#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:43:06 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178664 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/75/4077580.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_4077580
loop_
_publ_author_name
'Tayebani, Maryam'
'Conoci, Sabrina'
'Feghali, Khalil'
'Gambarotta, Sandro'
'Yap, Glenn P. A.'
_publ_section_title
;
 Tri- and Tetravalent and Mixed-Valence Niobium Complexes Supported by a
 Tripodal Tripyrrolylmethane Trianion
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              4568
_journal_paper_doi               10.1021/om000501t
_journal_volume                  19
_journal_year                    2000
_chemical_formula_sum            'C58 H84 Li2 N6 Nb O8'
_chemical_formula_weight         1100.10
_chemical_name_systematic
; 
 ? 
;
_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                117.166(3)
_cell_angle_beta                 90.288(4)
_cell_angle_gamma                96.559(4)
_cell_formula_units_Z            1
_cell_length_a                   10.562(2)
_cell_length_b                   12.247(3)
_cell_length_c                   12.799(3)
_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                     1460.2(6)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0694
_diffrn_reflns_av_sigmaI/netI    0.1668
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            11144
_diffrn_reflns_theta_full        23.25
_diffrn_reflns_theta_max         23.25
_diffrn_reflns_theta_min         1.79
_diffrn_standards_decay_%        <1
_diffrn_standards_number         '50 standard frames at start and end'
_exptl_absorpt_coefficient_mu    0.262
_exptl_absorpt_correction_T_max  0.928072
_exptl_absorpt_correction_T_min  0.617578
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing,R., Acta Cryst. (1995) A51 33-38.'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             585
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.844
_refine_diff_density_min         -1.261
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         4164
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1027
_refine_ls_R_factor_gt           0.0709
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1612
_refine_ls_wR_factor_ref         0.1748
_reflns_number_gt                2958
_reflns_number_total             4164
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om000501t.cif
_cod_data_source_block           sg248
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1460.1(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4077580
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 0.0000 0.0000 0.0000 0.0336(3) Uani 1 2 d S
N1 N 0.1036(4) -0.0727(5) -0.1537(4) 0.0532(14) Uani 1 1 d .
N2 N 0.0841(5) 0.1758(5) 0.0173(5) 0.0604(16) Uani 1 1 d .
N3 N 0.1747(4) 0.0070(5) 0.0889(4) 0.0467(13) Uani 1 1 d .
Li Li 0.3253(14) 0.3787(11) 0.6339(14) 0.086(4) Uani 1 1 d .
O1 O 0.2902(7) 0.4049(5) 0.5011(5) 0.112(2) Uani 1 1 d .
O2 O 0.1986(5) 0.2544(6) 0.6338(6) 0.101(2) Uani 1 1 d .
O3 O 0.4860(5) 0.3191(5) 0.6344(5) 0.0853(16) Uani 1 1 d .
O4 O 0.3162(8) 0.5253(5) 0.7713(6) 0.148(3) Uani 1 1 d .
C1 C 0.0752(6) -0.1658(7) -0.2661(6) 0.077(2) Uani 1 1 d .
H1A H -0.0034 -0.2173 -0.2929 0.093 Uiso 1 1 calc R
C2 C 0.1781(6) -0.1737(7) -0.3350(6) 0.0641(19) Uani 1 1 d .
H2A H 0.1818 -0.2288 -0.4151 0.077 Uiso 1 1 calc R
C3 C 0.2756(5) -0.0823(6) -0.2604(5) 0.0444(15) Uani 1 1 d .
H3A H 0.3583 -0.0656 -0.2809 0.053 Uiso 1 1 calc R
C4 C 0.2282(5) -0.0225(5) -0.1529(5) 0.0423(15) Uani 1 1 d .
C5 C 0.0382(7) 0.2865(7) 0.0472(9) 0.096(3) Uani 1 1 d .
