#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/31/2203165.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2203165
loop_
_publ_author_name
'Amini, Mostafa M.'
'Mirzaee, Mehdi'
'Yeganeh, Farnaz'
'Ng, Seik Weng'
_publ_section_title
;
 Tris(8-hydroxyquinolinato-κ²O,N)oxoniobium(V)
 dichloromethane disolvate
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m147
_journal_page_last               m148
_journal_paper_doi               10.1107/S1600536803029556
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '[Nb O (C9 H6 N O)3], 2C H2 Cl2'
_chemical_formula_moiety         '(C27 H18 N3 O4 Nb), 2(C H2 Cl2)'
_chemical_formula_sum            'C29 H22 Cl4 N3 Nb O4'
_chemical_formula_weight         711.21
_chemical_name_systematic
;
Tris(8-hydroxyquinolinato-κ²O,N)oxoniobium(V) dichloromethane disolvate
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5990(10)
_cell_length_b                   17.6590(10)
_cell_length_c                   13.0240(10)
_cell_measurement_reflns_used    5268
_cell_measurement_temperature    163(2)
_cell_measurement_theta_max      26.0
_cell_measurement_theta_min      2.4
_cell_volume                     2897.7(4)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      163(2)
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device_type  'Siemens P4/CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_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  0.066
_diffrn_reflns_av_sigmaI/netI    0.035
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            35672
_diffrn_reflns_theta_full        26.5
_diffrn_reflns_theta_max         26.5
_diffrn_reflns_theta_min         1.9
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.83
_exptl_absorpt_correction_T_max  0.945
_exptl_absorpt_correction_T_min  0.711
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.72
_refine_diff_density_min         -0.61
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.03
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         3058
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.03
_refine_ls_R_factor_all          0.054
_refine_ls_R_factor_gt           0.036
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0517P)²+2.9577P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.088
_refine_ls_wR_factor_ref         0.097
_reflns_number_gt                2422
_reflns_number_total             3058
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ci6322.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        2897.5(4)
