#------------------------------------------------------------------------------
#$Date: 2018-10-05 15:19:55 +0300 (Fri, 05 Oct 2018) $
#$Revision: 211332 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/11/09/7110946.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# 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_7110946
loop_
_publ_author_name
'Long, De-Liang'
'Blake, Alexander J.'
'Champness, Neil R.'
'Schröder, Martin'
_publ_section_title
;
 Lanthanide co-ordination frameworks of
 4,4′-bipyridine-N,N′-dioxide
;
_journal_issue                   15
_journal_name_full               'Chemical Communications'
_journal_page_first              1369
_journal_paper_doi               10.1039/b002363i
_journal_year                    2000
_chemical_formula_sum            'C20 H17 N7 O13.5 Sm'
_chemical_formula_weight         721.76
_chemical_name_systematic        ?
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   'difference Fourier synthesis'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.529(4)
_cell_length_b                   17.616(5)
_cell_length_c                   17.244(5)
_cell_measurement_reflns_used    35
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      34
_cell_measurement_theta_min      25
_cell_volume                     5021(2)
_computing_cell_refinement       'Stoe STADI4'
_computing_data_collection       'Stoe STADI4 v1.07 (Stoe & Cie,1997a)'
_computing_data_reduction        'X-RED v1.09 (Stoe & Cie, 1997b)'
_computing_molecular_graphics    'SHELXTL/PC v5.03 (Sheldrick, 1994)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean MoK\a
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Stoe Stadi-4 four-circle'
_diffrn_measurement_method       omega/theta
_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
_diffrn_reflns_av_sigmaI/netI    0.018
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4919
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         2.60
_diffrn_standards_decay_%        'random variation +/-2.6'
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.424
_exptl_absorpt_correction_T_max  0.541
_exptl_absorpt_correction_T_min  0.357
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-RED (Stoe & Cie, 1997b)'
_exptl_crystal_colour            'Pale yellow'
_exptl_crystal_density_diffrn    1.907
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2848
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.51
_exptl_crystal_size_min          0.31
_refine_diff_density_max         1.11
_refine_diff_density_min         -1.12
_refine_diff_density_rms         0.10
_refine_ls_extinction_coef       0.00035(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.165
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         4919
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.165
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.025P)²+17.34P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0686
_refine_ls_wR_factor_ref         0.0772
_reflns_number_gt                4144
_reflns_number_total             4919
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b002363isup1.cif
_cod_data_source_block           SMPYON
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z 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 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'Numerical'
changed to 'numerical' 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 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'placed geometrically' was
changed to 'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_sg_symbol_H-M      Pbcn
_cod_database_code               7110946
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, 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_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
Sm Sm 0.254063(12) 0.279345(10) 0.141298(11) 0.01643(8) Uani 1 1 d . . .
O1 O 0.12550(17) 0.34804(15) 0.11639(17) 0.0222(6) Uani 1 1 d . . .
O2 O 0.26528(17) 0.37142(16) 0.23810(17) 0.0244(7) Uani 1 1 d . . .
O3 O 0.15355(19) 0.24587(16) 0.24345(17) 0.0248(7) Uani 1 1 d . . .
O4 O 0.17994(17) 0.19896(15) 0.05124(16) 0.0210(6) Uani 1 1 d . . .
O11 O 0.2620(2) 0.13843(17) 0.17795(18) 0.0321(8) Uani 1 1 d . . .
O12 O 0.3307(2) 0.21295(18) 0.2517(2) 0.0419(9) Uani 1 1 d . . .
O13 O 0.3411(4) 0.0897(2) 0.2641(3) 0.110(3) Uani 1 1 d . . .
O21 O 0.3811(2) 0.21155(17) 0.0885(2) 0.0312(7) Uani 1 1 d . . .
O22 O 0.40292(18) 0.32231(16) 0.13713(19) 0.0285(7) Uani 1 1 d . . .
O23 O 0.5019(2) 0.26066(19) 0.0825(2) 0.0443(9) Uani 1 1 d . . .
O31 O 0.2790(2) 0.31584(16) 0.00195(18) 0.0277(7) Uani 1 1 d . . .
