#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/62/2016246.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_2016246
loop_
_publ_author_name
'Ana María Atria'
'María Teresa Garland'
'Ricardo Baggio'
_publ_section_title
;
 Three isomorphous Ln complexes:
 {[Ln₂(bt)₆(bno)(H₂O)₄]·bno}ₙ (bt is
 but-2-enoate and bno is 4,4'-bipyridyl N,N'-dioxide),
 with Ln = Nd, Er and Y
;
_journal_coeditor_code           FA3117
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m490
_journal_page_last               m493
_journal_paper_doi               10.1107/S0108270107045404
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac
'[Er2 (C4 H5 O2)6 (C10 H8 N2 O2) (H2 O)4], C10 H8 N2 O2'
_chemical_formula_moiety         'C34 H46 Er2 N2 O18, C10 H8 N2 O2'
_chemical_formula_sum            'C44 H54 Er2 N4 O20'
_chemical_formula_weight         1293.44
_chemical_name_systematic
;
catena-poly[[[di-μ-but-2-enoato-κ³O:O,O';κ³O,O':O'-bis[diaquadibut-2-\
enoato-\kO;κ²O,O'-erbium(III)]]-μ-4,4'-bipyridyl dioxide-κ²O:O']
4,4'-bipyridyl dioxide solvate]
;
_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                85.728(2)
_cell_angle_beta                 71.1810(10)
_cell_angle_gamma                69.0990(10)
_cell_formula_units_Z            1
_cell_length_a                   9.1731(9)
_cell_length_b                   12.0358(12)
_cell_length_c                   12.7221(13)
_cell_measurement_reflns_used    6237
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.05
_cell_measurement_theta_min      4.12
_cell_volume                     1240.7(2)
_computing_cell_refinement       'SAINT-NT (Bruker, 2001)'
_computing_data_collection       'SMART-NT (Bruker, 2001)'
_computing_data_reduction        'SAINT-NT (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL-NT (Bruker, 2001)'
_computing_publication_material
'SHELXTL-NT (Bruker, 2001) and PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_device_type  'Bruker SMART 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  0.0316
_diffrn_reflns_av_sigmaI/netI    0.0540
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9217
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.98
_diffrn_reflns_theta_min         1.69
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.439
_exptl_absorpt_correction_T_max  0.67
_exptl_absorpt_correction_T_min  0.56
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.731
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             642
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.088
_refine_diff_density_min         -1.606
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         5394
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0380
_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)+(0.0492P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0907