_cod_database_code               2203165
_cod_database_fobs_code          2203165
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
Nb1 0.12824(3) 0.2500 0.01209(3) 0.01960(10) Uani d S 1 Nb
Cl1 0.51960(10) 0.40630(7) -0.07858(9) 0.0756(4) Uani d . 1 Cl
Cl2 0.45550(10) 0.36682(8) 0.12763(9) 0.0803(4) Uani d . 1 Cl
O1 0.2534(2) 0.2500 -0.0429(2) 0.0290(6) Uani d S 1 O
O2 0.1452(2) 0.31900(10) 0.13780(10) 0.0272(5) Uani d . 1 O
O3 0.0417(2) 0.2500 -0.1216(2) 0.0219(6) Uani d S 1 O
N1 0.1121(2) 0.37790(10) -0.0399(2) 0.0229(5) Uani d . 1 N
N2 -0.0552(3) 0.2500 0.0580(2) 0.0213(7) Uani d S 1 N
C1 0.0926(2) 0.4054(2) -0.1329(2) 0.0280(10) Uani d . 1 C
C2 0.0975(3) 0.4841(2) -0.1542(3) 0.0340(10) Uani d . 1 C
C3 0.1234(2) 0.5338(2) -0.0787(3) 0.0340(10) Uani d . 1 C
C4 0.1437(2) 0.5076(2) 0.0219(3) 0.0300(10) Uani d . 1 C
C5 0.1686(3) 0.5525(2) 0.1083(3) 0.0370(10) Uani d . 1 C
C6 0.1825(3) 0.5197(2) 0.2020(3) 0.0400(10) Uani d . 1 C
C7 0.1748(3) 0.4399(2) 0.2167(3) 0.0340(10) Uani d . 1 C
C8 0.1526(2) 0.3944(2) 0.1340(2) 0.0260(10) Uani d . 1 C
C9 0.1362(2) 0.4283(2) 0.0369(2) 0.0230(10) Uani d . 1 C
C10 -0.1001(4) 0.2500 0.1496(3) 0.0300(10) Uani d S 1 C
C11 -0.2114(4) 0.2500 0.1636(4) 0.0370(10) Uani d S 1 C
C12 -0.2749(4) 0.2500 0.0790(4) 0.0360(10) Uani d S 1 C
C13 -0.2316(3) 0.2500 -0.0203(3) 0.0270(10) Uani d S 1 C
C14 -0.2889(4) 0.2500 -0.1138(4) 0.0340(10) Uani d S 1 C
C15 -0.2352(4) 0.2500 -0.2065(4) 0.0340(10) Uani d S 1 C
C16 -0.1248(3) 0.2500 -0.2113(3) 0.0290(10) Uani d S 1 C
C17 -0.0648(3) 0.2500 -0.1230(3) 0.0220(10) Uani d S 1 C
C18 -0.1188(3) 0.2500 -0.0273(3) 0.0210(10) Uani d S 1 C
C19 0.4120(3) 0.3933(2) 0.0056(3) 0.0530(10) Uani d . 1 C
H1 0.0747 0.3713 -0.1867 0.034 Uiso calc R 1 H
H2 0.0826 0.5020 -0.2215 0.040 Uiso calc R 1 H
H3 0.1280 0.5864 -0.0936 0.041 Uiso calc R 1 H
H5 0.1758 0.6058 0.1010 0.044 Uiso calc R 1 H
H6 0.1978 0.5510 0.2594 0.048 Uiso calc R 1 H
H7 0.1849 0.4185 0.2829 0.041 Uiso calc R 1 H
H10 -0.0557 0.2500 0.2086 0.035 Uiso calc SR 1 H
H11 -0.2412 0.2500 0.2306 0.044 Uiso calc SR 1 H
H12 -0.3498 0.2500 0.0873 0.043 Uiso calc SR 1 H
H14 -0.3643 0.2500 -0.1129 0.041 Uiso calc SR 1 H
H15 -0.2748 0.2500 -0.2686 0.040 Uiso calc SR 1 H
H16 -0.0905 0.2500 -0.2762 0.034 Uiso calc SR 1 H
H19a 0.3710 0.4410 0.0106 0.064 Uiso calc R 1 H
H19b 0.3644 0.3537 -0.0220 0.064 Uiso calc R 1 H
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'
Cl Cl 0.1484 0.1585 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Nb1 O2 . . 103.60(10) yes
