#------------------------------------------------------------------------------
#$Date: 2016-02-20 17:35:30 +0100 (Sat 20 de Feb de 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/61/2216110.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_2216110
loop_
_publ_author_name
'Liu, Yin-Qiu'
'Zeng, Xi-Rui'
'Lei, Liang-Ping'
_publ_section_title
;(2,2-Bipyridyl
 N,N'-dioxide-κ²O,O')trichloridobis(methanol-κO)terbium(III)
;
_journal_coeditor_code           SG2182
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2693
_journal_page_last               m2693
_journal_paper_doi               10.1107/S1600536807033910
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Tb Cl3 (C10 H12 N2 O2) (C1 H4 O1)2]'
_chemical_formula_moiety         'C12 H16 Cl3 N2 O4 Tb'
_chemical_formula_sum            'C12 H16 Cl3 N2 O4 Tb'
_chemical_formula_weight         517.54
_chemical_name_systematic
;(2,2-Bipyridyl
 N,N'-dioxide-κ²O,O')trichloridobis(methanol-\kO)terbium(III)
;
_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           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.985(4)
_cell_length_b                   15.054(4)
_cell_length_c                   7.976(2)
_cell_measurement_temperature    298(2)
_cell_volume                     1679.2(8)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Siemens, 1996)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Bruker APEXII 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  0.0702
_diffrn_reflns_av_sigmaI/netI    0.1019
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            4917
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         2.71
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.705
_exptl_absorpt_correction_T_max  0.5953
_exptl_absorpt_correction_T_min  0.4530
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.047
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.938
_refine_diff_density_min         -1.217
_refine_ls_abs_structure_details 'Flack (1983), with how many Friedel pairs?'
_refine_ls_abs_structure_Flack   -0.06(3)
_refine_ls_extinction_coef       0.00061(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     95
_refine_ls_number_reflns         1480
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      0.959
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0391
_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)+(0.018P)²+0.004P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0720
_refine_ls_wR_factor_ref         0.0731
_reflns_number_gt                1156
_reflns_number_total             1480
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            sg2182.cif
_cod_data_source_block           I
_cod_database_code               2216110
_cod_database_fobs_code          2216110
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_type_symbol
_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
Cl Cl1 0.7799(2) 0.15435(17) -0.1542(4) 0.0439(7) Uani d U 1
N N3 0.5828(3) 0.0943(3) 0.0755(7) 0.0290(10) Uani d GU 1
C C5 0.5081(4) 0.0484(3) -0.0001(9) 0.0292(11) Uani d GU 1
C C4 0.4313(3) 0.0947(4) -0.0678(8) 0.0308(12) Uani d GU 1
H H4 0.3814 0.0640 -0.1184 0.037 Uiso calc R 1
C C3 0.4292(3) 0.1869(4) -0.0600(8) 0.0320(12) Uani d GU 1
H H3 0.3778 0.2179 -0.1053 0.038 Uiso calc R 1
C C2 0.5039(4) 0.2328(3) 0.0156(9) 0.0315(12) Uani d GU 1
H H2 0.5025 0.2945 0.0208 0.038 Uiso calc R 1
C C1 0.5807(3) 0.1865(3) 0.0834(8) 0.0302(11) Uani d GU 1
H H1 0.6307 0.2172 0.1339 0.036 Uiso calc R 1
O O1 0.6523(4) 0.0482(4) 0.1438(8) 0.0287(11) Uani d U 1
Tb Tb1 0.78927(4) 0.0000 0.0000 0.0237(2) Uani d SU 1
O O2 0.8425(6) 0.0574(6) 0.2615(10) 0.0487(19) Uani d U 1
C C7 0.8075(8) 0.1191(8) 0.3768(13) 0.052(2) Uani d U 1
H H7A 0.8356 0.1082 0.4847 0.077 Uiso calc R 1
H H7B 0.7393 0.1136 0.3847 0.077 Uiso calc R 1
H H7C 0.8236 0.1781 0.3404 0.077 Uiso calc R 1
Cl Cl2 0.9862(2) 0.0000 0.0000 0.0493(9) Uani d SU 1
H H7 0.860(8) 0.013(11) 0.320(13) 0.08(5) Uiso d . 1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Cl1 0.0432(16) 0.0358(14) 0.0528(18) -0.0030(15) 0.0040(16) 0.0116(12)
N3 0.0264(18) 0.027(2) 0.033(2) 0.0045(17) 0.0051(18) -0.0006(19)
C5 0.027(2) 0.028(2) 0.033(3) 0.0028(18) 0.005(2) 0.000(2)
C4 0.029(2) 0.030(2) 0.034(3) 0.004(2) 0.004(2) 0.001(2)
C3 0.030(2) 0.030(2) 0.035(3) 0.005(2) 0.005(2) 0.001(2)
C2 0.031(2) 0.028(2) 0.036(3) 0.0040(19) 0.006(2) 0.001(2)
C1 0.028(2) 0.027(2) 0.035(3) 0.0028(19) 0.006(2) -0.001(2)
O1 0.0264(19) 0.027(2) 0.033(3) 0.0063(18) 0.0041(17) -0.002(2)
Tb1 0.0189(3) 0.0285(3) 0.0238(3) 0.000 0.000 -0.0023(7)
O2 0.041(3) 0.069(5) 0.036(3) 0.024(4) -0.013(3) -0.025(3)
C7 0.043(4) 0.070(6) 0.041(4) 0.024(4) -0.013(4) -0.027(3)
Cl2 0.0222(12) 0.083(3) 0.042(2) 0.000 0.000 0.000(5)
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'
Tb Tb -0.1723 4.1537 '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'
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 N3 C5 . . 118.3(5) ?