_refine_ls_wR_factor_ref         0.0948
_reflns_number_gt                4772
_reflns_number_total             5394
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            fa3117.cif
_cod_data_source_block           II
_cod_original_sg_symbol_Hall     '-P 1 '
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               2016246
_cod_database_fobs_code          2016246
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
Er Er1 0.84952(2) 0.889230(18) 0.521512(16) 0.03019(9) Uani d . 1
O O11 0.7222(4) 1.0533(3) 0.4248(3) 0.0418(8) Uani d . 1
O O12 0.9138(4) 1.0965(4) 0.4560(3) 0.0468(9) Uani d . 1
C C11 0.8103(5) 1.1167(4) 0.4047(4) 0.0331(10) Uani d . 1
C C12 0.8064(10) 1.2089(6) 0.3260(6) 0.0685(19) Uani d D 1
H H12 0.8764 1.2505 0.3205 0.082 Uiso calc R 1
C C13 0.7188(11) 1.2385(8) 0.2646(7) 0.088(3) Uani d D 1
H H13 0.6493 1.1969 0.2682 0.106 Uiso calc R 1
C C14 0.7182(15) 1.3397(10) 0.1828(10) 0.140(5) Uani d . 1
H H14A 0.7706 1.3884 0.2010 0.210 Uiso calc R 1
H H14B 0.6067 1.3874 0.1883 0.210 Uiso calc R 1
H H14C 0.7768 1.3063 0.1084 0.210 Uiso calc R 1
O O21 1.0396(4) 0.8627(3) 0.3338(3) 0.0312(7) Uani d . 1
O O22 1.0650(4) 0.7024(3) 0.4287(3) 0.0408(8) Uani d . 1
C C21 1.1071(6) 0.7511(4) 0.3402(4) 0.0329(10) Uani d . 1
C C22 1.2422(7) 0.6788(5) 0.2444(5) 0.0475(13) Uani d D 1
H H22 1.2746 0.5964 0.2466 0.057 Uiso calc R 1
C C23 1.3179(8) 0.7237(6) 0.1576(5) 0.0575(16) Uani d D 1
H H23 1.2767 0.8060 0.1533 0.069 Uiso calc R 1
C C24 1.4652(10) 0.6560(8) 0.0638(6) 0.088(3) Uani d . 1
H H24A 1.5604 0.6692 0.0680 0.132 Uiso calc R 1
H H24B 1.4476 0.6827 -0.0056 0.132 Uiso calc R 1
H H24C 1.4821 0.5726 0.0687 0.132 Uiso calc R 1
O O31 0.8454(4) 0.7488(3) 0.6498(3) 0.0443(9) Uani d . 1
O O32 0.6091(6) 0.8020(5) 0.7890(4) 0.0757(14) Uani d . 1
C C31 0.7531(7) 0.7342(6) 0.7441(5) 0.0523(14) Uani d . 1
C C32 0.8237(9) 0.6288(7) 0.8056(6) 0.0683(19) Uani d D 1
H H32 0.7601 0.6238 0.8781 0.082 Uiso calc R 1
C C33 0.9626(9) 0.5452(6) 0.7685(6) 0.0633(18) Uani d D 1
H H33 1.0268 0.5525 0.6968 0.076 Uiso calc R 1
C C34 1.0345(12) 0.4370(8) 0.8262(8) 0.094(3) Uani d . 1
H H34A 0.9563 0.4354 0.8973 0.141 Uiso calc R 1
H H34B 1.1328 0.4389 0.8365 0.141 Uiso calc R 1
H H34C 1.0608 0.3670 0.7820 0.141 Uiso calc R 1
O O41 0.7417(4) 0.8064(3) 0.4151(3) 0.0370(8) Uani d . 1
N N41 0.6770(5) 0.7221(3) 0.4387(3) 0.0304(8) Uani d . 1
C C41 0.5455(6) 0.7335(4) 0.4091(4) 0.0398(12) Uani d . 1
H H41 0.5016 0.8000 0.3718 0.048 Uiso calc R 1
C C42 0.4749(6) 0.6481(5) 0.4332(5) 0.0419(12) Uani d . 1
H H42 0.3817 0.6587 0.4135 0.050 Uiso calc R 1
C C43 0.5390(6) 0.5457(4) 0.4864(4) 0.0316(10) Uani d . 1
C C44 0.6777(6) 0.5365(5) 0.5135(5) 0.0415(12) Uani d . 1