H5A H -0.0458 0.3019 0.0668 0.115 Uiso 1 1 calc R
C6 C 0.1335(7) 0.3710(7) 0.0441(8) 0.090(3) Uani 1 1 d .
H6A H 0.1269 0.4535 0.0618 0.108 Uiso 1 1 calc R
C7 C 0.2426(6) 0.3104(6) 0.0096(6) 0.0553(17) Uani 1 1 d .
H7A H 0.3226 0.3441 -0.0019 0.066 Uiso 1 1 calc R
C8 C 0.2101(5) 0.1931(5) -0.0041(5) 0.0411(14) Uani 1 1 d .
C9 C 0.2059(6) -0.0190(6) 0.1795(6) 0.0540(17) Uani 1 1 d .
H9A H 0.1473 -0.0494 0.2181 0.065 Uiso 1 1 calc R
C10 C 0.3338(6) 0.0058(6) 0.2040(6) 0.0498(16) Uani 1 1 d .
H10A H 0.3787 -0.0051 0.2614 0.060 Uiso 1 1 calc R
C11 C 0.3880(5) 0.0508(5) 0.1285(5) 0.0389(14) Uani 1 1 d .
H11A H 0.4749 0.0770 0.1271 0.047 Uiso 1 1 calc R
C12 C 0.2899(5) 0.0490(5) 0.0582(5) 0.0368(14) Uani 1 1 d .
C13 C 0.2861(5) 0.0860(5) -0.0388(5) 0.0347(13) Uani 1 1 d .
H13A H 0.3745 0.1125 -0.0510 0.042 Uiso 1 1 calc R
C14 C 0.1864(19) 0.4725(16) 0.4963(13) 0.233(10) Uani 1 1 d .
H14A H 0.1064 0.4374 0.5143 0.279 Uiso 1 1 calc R
H14B H 0.2051 0.5596 0.5551 0.279 Uiso 1 1 calc R
C15 C 0.1734(12) 0.4636(10) 0.3816(11) 0.130(4) Uani 1 1 d .
H15A H 0.1938 0.5451 0.3845 0.157 Uiso 1 1 calc R
H15B H 0.0864 0.4289 0.3466 0.157 Uiso 1 1 calc R
C16 C 0.2669(11) 0.3795(14) 0.3135(11) 0.144(5) Uani 1 1 d .
H16A H 0.2222 0.3060 0.2467 0.173 Uiso 1 1 calc R
H16B H 0.3285 0.4219 0.2828 0.173 Uiso 1 1 calc R
C17 C 0.3301(15) 0.3447(13) 0.3866(11) 0.168(6) Uani 1 1 d .
H17A H 0.4225 0.3663 0.3872 0.202 Uiso 1 1 calc R
H17B H 0.3121 0.2549 0.3568 0.202 Uiso 1 1 calc R
C18 C 0.0663(11) 0.2504(17) 0.6120(18) 0.222(9) Uani 1 1 d .
H18A H 0.0444 0.2100 0.5270 0.266 Uiso 1 1 calc R
H18B H 0.0433 0.3346 0.6458 0.266 Uiso 1 1 calc R
C19 C -0.0026(10) 0.1817(17) 0.6651(16) 0.220(9) Uani 1 1 d .
H19A H -0.0439 0.2378 0.7341 0.264 Uiso 1 1 calc R
H19B H -0.0688 0.1196 0.6087 0.264 Uiso 1 1 calc R
C20 C 0.0835(8) 0.1251(11) 0.6977(10) 0.126(4) Uani 1 1 d .
H20A H 0.0607 0.0350 0.6562 0.152 Uiso 1 1 calc R
H20B H 0.0835 0.1522 0.7825 0.152 Uiso 1 1 calc R
C21 C 0.2112(7) 0.1606(8) 0.6665(9) 0.092(3) Uani 1 1 d .