O1 N3 C1 . . 121.7(5) ?
C5 N3 C1 . . 120.0 ?
N3 C5 C4 . . 120.0 ?
N3 C5 C5 . 4 119.8(5) ?
C4 C5 C5 . 4 120.1(5) ?
C3 C4 C5 . . 120.0 ?
C3 C4 H4 . . 120.0 ?
C5 C4 H4 . . 120.0 ?
C4 C3 C2 . . 120.0 ?
C4 C3 H3 . . 120.0 ?
C2 C3 H3 . . 120.0 ?
C1 C2 C3 . . 120.0 ?
C1 C2 H2 . . 120.0 ?
C3 C2 H2 . . 120.0 ?
C2 C1 N3 . . 120.0 ?
C2 C1 H1 . . 120.0 ?
N3 C1 H1 . . 120.0 ?
N3 O1 Tb1 . . 124.4(5) ?
O1 Tb1 O1 4 . 70.6(3) ?
O1 Tb1 O2 4 . 142.8(3) yes
O1 Tb1 O2 . . 73.4(3) yes
O1 Tb1 O2 4 4 73.4(3) yes
O1 Tb1 O2 . 4 142.8(3) ?
O2 Tb1 O2 . 4 143.5(4) ?
O1 Tb1 Cl1 4 . 90.21(17) ?
O1 Tb1 Cl1 . . 85.13(17) yes
O2 Tb1 Cl1 . . 96.0(2) yes
O2 Tb1 Cl1 4 . 85.8(2) ?
O1 Tb1 Cl1 4 4 85.13(17) ?
O1 Tb1 Cl1 . 4 90.21(17) yes
O2 Tb1 Cl1 . 4 85.8(2) yes
O2 Tb1 Cl1 4 4 96.0(2) ?
Cl1 Tb1 Cl1 . 4 174.30(14) yes
O1 Tb1 Cl2 4 . 144.69(16) ?
O1 Tb1 Cl2 . . 144.69(16) yes
O2 Tb1 Cl2 . . 71.7(2) yes
O2 Tb1 Cl2 4 . 71.7(2) ?
Cl1 Tb1 Cl2 . . 92.85(7) ?
Cl1 Tb1 Cl2 4 . 92.85(7) ?
C7 O2 Tb1 . . 135.3(7) ?
C7 O2 H7 . . 105(9) ?
Tb1 O2 H7 . . 107(10) ?
O2 C7 H7A . . 109.5 ?
O2 C7 H7B . . 109.5 ?
H7A C7 H7B . . 109.5 ?
O2 C7 H7C . . 109.5 ?
H7A C7 H7C . . 109.5 ?
H7B C7 H7C . . 109.5 ?
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
Cl1 Tb1 . 2.632(3) yes
N3 O1 . 1.312(7) ?
N3 C5 . 1.3900 ?
N3 C1 . 1.3900 ?
C5 C4 . 1.3900 ?
C5 C5 4 1.45723 ?
C4 C3 . 1.3900 ?
C4 H4 . 0.9300 ?
C3 C2 . 1.3900 ?
C3 H3 . 0.9300 ?
C2 C1 . 1.3900 ?
C2 H2 . 0.9300 ?
C1 H1 . 0.9300 ?
O1 Tb1 . 2.347(6) yes
Tb1 O1 4 2.347(6) ?
Tb1 O2 . 2.377(7) yes
Tb1 O2 4 2.377(7) ?
Tb1 Cl1 4 2.632(3) ?
Tb1 Cl2 . 2.754(3) yes
O2 C7 . 1.396(12) ?
O2 H7 . 0.85(14) ?
C7 H7A . 0.9600 ?
C7 H7B . 0.9600 ?
C7 H7C . 0.9600 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O2 H7 Cl2 2_755 0.85(9) 2.59(9) 3.179(8) 128(10)