O32 O 0.28519(19) 0.41261(16) 0.07772(18) 0.0275(7) Uani 1 1 d . . .
O33 O 0.3183(2) 0.4252(2) -0.0431(2) 0.0445(9) Uani 1 1 d . . .
N1 N 0.3110(3) 0.1461(2) 0.2329(3) 0.0512(14) Uani 1 1 d . A .
N2 N 0.4314(2) 0.2644(2) 0.1023(2) 0.0274(8) Uani 1 1 d . . .
N3 N 0.2950(2) 0.3858(2) 0.0106(2) 0.0244(8) Uani 1 1 d . . .
N10 N 0.1181(2) 0.40564(19) 0.06738(19) 0.0195(7) Uani 1 1 d . . .
N20 N 0.3227(2) 0.41477(18) 0.26853(18) 0.0179(7) Uani 1 1 d . . .
N30 N 0.1400(2) 0.2974(2) 0.2985(2) 0.0224(8) Uani 1 1 d . . .
N40 N 0.1198(2) 0.15349(18) 0.07354(19) 0.0178(7) Uani 1 1 d . . .
C11 C 0.1266(3) 0.4770(2) 0.0939(2) 0.0232(9) Uani 1 1 d . . .
H11A H 0.1336 0.4859 0.1478 0.028 Uiso 1 1 calc R . .
C12 C 0.1251(3) 0.5372(2) 0.0431(3) 0.0253(9) Uani 1 1 d . . .
H12A H 0.1313 0.5874 0.0623 0.030 Uiso 1 1 calc R . .
C13 C 0.1146(3) 0.5253(2) -0.0360(2) 0.0209(9) Uani 1 1 d . . .
C14 C 0.1024(3) 0.4506(2) -0.0604(2) 0.0243(9) Uani 1 1 d . . .
H14A H 0.0930 0.4406 -0.1137 0.029 Uiso 1 1 calc R . .
C15 C 0.1036(3) 0.3916(2) -0.0087(2) 0.0233(9) Uani 1 1 d . . .
H15A H 0.0944 0.3412 -0.0261 0.028 Uiso 1 1 calc R . .
C21 C 0.3790(3) 0.3845(2) 0.3155(3) 0.0266(10) Uani 1 1 d . . .
H21A H 0.3798 0.3314 0.3247 0.032 Uiso 1 1 calc R . .
C22 C 0.4354(3) 0.4308(2) 0.3500(3) 0.0250(9) Uani 1 1 d . . .
H22A H 0.4750 0.4090 0.3830 0.030 Uiso 1 1 calc R . .
C23 C 0.4357(2) 0.5092(2) 0.3375(2) 0.0170(8) Uani 1 1 d . . .
C24 C 0.3761(3) 0.5374(2) 0.2884(3) 0.0225(9) Uani 1 1 d . . .
H24A H 0.3736 0.5903 0.2782 0.027 Uiso 1 1 calc R . .
C25 C 0.3205(3) 0.4896(2) 0.2544(3) 0.0244(9) Uani 1 1 d . . .
H25A H 0.2803 0.5097 0.2207 0.029 Uiso 1 1 calc R . .
C31 C 0.1782(3) 0.2921(2) 0.3674(2) 0.0261(9) Uani 1 1 d . . .
H31A H 0.2116 0.2494 0.3779 0.031 Uiso 1 1 calc R . .
C32 C 0.1694(3) 0.3476(2) 0.4226(2) 0.0244(9) Uani 1 1 d . . .
H32A H 0.1963 0.3428 0.4710 0.029 Uiso 1 1 calc R . .
C33 C 0.1213(2) 0.4111(2) 0.4080(2) 0.0209(9) Uani 1 1 d . . .
C34 C 0.0811(3) 0.4134(3) 0.3369(3) 0.0276(10) Uani 1 1 d . . .
H34A H 0.0461 0.4547 0.3254 0.033 Uiso 1 1 calc R . .
C35 C 0.0917(3) 0.3569(3) 0.2837(2) 0.0275(10) Uani 1 1 d . . .
H35A H 0.0644 0.3597 0.2353 0.033 Uiso 1 1 calc R . .
