#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/27/7012718.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_7012718
loop_
_publ_author_name
'Otero, A.'
'Fernández-Baeza, J.'
'Antiñolo, A.'
'Tejeda, J.'
'Lara-Sánchez, A.'
'Sánchez-Barba, L.'
'Expósito, M. T.'
'Rodríguez, A. M.'
_publ_section_title
;
 Niobium complexes containing a new chiral heteroscorpionate ligand and
 the reactivity of such a complex with O2 to give the first gem-diolate
 niobium complex
;
_journal_issue                   8
_journal_name_full               'Dalton Transactions'
_journal_page_first              1614
_journal_paper_doi               10.1039/b300497j
_journal_year                    2003
_chemical_formula_sum            'C43 H38 Cl4 N8 Nb2 O4'
_chemical_formula_weight         1058.44
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            18
_cell_length_a                   36.442(5)
_cell_length_b                   36.442(8)
_cell_length_c                   19.618(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_volume                     22563(7)
_computing_cell_refinement       'Nonius (control program)'
_computing_data_collection       'Nonius (control program)'
_computing_data_reduction        'XCAD4 (Harms, Wocadlo, 1995)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'four circle diffractometer Nonius-Mach3'
_diffrn_measurement_method       'ω/2θ 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  0.1485
_diffrn_reflns_av_sigmaI/netI    0.1305
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            17979
_diffrn_reflns_theta_full        27.99
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         2.24
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.716
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             9612
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.294
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.831
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         5954
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.831
_refine_ls_R_factor_all          0.3362
_refine_ls_R_factor_gt           0.0531
_refine_ls_shift/su_max          0.159
_refine_ls_shift/su_mean         0.022
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0452P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0912
_refine_ls_wR_factor_ref         0.1659
_reflns_number_gt                1184
_reflns_number_total             5954
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b300497j.txt
_cod_data_source_block           7
_cod_original_sg_symbol_H-M      R-3c
_cod_database_code               7012718
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'y, x, -z+1/2'
'-x+y, -x, z'
'-x, -x+y, -z+1/2'
'x-y, -y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'-x+y+2/3, -x+1/3, z+1/3'
'-x+2/3, -x+y+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'-x+y+1/3, -x+2/3, z+2/3'
'-x+1/3, -x+y+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'-y, -x, z-1/2'
'x-y, x, -z'
'x, x-y, z-1/2'
'-x+y, y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'x-y+2/3, x+1/3, -z+1/3'
'x+2/3, x-y+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'x-y+1/3, x+2/3, -z+2/3'
'x+1/3, x-y+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb 0.31443(3) 0.41682(3) 0.14690(4) 0.0811(3) Uani 1 1 d . . .
Cl1 Cl 0.33156(8) 0.46808(8) 0.06312(13) 0.1121(10) Uani 1 1 d . . .
Cl2 Cl 0.32089(8) 0.46147(8) 0.23815(13) 0.1104(10) Uani 1 1 d . . .
O1 O 0.28562(17) 0.36982(17) 0.0867(2) 0.0698(16) Uani 1 1 d . . .
O2 O 0.36202(17) 0.41836(18) 0.1531(3) 0.0936(18) Uani 1 1 d . . .
N1 N 0.2829(3) 0.3638(3) 0.2224(4) 0.077(2) Uani 1 1 d . . .
N2 N 0.2439(3) 0.3294(3) 0.2073(4) 0.074(2) Uani 1 1 d . . .
N3 N 0.2378(2) 0.4023(3) 0.1486(4) 0.084(2) Uani 1 1 d . A .
N4 N 0.2083(3) 0.3610(3) 0.1561(4) 0.077(2) Uani 1 1 d . . .
C1 C 0.2197(3) 0.3287(3) 0.1485(4) 0.065(2) Uani 1 1 d . . .
H1 H 0.1937 0.3010 0.1469 0.078 Uiso 1 1 calc . . .