O1 Nb1 O2 . 7_565 103.60(10) no
O1 Nb1 O3 . . 97.60(10) yes
O1 Nb1 N1 . . 87.70(10) yes
O1 Nb1 N1 . 7_565 87.70(10) no
O1 Nb1 N2 . . 170.10(10) yes
O2 Nb1 O2 . 7_565 72.80(10) yes
O2 Nb1 O3 . . 137.00(10) yes
O2 Nb1 N1 . . 70.80(10) yes
O2 Nb1 N1 . 7_565 143.50(10) yes
O2 Nb1 N2 . . 84.30(10) yes
O2 Nb1 O3 7_565 . 137.00(10) no
O2 Nb1 N1 7_565 . 143.50(10) no
O2 Nb1 N1 7_565 7_565 70.80(10) no
O2 Nb1 N2 7_565 . 84.30(10) no
O3 Nb1 N1 . . 73.30(10) yes
O3 Nb1 N1 . 7_565 73.30(10) no
N1 Nb1 N1 7_565 . 145.20(10) yes
O3 Nb1 N2 . . 72.50(10) yes
N1 Nb1 N2 . . 89.40(10) yes
N1 Nb1 N2 7_565 . 89.40(10) no
C8 O2 Nb1 . . 124.7(2) no
C17 O3 Nb1 . . 122.9(2) no
C1 N1 C9 . . 117.9(3) no
C1 N1 Nb1 . . 128.8(2) no
C9 N1 Nb1 . . 113.0(2) no
C10 N2 C18 . . 118.8(4) no
C10 N2 Nb1 . . 129.9(3) no
C18 N2 Nb1 . . 111.3(2) no
N1 C1 C2 . . 121.9(3) no
C3 C2 C1 . . 120.1(3) no
C2 C3 C4 . . 120.1(3) no
C5 C4 C9 . . 117.4(3) no
C5 C4 C3 . . 126.5(3) no
C9 C4 C3 . . 116.1(3) no
C6 C5 C4 . . 120.3(3) no
C5 C6 C7 . . 122.1(3) no
C8 C7 C6 . . 119.2(3) no
O2 C8 C7 . . 124.7(3) no
O2 C8 C9 . . 116.4(2) no
C7 C8 C9 . . 118.9(3) no
N1 C9 C8 . . 114.2(2) no
N1 C9 C4 . . 123.7(3) no
C8 C9 C4 . . 122.1(3) no
N2 C10 C11 . . 122.8(4) no
C12 C11 C10 . . 118.6(4) no
C11 C12 C13 . . 121.1(4) no
C12 C13 C14 . . 126.5(4) no
C12 C13 C18 . . 116.6(4) no
C14 C13 C18 . . 116.9(4) no
C15 C14 C13 . . 120.1(4) no
C16 C15 C14 . . 121.7(4) no
C17 C16 C15 . . 120.8(4) no
O3 C17 C16 . . 124.2(4) no
O3 C17 C18 . . 117.8(3) no
C16 C17 C18 . . 118.0(4) no
N2 C18 C17 . . 115.6(3) no
N2 C18 C13 . . 122.1(4) no
C17 C18 C13 . . 122.3(4) no
Cl2 C19 Cl1 . . 111.1(2) no
N1 C1 H1 . . 119.0 no
C2 C1 H1 . . 119.0 no
C3 C2 H2 . . 119.9 no
C1 C2 H2 . . 119.9 no
C2 C3 H3 . . 119.9 no
C4 C3 H3 . . 119.9 no
C6 C5 H5 . . 119.9 no
C4 C5 H5 . . 119.9 no
C5 C6 H6 . . 118.9 no
C7 C6 H6 . . 118.9 no
C8 C7 H7 . . 120.4 no
C6 C7 H7 . . 120.4 no
N2 C10 H10 . . 118.6 no
C11 C10 H10 . . 118.6 no
C12 C11 H11 . . 120.7 no
C10 C11 H11 . . 120.7 no
C11 C12 H12 . . 119.4 no
C13 C12 H12 . . 119.4 no
C15 C14 H14 . . 119.9 no
C13 C14 H14 . . 119.9 no
C16 C15 H15 . . 119.1 no
C14 C15 H15 . . 119.1 no
C17 C16 H16 . . 119.6 no
C15 C16 H16 . . 119.6 no
Cl2 C19 H19a . . 109.4 no
Cl1 C19 H19a . . 109.4 no
Cl2 C19 H19b . . 109.4 no
Cl1 C19 H19b . . 109.4 no
H19a C19 H19b . . 108.0 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Nb1 O1 . 1.732(3) yes
Nb1 O2 . 2.052(2) yes
Nb1 O2 7_565 2.052(2) no
Nb1 O3 . 2.054(3) yes