H H44 0.7261 0.4696 0.5487 0.050 Uiso calc R 1
C C45 0.7447(6) 0.6241(5) 0.4894(5) 0.0405(12) Uani d . 1
H H45 0.8378 0.6159 0.5083 0.049 Uiso calc R 1
O O51 0.5304(5) 0.8752(4) 0.1544(3) 0.0597(11) Uani d . 1
N N51 0.6594(5) 0.9064(4) 0.1121(4) 0.0445(11) Uani d . 1
C C51 0.7466(7) 0.9165(5) 0.1754(4) 0.0468(13) Uani d . 1
H H51 0.7155 0.8993 0.2501 0.056 Uiso calc R 1
C C52 0.8791(6) 0.9513(5) 0.1334(4) 0.0421(12) Uani d . 1
H H52 0.9371 0.9564 0.1797 0.051 Uiso calc R 1
C C53 0.9298(6) 0.9791(5) 0.0226(4) 0.0379(11) Uani d . 1
C C54 0.8420(7) 0.9625(6) -0.0418(4) 0.0516(15) Uani d . 1
H H54 0.8747 0.9757 -0.1174 0.062 Uiso calc R 1
C C55 0.7081(7) 0.9271(6) 0.0024(5) 0.0506(14) Uani d . 1
H H55 0.6513 0.9175 -0.0429 0.061 Uiso calc R 1
O O1W 0.5649(4) 0.9358(4) 0.6189(3) 0.0504(10) Uani d D 1
H H1WA 0.481(5) 0.939(5) 0.602(4) 0.060 Uiso d D 1
H H1WB 0.564(7) 0.894(5) 0.676(3) 0.060 Uiso d D 1
O O2W 0.7644(4) 1.0099(4) 0.6826(3) 0.0450(9) Uani d D 1
H H2WA 0.808(5) 1.061(4) 0.684(4) 0.054 Uiso d D 1
H H2WB 0.672(3) 1.034(4) 0.733(4) 0.054 Uiso d D 1
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'
Er Er -0.2586 4.9576 '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
O31 Er1 O12 . 2_776 90.99(14)
O31 Er1 O2W . . 80.74(14)
O12 Er1 O2W 2_776 . 72.71(12)
O31 Er1 O41 . . 93.60(12)
O12 Er1 O41 2_776 . 146.49(12)
O2W Er1 O41 . . 140.78(12)
O31 Er1 O1W . . 76.40(14)
O12 Er1 O1W 2_776 . 140.39(13)
O2W Er1 O1W . . 68.29(13)
O41 Er1 O1W . . 72.64(13)
O31 Er1 O11 . . 153.43(13)
O12 Er1 O11 2_776 . 111.30(13)
O2W Er1 O11 . . 91.96(14)
O41 Er1 O11 . . 75.96(12)
O1W Er1 O11 . . 77.17(13)
O31 Er1 O21 . . 126.51(12)
O12 Er1 O21 2_776 . 76.16(11)
O2W Er1 O21 . . 138.72(11)
O41 Er1 O21 . . 74.49(11)
O1W Er1 O21 . . 140.89(12)
O11 Er1 O21 . . 74.80(11)
O31 Er1 O22 . . 73.67(12)
O12 Er1 O22 2_776 . 77.61(12)
O2W Er1 O22 . . 140.11(13)
O41 Er1 O22 . . 71.96(12)
O1W Er1 O22 . . 131.34(14)
O11 Er1 O22 . . 123.83(12)
O21 Er1 O22 . . 52.93(11)
O31 Er1 O12 . . 146.95(12)
O12 Er1 O12 2_776 . 62.99(15)
O2W Er1 O12 . . 72.53(12)
O41 Er1 O12 . . 119.39(11)
O1W Er1 O12 . . 109.96(13)
O11 Er1 O12 . . 48.72(10)
O21 Er1 O12 . . 69.46(10)
O22 Er1 O12 . . 116.13(11)
C11 O11 Er1 . . 105.4(3)
C11 O12 Er1 . 2_776 152.3(3)
C11 O12 Er1 . . 86.6(3)
Er1 O12 Er1 2_776 . 117.01(15)
O11 C11 O12 . . 117.6(5)
O11 C11 C12 . . 125.5(5)
O12 C11 C12 . . 116.9(5)
C13 C12 C11 . . 126.5(8)
C13 C12 H12 . . 116.7
C11 C12 H12 . . 116.7
C12 C13 C14 . . 124.1(9)
C12 C13 H13 . . 117.9
C14 C13 H13 . . 117.9
C13 C14 H14A . . 109.5
C13 C14 H14B . . 109.5
H14A C14 H14B . . 109.5
C13 C14 H14C . . 109.5
H14A C14 H14C . . 109.5
H14B C14 H14C . . 109.5
C21 O21 Er1 . . 94.0(3)
C21 O22 Er1 . . 92.8(3)
O22 C21 O21 . . 120.2(4)
C23 C22 C21 . . 123.8(6)