C2 C 0.2462(4) 0.3333 0.0833 0.073(4) Uani 1 2 d S . .
C3 C 0.2325(4) 0.2982(3) 0.2546(5) 0.073(3) Uani 1 1 d . . .
C4 C 0.2655(4) 0.3143(5) 0.2991(5) 0.095(3) Uani 1 1 d . . .
H4 H 0.2671 0.3000 0.3372 0.114 Uiso 1 1 calc . . .
C5 C 0.2959(4) 0.3539(4) 0.2806(5) 0.091(3) Uani 1 1 d . . .
C6 C 0.1920(4) 0.2579(3) 0.2521(5) 0.106(4) Uani 1 1 d . . .
H6A H 0.1767 0.2572 0.2119 0.159 Uiso 1 1 calc . . .
H6B H 0.1755 0.2555 0.2918 0.159 Uiso 1 1 calc . . .
H6C H 0.1975 0.2347 0.2510 0.159 Uiso 1 1 calc . . .
C7 C 0.3370(3) 0.3835(4) 0.3121(5) 0.122(4) Uani 1 1 d . . .
H7A H 0.3509 0.4090 0.2856 0.183 Uiso 1 1 calc . . .
H7B H 0.3544 0.3706 0.3137 0.183 Uiso 1 1 calc . . .
H7C H 0.3324 0.3901 0.3576 0.183 Uiso 1 1 calc . . .
C8 C 0.1737(4) 0.3587(5) 0.1876(5) 0.084(3) Uani 1 1 d . . .
C9 C 0.1797(4) 0.3965(5) 0.1985(6) 0.104(4) Uani 1 1 d . A .
H9 H 0.1612 0.4037 0.2191 0.124 Uiso 1 1 calc . . .
C10 C 0.2187(4) 0.4231(4) 0.1733(6) 0.103(4) Uani 1 1 d . . .
C11 C 0.1372(4) 0.3165(4) 0.2056(7) 0.093(3) Uani 1 1 d . . .
C12 C 0.1154(4) 0.2851(5) 0.1615(6) 0.111(4) Uani 1 1 d . . .
H12 H 0.1232 0.2897 0.1158 0.133 Uiso 1 1 calc . . .
C13 C 0.0815(5) 0.2457(5) 0.1805(9) 0.138(5) Uani 1 1 d . . .
H13 H 0.0671 0.2242 0.1487 0.165 Uiso 1 1 calc . . .
C14 C 0.0699(4) 0.2400(5) 0.2498(10) 0.137(5) Uani 1 1 d . . .
H14 H 0.0483 0.2137 0.2642 0.164 Uiso 1 1 calc . . .
C15 C 0.0887(6) 0.2704(6) 0.2947(8) 0.148(6) Uani 1 1 d . . .
H15 H 0.0798 0.2665 0.3399 0.178 Uiso 1 1 calc . . .
C16 C 0.1225(4) 0.3091(4) 0.2723(8) 0.116(4) Uani 1 1 d . . .
H16 H 0.1357 0.3310 0.3037 0.140 Uiso 1 1 calc . . .