Nb1 N1 . 2.366(2) yes
Nb1 N1 7_565 2.366(2) no
Nb1 N2 . 2.386(3) yes
Cl1 C19 . 1.759(4) no
Cl2 C19 . 1.745(4) no
O2 C8 . 1.337(3) no
O3 C17 . 1.342(5) no
N1 C1 . 1.328(4) no
N1 C9 . 1.373(4) no
N2 C10 . 1.321(5) no
N2 C18 . 1.370(5) no
C1 C2 . 1.419(4) no
C2 C3 . 1.358(5) no
C3 C4 . 1.413(5) no
C4 C5 . 1.412(5) no
C4 C9 . 1.417(4) no
C5 C6 . 1.362(5) no
C6 C7 . 1.425(4) no
C7 C8 . 1.372(4) no
C8 C9 . 1.414(4) no
C10 C11 . 1.414(7) no
C11 C12 . 1.362(7) no
C12 C13 . 1.403(6) no
C13 C14 . 1.416(6) no
C13 C18 . 1.424(5) no
C14 C15 . 1.384(7) no
C15 C16 . 1.393(6) no
C16 C17 . 1.376(6) no
C17 C18 . 1.420(6) no
C1 H1 . 0.95 no
C2 H2 . 0.95 no
C3 H3 . 0.95 no
C5 H5 . 0.95 no
C6 H6 . 0.95 no
C7 H7 . 0.95 no
C10 H10 . 0.95 no
C11 H11 . 0.95 no
C12 H12 . 0.95 no
C14 H14 . 0.95 no
C15 H15 . 0.95 no
C16 H16 . 0.95 no
C19 H19a . 0.99 no
C19 H19b . 0.99 no
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion
_geom_torsion_publ_flag
O1 Nb1 O2 C8 . 74.5(2) no
O2 Nb1 O2 C8 7_565 174.8(2) no
O3 Nb1 O2 C8 . -42.8(3) no
N1 Nb1 O2 C8 7_565 179.5(2) no
N1 Nb1 O2 C8 . -8.1(2) no
N2 Nb1 O2 C8 . -99.4(2) no
O2 Nb1 O3 C17 . -60.50(10) no
O2 Nb1 O3 C17 7_565 60.50(10) no
N1 Nb1 O3 C17 7_565 94.70(10) no
N1 Nb1 O3 C17 . -94.70(10) no
O1 Nb1 N1 C1 . 76.4(3) no
O2 Nb1 N1 C1 . -178.3(3) no
O2 Nb1 N1 C1 7_565 -173.6(2) no
O3 Nb1 N1 C1 . -22.3(2) no
N1 Nb1 N1 C1 7_565 -6.2(4) no
N2 Nb1 N1 C1 . -94.1(3) no
O1 Nb1 N1 C9 . -97.2(2) no
O2 Nb1 N1 C9 . 8.03(17) no
O2 Nb1 N1 C9 7_565 12.7(3) no
O3 Nb1 N1 C9 . 164.1(2) no
N1 Nb1 N1 C9 7_565 -179.90(10) no
N2 Nb1 N1 C9 . 92.2(2) no
O2 Nb1 N2 C10 . -36.60(10) no
O2 Nb1 N2 C10 7_565 36.60(10) no
N1 Nb1 N2 C10 7_565 107.40(10) no
N1 Nb1 N2 C10 . -107.40(10) no
O2 Nb1 N2 C18 . 143.40(10) no
O2 Nb1 N2 C18 7_565 -143.40(10) no
N1 Nb1 N2 C18 7_565 -72.60(10) no
N1 Nb1 N2 C18 . 72.60(10) no
C9 N1 C1 C2 . 0.9(4) no
Nb1 N1 C1 C2 . -172.5(2) no
N1 C1 C2 C3 . 0.4(5) no
C1 C2 C3 C4 . -1.2(5) no
C2 C3 C4 C5 . -178.2(3) no
C2 C3 C4 C9 . 0.7(4) no
C9 C4 C5 C6 . -1.3(5) no
C3 C4 C5 C6 . 177.6(3) no
C4 C5 C6 C7 . 1.3(5) no
C5 C6 C7 C8 . 0.0(5) no
Nb1 O2 C8 C7 . -173.0(2) no
Nb1 O2 C8 C9 . 7.0(4) no
C6 C7 C8 O2 . 178.8(3) no
C6 C7 C8 C9 . -1.1(5) no
C1 N1 C9 C8 . 178.1(2) no
Nb1 N1 C9 C8 . -7.5(3) no
C1 N1 C9 C4 . -1.5(4) no
Nb1 N1 C9 C4 . 172.9(2) no
O2 C8 C9 N1 . 1.5(4) no
C7 C8 C9 N1 . -178.5(3) no
O2 C8 C9 C4 . -178.9(2) no
C7 C8 C9 C4 . 1.1(4) no
C5 C4 C9 N1 . 179.7(3) no
C3 C4 C9 N1 . 0.7(4) no
C5 C4 C9 C8 . 0.1(4) no
C3 C4 C9 C8 . -178.9(3) no