H21A H 0.2733 0.1911 0.7340 0.111 Uiso 1 1 calc R
H21B H 0.2405 0.0890 0.6010 0.111 Uiso 1 1 calc R
C22 C 0.5269(8) 0.2160(8) 0.5337(7) 0.088(3) Uani 1 1 d .
H22A H 0.5735 0.2443 0.4827 0.106 Uiso 1 1 calc R
H22B H 0.4535 0.1557 0.4878 0.106 Uiso 1 1 calc R
C23 C 0.6135(10) 0.1594(9) 0.5851(8) 0.102(3) Uani 1 1 d .
H23A H 0.5651 0.0921 0.5953 0.123 Uiso 1 1 calc R
H23B H 0.6827 0.1265 0.5336 0.123 Uiso 1 1 calc R
C24 C 0.6650(11) 0.2609(10) 0.6995(10) 0.119(3) Uani 1 1 d .
H24A H 0.7419 0.3083 0.6908 0.143 Uiso 1 1 calc R
H24B H 0.6856 0.2295 0.7547 0.143 Uiso 1 1 calc R
C25 C 0.5574(9) 0.3392(9) 0.7405(8) 0.109(3) Uani 1 1 d .
H25A H 0.5025 0.3139 0.7892 0.130 Uiso 1 1 calc R
H25B H 0.5913 0.4268 0.7868 0.130 Uiso 1 1 calc R
C26 C 0.2480(15) 0.5210(10) 0.8660(11) 0.157(6) Uani 1 1 d .
H26A H 0.2614 0.4476 0.8747 0.188 Uiso 1 1 calc R
H26B H 0.1562 0.5208 0.8539 0.188 Uiso 1 1 calc R
C27 C 0.3045(11) 0.6360(12) 0.9697(9) 0.121(4) Uani 1 1 d .
H27A H 0.3792 0.6220 1.0055 0.145 Uiso 1 1 calc R
H27B H 0.2419 0.6683 1.0291 0.145 Uiso 1 1 calc R
C28 C 0.3422(10) 0.7233(9) 0.9178(10) 0.118(4) Uani 1 1 d .
H28A H 0.2742 0.7740 0.9250 0.141 Uiso 1 1 calc R
H28B H 0.4205 0.7783 0.9589 0.141 Uiso 1 1 calc R
C29 C 0.3610(16) 0.6522(9) 0.8039(12) 0.189(7) Uani 1 1 d .
H29A H 0.4522 0.6611 0.7910 0.226 Uiso 1 1 calc R
H29B H 0.3150 0.6791 0.7548 0.226 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'
Li Li -0.0003 0.0001 '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
N1 Nb N1 180.0(3) 2 .
N1 Nb N3 84.51(18) 2 2
N1 Nb N3 95.49(18) . 2
N1 Nb N3 95.49(18) 2 .
N1 Nb N3 84.51(18) . .
N3 Nb N3 180.0(3) 2 .
N1 Nb N2 95.9(2) 2 .
N1 Nb N2 84.1(2) . .
N3 Nb N2 96.03(18) 2 .
N3 Nb N2 83.97(18) . .
N1 Nb N2 84.1(2) 2 2
N1 Nb N2 95.9(2) . 2
N3 Nb N2 83.97(18) 2 2
N3 Nb N2 96.03(18) . 2
N2 Nb N2 180.0(3) . 2
C1 N1 C4 105.3(5) . .
C1 N1 Nb 134.1(4) . .
C4 N1 Nb 120.6(4) . .
C8 N2 C5 106.1(5) . .
C8 N2 Nb 120.2(4) . .
C5 N2 Nb 133.7(4) . .
C9 N3 C12 105.9(4) . .
C9 N3 Nb 134.5(4) . .
C12 N3 Nb 119.5(4) . .
O4 Li O2 108.2(7) . .
O4 Li O1 109.0(7) . .
O2 Li O1 109.2(8) . .
O4 Li O3 110.4(9) . .
O2 Li O3 105.4(6) . .
O1 Li O3 114.4(7) . .