C17 C 0.2350(4) 0.4666(4) 0.1549(12) 0.104(7) Uani 0.60 1 d PG A 1
C18 C 0.2335(4) 0.4909(7) 0.2082(7) 0.115(7) Uani 0.60 1 d PG A 1
H18 H 0.2228 0.4785 0.2504 0.138 Uiso 0.60 1 calc P B 1
C19 C 0.2479(5) 0.5338(7) 0.1985(9) 0.228(15) Uani 0.60 1 d PG A 1
H19 H 0.2469 0.5501 0.2341 0.274 Uiso 0.60 1 calc P C 1
C20 C 0.2639(5) 0.5523(5) 0.1354(12) 0.166(10) Uani 0.60 1 d PG A 1
H20 H 0.2736 0.5810 0.1289 0.199 Uiso 0.60 1 calc P D 1
C21 C 0.2655(5) 0.5280(8) 0.0821(7) 0.184(10) Uani 0.60 1 d PG A 1
H21 H 0.2762 0.5404 0.0400 0.221 Uiso 0.60 1 calc P E 1
C22 C 0.2510(5) 0.4851(8) 0.0919(9) 0.146(9) Uani 0.60 1 d PG A 1
H22 H 0.2521 0.4689 0.0562 0.175 Uiso 0.60 1 calc P F 1
C17A C 0.2454 0.4713 0.1875 0.121 Uani 0.40 1 d P A 2
C18A C 0.2454 0.4922 0.2466 0.181 Uani 0.40 1 d P A 2
H18A H 0.2345 0.4771 0.2869 0.217 Uiso 0.40 1 calc P G 2
C19A C 0.2616 0.5358 0.2457 0.346 Uani 0.40 1 d P A 2
H19A H 0.2616 0.5498 0.2853 0.415 Uiso 0.40 1 calc P H 2
C20A C 0.2778 0.5584 0.1856 0.222 Uani 0.40 1 d P A 2
H20A H 0.2887 0.5875 0.1850 0.267 Uiso 0.40 1 calc P I 2
C21A C 0.2779 0.5374 0.1264 0.242 Uani 0.40 1 d P A 2
H21A H 0.2887 0.5526 0.0862 0.290 Uiso 0.40 1 calc P J 2
C22A C 0.2616 0.4939 0.1274 0.170 Uani 0.40 1 d P A 2
H22A H 0.2617 0.4798 0.0878 0.204 Uiso 0.40 1 calc P K 2
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'
Cl Cl 0.1484 0.1585 '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'
O O 0.0106 0.0060 '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
O2 Nb1 O1 99.6(3) . . ?
O2 Nb1 N1 93.2(3) . . ?
O1 Nb1 N1 79.7(3) . . ?
O2 Nb1 Cl1 99.4(2) . . ?
O1 Nb1 Cl1 95.14(17) . . ?
N1 Nb1 Cl1 167.0(2) . . ?
O2 Nb1 Cl2 100.1(2) . . ?
O1 Nb1 Cl2 156.01(18) . . ?
N1 Nb1 Cl2 85.6(2) . . ?
Cl1 Nb1 Cl2 95.08(10) . . ?
O2 Nb1 N3 170.1(3) . . ?
O1 Nb1 N3 76.7(3) . . ?
N1 Nb1 N3 77.2(3) . . ?
Cl1 Nb1 N3 90.13(19) . . ?
Cl2 Nb1 N3 81.7(2) . . ?
C2 O1 Nb1 137.0(4) . . ?
C5 N1 N2 106.2(8) . . ?
C5 N1 Nb1 133.6(9) . . ?
N2 N1 Nb1 119.5(6) . . ?
N1 N2 C3 110.9(8) . . ?
N1 N2 C1 122.2(8) . . ?
C3 N2 C1 126.9(9) . . ?
N4 N3 C10 103.8(9) . . ?
N4 N3 Nb1 114.2(6) . . ?
C10 N3 Nb1 134.6(8) . . ?
N3 N4 C8 108.2(9) . . ?
N3 N4 C1 120.3(8) . . ?
C8 N4 C1 129.2(10) . . ?
N4 C1 N2 109.1(7) . . ?
N4 C1 C2 114.3(7) . . ?
N2 C1 C2 108.3(7) . . ?
O1 C2 O1 112.5(11) . 18_554 ?
O1 C2 C1 105.9(4) . 18_554 ?
O1 C2 C1 110.7(4) 18_554 18_554 ?
O1 C2 C1 110.7(4) . . ?
O1 C2 C1 105.9(4) 18_554 . ?
C1 C2 C1 111.3(11) 18_554 . ?
