ?
C1 C3 1.512(6) . ?
C2 C1 1.384(4) 3_556 ?
C3 C4 1.470(6) . ?
C3 C6 1.519(8) . ?
C3 C5 1.526(7) . ?
N2 C7 1.354(4) . ?
N2 N3 1.388(4) . ?
N3 C9 1.343(4) . ?
C7 C8 1.367(5) . ?
C7 C10 1.526(5) . ?
C8 C9 1.391(5) . ?
C9 C14 1.517(5) . ?
C10 C11 1.480(6) . ?
C10 C12 1.497(7) . ?
C10 C13 1.531(7) . ?
C14 C16 1.490(10) . ?
C14 C17 1.488(8) . ?
C14 C15 1.531(7) . ?
N4 C18 1.347(4) . ?
N4 N5 1.403(4) . ?
N5 C19 1.317(5) . ?
C18 N6 1.334(5) . ?
C18 C20 1.500(5) . ?
N6 C19 1.340(5) . ?
C19 C21 1.501(5) . ?