C41 C 0.1279(3) 0.0777(2) 0.0675(3) 0.0249(9) Uani 1 1 d . . .
H41A H 0.1754 0.0569 0.0450 0.030 Uiso 1 1 calc R . .
C42 C 0.0677(3) 0.0302(2) 0.0937(3) 0.0233(9) Uani 1 1 d . . .
H42A H 0.0741 -0.0232 0.0889 0.028 Uiso 1 1 calc R . .
C43 C -0.0025(2) 0.0592(2) 0.1271(2) 0.0179(8) Uani 1 1 d . . .
C44 C -0.0102(3) 0.1382(2) 0.1290(3) 0.0250(9) Uani 1 1 d . . .
H44A H -0.0582 0.1604 0.1492 0.030 Uiso 1 1 calc R . .
C45 C 0.0506(3) 0.1840(2) 0.1020(3) 0.0237(9) Uani 1 1 d . . .
H45A H 0.0442 0.2376 0.1032 0.028 Uiso 1 1 calc R . .
O1W O 0.5000 0.0607(13) 0.2500 0.143(6) Uiso 0.591(15) 2 d SP A 1
O1W' O 0.5000 0.1365(19) 0.2500 0.143(6) Uiso 0.409(15) 2 d SP A 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'
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'
Sm Sm -0.1638 3.4418 '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_3
O2 Sm O4 154.26(10) .
O2 Sm O1 81.55(10) .
O4 Sm O1 75.06(10) .
O2 Sm O3 73.26(10) .
O4 Sm O3 88.73(9) .
O1 Sm O3 70.55(10) .
O2 Sm O31 119.42(10) .
O4 Sm O31 67.81(9) .
O1 Sm O31 81.42(10) .
O3 Sm O31 147.45(10) .
O2 Sm O11 119.48(10) .
O4 Sm O11 67.65(10) .
O1 Sm O11 123.93(10) .
O3 Sm O11 68.35(10) .
O31 Sm O11 118.24(10) .
O2 Sm O12 75.36(11) .
O4 Sm O12 117.17(10) .
O1 Sm O12 140.57(12) .
O3 Sm O12 72.38(12) .
O31 Sm O12 137.88(12) .
O11 Sm O12 49.56(10) .
O2 Sm O22 74.93(10) .
O4 Sm O22 129.38(9) .
O1 Sm O22 132.04(9) .
O3 Sm O22 136.57(10) .
O31 Sm O22 75.07(10) .
O11 Sm O22 104.02(10) .
O12 Sm O22 71.52(11) .
O2 Sm O21 120.58(10) .
O4 Sm O21 85.15(10) .
O1 Sm O21 149.40(10) .
O3 Sm O21 133.00(10) .
O31 Sm O21 69.46(11) .
O11 Sm O21 66.26(11) .
O12 Sm O21 69.46(12) .
O22 Sm O21 49.37(9) .
O2 Sm O32 70.36(10) .
O4 Sm O32 110.52(10) .
O1 Sm O32 70.23(9) .
O3 Sm O32 129.31(10) .
O31 Sm O32 49.16(9) .
O11 Sm O32 162.24(11) .
O12 Sm O32 128.03(10) .
O22 Sm O32 62.69(10) .
O21 Sm O32 96.10(10) .
N10 O1 Sm 124.2(2) .
N20 O2 Sm 137.7(2) .
N30 O3 Sm 117.1(2) .
N40 O4 Sm 122.8(2) .
N1 O11 Sm 96.6(3) .
N1 O12 Sm 96.1(3) .
N1 O13 O1W 120.5(7) .
N1 O13 O1W' 96.0(7) .
O1W O13 O1W' 28.3(6) .
N2 O21 Sm 97.3(2) .
N2 O22 Sm 97.5(2) .
N3 O31 Sm 99.8(2) .
N3 O32 Sm 94.2(2) .
O13 N1 O11 120.2(4) .
O13 N1 O12 122.3(5) .
O11 N1 O12 117.4(4) .
O13 N1 Sm 172.5(5) .
O11 N1 Sm 58.7(2) .
O12 N1 Sm 58.9(2) .
O23 N2 O21 122.3(4) .