N2 C3 C4 104.1(9) . . ?
N2 C3 C6 123.0(10) . . ?
C4 C3 C6 132.9(11) . . ?
C5 C4 C3 111.2(10) . . ?
N1 C5 C4 107.5(10) . . ?
N1 C5 C7 121.5(12) . . ?
C4 C5 C7 131.0(12) . . ?
C9 C8 N4 110.3(11) . . ?
C9 C8 C11 130.5(12) . . ?
N4 C8 C11 119.2(12) . . ?
C8 C9 C10 105.2(10) . . ?
N3 C10 C9 112.4(10) . . ?
N3 C10 C17 118.9(14) . . ?
C9 C10 C17 126.4(13) . . ?
N3 C10 C17A 119.4(11) . . ?
C9 C10 C17A 126.0(12) . . ?
C17 C10 C17A 27.5(8) . . ?
C12 C11 C16 116.0(12) . . ?
C12 C11 C8 125.0(12) . . ?
C16 C11 C8 118.9(12) . . ?
C11 C12 C13 123.3(12) . . ?
C12 C13 C14 117.0(12) . . ?
C15 C14 C13 122.3(16) . . ?
C14 C15 C16 117.7(15) . . ?
C15 C16 C11 123.5(12) . . ?
C18 C17 C22 120.0 . . ?
C18 C17 C10 112.9(18) . . ?
C22 C17 C10 127.1(18) . . ?
C19 C18 C17 120.0 . . ?
C18 C19 C20 120.0 . . ?
C21 C20 C19 120.0 . . ?
C20 C21 C22 120.0 . . ?
C21 C22 C17 120.0 . . ?
C18A C17A C22A 120.0 . . ?
C18A C17A C10 126.9(5) . . ?
C22A C17A C10 111.1(5) . . ?
C19A C18A C17A 120.0 . . ?
C18A C19A C20A 120.0 . . ?
C19A C20A C21A 120.0 . . ?
C22A C21A C20A 120.0 . . ?
C21A C22A C17A 120.0 . . ?
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 O2 1.711(5) . ?
Nb1 O1 1.906(5) . ?
Nb1 N1 2.243(7) . ?
Nb1 Cl1 2.327(3) . ?
Nb1 Cl2 2.350(3) . ?
Nb1 N3 2.568(8) . ?
O1 C2 1.387(8) . ?
N1 C5 1.353(11) . ?
N1 N2 1.376(9) . ?
N2 C3 1.362(10) . ?
N2 C1 1.442(10) . ?
N3 N4 1.352(9) . ?
N3 C10 1.352(10) . ?
N4 C8 1.371(11) . ?
N4 C1 1.441(10) . ?
C1 C2 1.560(10) . ?
C2 O1 1.387(8) 18_554 ?
C2 C1 1.560(10) 18_554 ?
C3 C4 1.359(11) . ?
C3 C6 1.473(12) . ?
C4 C5 1.357(12) . ?
C5 C7 1.473(13) . ?
C8 C9 1.297(12) . ?
C8 C11 1.487(14) . ?
C9 C10 1.350(13) . ?
C10 C17 1.433(15) . ?
C10 C17A 1.548(12) . ?
C11 C12 1.335(13) . ?
C11 C16 1.388(14) . ?
C12 C13 1.399(15) . ?
C13 C14 1.407(17) . ?
C14 C15 1.309(16) . ?
C15 C16 1.401(16) . ?
C17 C18 1.3900 . ?
C17 C22 1.3900 . ?
C18 C19 1.3900 . ?
C19 C20 1.3900 . ?
C20 C21 1.3900 . ?
C21 C22 1.3900 . ?
C17A C18A 1.3900 . ?
C17A C22A 1.3900 . ?
C18A C19A 1.3900 . ?
C19A C20A 1.3900 . ?
C20A C21A 1.3900 . ?
C21A C22A 1.3900 . ?