C17 O1 C14 106.8(9) . .
C17 O1 Li 129.3(8) . .
C14 O1 Li 122.3(8) . .
C21 O2 C18 106.4(7) . .
C21 O2 Li 129.5(7) . .
C18 O2 Li 123.7(8) . .
C22 O3 C25 109.7(6) . .
C22 O3 Li 123.0(7) . .
C25 O3 Li 124.0(7) . .
C29 O4 C26 108.1(7) . .
C29 O4 Li 132.5(7) . .
C26 O4 Li 119.3(7) . .
N1 C1 C2 110.8(6) . .
C1 C2 C3 105.9(6) . .
C4 C3 C2 107.3(5) . .
C3 C4 N1 110.8(5) . .
C3 C4 C13 131.8(5) . .
N1 C4 C13 117.4(5) . .
C6 C5 N2 109.9(6) . .
C5 C6 C7 106.8(6) . .
C8 C7 C6 106.9(5) . .
C7 C8 N2 110.3(5) . .
C7 C8 C13 131.6(5) . .
N2 C8 C13 118.1(4) . .
C10 C9 N3 109.5(5) . .
C9 C10 C11 108.2(5) . .
C12 C11 C10 106.5(5) . .
C11 C12 N3 109.8(5) . .
C11 C12 C13 132.0(5) . .
N3 C12 C13 118.2(4) . .
C12 C13 C8 109.8(5) . .
C12 C13 C4 110.6(4) . .
C8 C13 C4 110.2(4) . .
C15 C14 O1 109.4(11) . .
C14 C15 C16 104.3(12) . .
C17 C16 C15 109.2(10) . .
C16 C17 O1 110.0(10) . .
O2 C18 C19 108.3(9) . .
C20 C19 C18 107.9(9) . .
C19 C20 C21 107.5(8) . .
O2 C21 C20 107.0(7) . .
O3 C22 C23 104.9(7) . .
C24 C23 C22 105.4(8) . .
C23 C24 C25 103.3(9) . .
O3 C25 C24 106.0(8) . .
O4 C26 C27 103.0(10) . .
C26 C27 C28 102.9(8) . .
C29 C28 C27 106.7(9) . .
C28 C29 O4 109.8(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Nb N1 2.123(5) 2
Nb N1 2.123(5) .
Nb N3 2.135(4) 2
Nb N3 2.135(4) .
Nb N2 2.144(5) .
Nb N2 2.144(5) 2
N1 C1 1.371(8) .
N1 C4 1.386(7) .
N2 C8 1.372(7) .
N2 C5 1.378(8) .
N3 C9 1.384(7) .
N3 C12 1.395(7) .
Li O4 1.866(15) .
Li O2 1.908(14) .
Li O1 1.911(17) .
Li O3 1.924(15) .
O1 C17 1.400(11) .
O1 C14 1.464(14) .
O2 C21 1.409(9) .
O2 C18 1.415(12) .
O3 C22 1.444(8) .
O3 C25 1.454(10) .
O4 C29 1.432(10) .
O4 C26 1.432(10) .
C1 C2 1.387(9) .
C2 C3 1.406(8) .
C3 C4 1.360(8) .
C4 C13 1.518(8) .
C5 C6 1.373(10) .
C6 C7 1.405(9) .
C7 C8 1.367(8) .
C8 C13 1.508(7) .
C9 C10 1.352(8) .
C10 C11 1.409(8) .
C11 C12 1.361(7) .
C12 C13 1.506(8) .
C14 C15 1.426(15) .
C15 C16 1.489(14) .
C16 C17 1.388(15) .
C18 C19 1.444(14) .
C19 C20 1.373(12) .
C20 C21 1.482(10) .
C22 C23 1.518(11) .
C23 C24 1.470(13) .
C24 C25 1.510(13) .
C26 C27 1.482(14) .
C27 C28 1.515(13) .
C28 C29 1.344(13) .