O23 N2 O22 122.0(4) .
O21 N2 O22 115.7(3) .
O33 N3 O32 121.7(4) .
O33 N3 O31 121.9(4) .
O32 N3 O31 116.4(3) .
O1 N10 C11 119.3(3) .
O1 N10 C15 119.6(3) .
C11 N10 C15 121.1(4) .
O2 N20 C25 118.3(3) .
O2 N20 C21 120.4(3) .
C25 N20 C21 121.2(4) .
O3 N30 C35 119.7(4) .
O3 N30 C31 120.1(4) .
C35 N30 C31 120.1(4) .
O4 N40 C41 120.0(3) .
O4 N40 C45 119.7(3) .
C41 N40 C45 120.4(3) .
N10 C11 C12 120.1(4) .
C11 C12 C13 120.7(4) .
C12 C13 C14 117.1(4) .
C12 C13 C33 121.0(4) 7_565
C14 C13 C33 121.8(4) 7_565
C15 C14 C13 121.2(4) .
N10 C15 C14 119.6(4) .
N20 C21 C22 119.7(4) .
C21 C22 C23 121.5(4) .
C24 C23 C22 116.3(4) .
C24 C23 C43 121.8(4) 6_666
C22 C23 C43 121.9(4) 6_666
C25 C24 C23 120.9(4) .
N20 C25 C24 120.3(4) .
N30 C31 C32 120.7(4) .
C31 C32 C33 120.5(4) .
C34 C33 C32 116.9(4) .
C34 C33 C13 121.0(4) 7_566
C32 C33 C13 122.1(4) 7_566
C35 C34 C33 120.6(4) .
N30 C35 C34 121.2(4) .
N40 C41 C42 120.4(4) .
C41 C42 C43 121.0(4) .
C42 C43 C44 116.8(4) .
C42 C43 C23 121.8(4) 6_556
C44 C43 C23 121.4(4) 6_556
C45 C44 C43 120.8(4) .
N40 C45 C44 120.5(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
Sm O1 2.483(3) . y
Sm O2 2.335(3) . y
Sm O3 2.492(3) . y
Sm O4 2.433(3) . y
Sm O11 2.565(3) . y
Sm O12 2.569(4) . y
Sm O22 2.575(3) . y
Sm O21 2.582(3) . y
Sm O31 2.521(3) . y
Sm O32 2.642(3) . y
O1 N10 1.326(4) . ?
O2 N20 1.326(4) . ?
O3 N30 1.333(4) . ?
O4 N40 1.333(4) . ?
O11 N1 1.254(5) . ?
O12 N1 1.264(5) . ?
O13 N1 1.234(6) . ?
O13 O1W 2.687(9) . ?
O13 O1W' 2.763(12) . ?
O21 N2 1.271(5) . ?
O22 N2 1.274(4) . ?
O23 N2 1.216(5) . ?
O31 N3 1.269(4) . ?
O32 N3 1.260(5) . ?
O33 N3 1.220(5) . ?
N10 C11 1.346(5) . ?
N10 C15 1.357(5) . ?
N20 C25 1.340(5) . ?
N20 C21 1.344(6) . ?
N30 C35 1.342(6) . ?
N30 C31 1.349(5) . ?
N40 C41 1.345(5) . ?
N40 C45 1.356(5) . ?
C11 C12 1.375(6) . ?
C12 C13 1.391(6) . ?
C13 C14 1.394(6) . ?
C13 C33 1.483(6) 7_565 ?
C14 C15 1.369(6) . ?
C21 C22 1.374(6) . ?
C22 C23 1.397(6) . ?
C23 C24 1.391(6) . ?
C23 C43 1.480(5) 6_666 ?
C24 C25 1.378(6) . ?
C31 C32 1.372(6) . ?
C32 C33 1.396(6) . ?
C33 C34 1.395(6) . ?
C33 C13 1.483(6) 7_566 ?
C34 C35 1.366(6) . ?
C41 C42 1.377(6) . ?
C42 C43 1.393(6) . ?
C43 C44 1.397(5) . ?
C43 C23 1.480(5) 6_556 ?
C44 C45 1.371(6) . ?