C23 C22 H22 . . 118.1
C21 C22 H22 . . 118.1
C22 C23 C24 . . 126.2(7)
C22 C23 H23 . . 116.9
C24 C23 H23 . . 116.9
C23 C24 H24A . . 109.5
C23 C24 H24B . . 109.5
H24A C24 H24B . . 109.5
C23 C24 H24C . . 109.5
H24A C24 H24C . . 109.5
H24B C24 H24C . . 109.5
C31 O31 Er1 . . 139.1(4)
O32 C31 O31 . . 124.5(6)
O32 C31 C32 . . 118.2(5)
O31 C31 C32 . . 117.3(5)
C33 C32 C31 . . 126.5(6)
C33 C32 H32 . . 116.8
C31 C32 H32 . . 116.8
C32 C33 C34 . . 127.8(7)
C32 C33 H33 . . 116.1
C34 C33 H33 . . 116.1
C33 C34 H34A . . 109.5
C33 C34 H34B . . 109.5
H34A C34 H34B . . 109.5
C33 C34 H34C . . 109.5
H34A C34 H34C . . 109.5
H34B C34 H34C . . 109.5
N41 O41 Er1 . . 130.0(3)
O41 N41 C41 . . 119.1(4)
O41 N41 C45 . . 120.7(4)
C41 N41 C45 . . 120.1(4)
N41 C41 C42 . . 120.5(4)
N41 C41 H41 . . 119.7
C42 C41 H41 . . 119.7
C41 C42 C43 . . 121.7(4)
C41 C42 H42 . . 119.2
C43 C42 H42 . . 119.2
C44 C43 C42 . . 115.8(4)
C44 C43 C43 . 2_666 122.7(5)
C42 C43 C43 . 2_666 121.5(5)
C45 C44 C43 . . 121.3(5)
C45 C44 H44 . . 119.4
C43 C44 H44 . . 119.4
N41 C45 C44 . . 120.6(4)
N41 C45 H45 . . 119.7
C44 C45 H45 . . 119.7
O51 N51 C51 . . 121.0(5)
O51 N51 C55 . . 119.8(5)
C51 N51 C55 . . 119.2(5)
N51 C51 C52 . . 121.9(5)
N51 C51 H51 . . 119.1
C52 C51 H51 . . 119.1
C51 C52 C53 . . 121.4(5)
C51 C52 H52 . . 119.3
C53 C52 H52 . . 119.3
C54 C53 C52 . . 115.4(5)
C54 C53 C53 . 2_775 122.9(5)
C52 C53 C53 . 2_775 121.6(6)
C55 C54 C53 . . 122.2(5)
C55 C54 H54 . . 118.9
C53 C54 H54 . . 118.9
N51 C55 C54 . . 119.9(5)
N51 C55 H55 . . 120.1
C54 C55 H55 . . 120.1
Er1 O1W H1WA . . 136(4)
Er1 O1W H1WB . . 104(4)
H1WA O1W H1WB . . 105(5)
Er1 O2W H2WA . . 120(3)
Er1 O2W H2WB . . 130(3)
H2WA O2W H2WB . . 105(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
Er1 O31 . 2.262(4) y
Er1 O12 2_776 2.344(3) y
Er1 O2W . 2.350(3) y
Er1 O41 . 2.361(3) y
Er1 O1W . 2.375(3) y
Er1 O11 . 2.387(4) y
Er1 O21 . 2.423(3) y
Er1 O22 . 2.465(3) y
Er1 O12 . 2.773(4) y
O11 C11 . 1.256(5) ?
O12 C11 . 1.265(6) ?
C11 C12 . 1.437(8) ?
C12 C13 . 1.241(9) ?
C12 H12 . 0.9300 ?
C13 C14 . 1.542(12) ?
C13 H13 . 0.9300 ?
C14 H14A . 0.9600 ?
C14 H14B . 0.9600 ?
C14 H14C . 0.9600 ?
O21 C21 . 1.271(6) ?
O22 C21 . 1.242(6) ?
C22 C23 . 1.295(7) ?
C22 H22 . 0.9300 ?
C23 C24 . 1.494(9) ?
C23 H23 . 0.9300 ?
C24 H24A . 0.9600 ?
C24 H24B . 0.9600 ?
C24 H24C . 0.9600 ?
O31 C31 . 1.268(6) ?
O32 C31 . 1.245(7) ?
C31 C32 . 1.494(9) ?
C32 C33 . 1.276(8) ?
C32 H32 . 0.9300 ?
C33 C34 . 1.492(11) ?
C33 H33 . 0.9300 ?
C34 H34A . 0.9600 ?
C34 H34B . 0.9600 ?
C34 H34C . 0.9600 ?
O41 N41 . 1.320(5) ?
N41 C41 . 1.335(6) ?
N41 C45 . 1.348(6) ?
C41 C42 . 1.367(7) ?
C41 H41 . 0.9300 ?
C42 C43 . 1.392(7) ?
C42 H42 . 0.9300 ?
C43 C44 . 1.389(7) ?
C43 C43 2_666 1.478(9) ?
C44 C45 . 1.369(7) ?
C44 H44 . 0.9300 ?
C45 H45 . 0.9300 ?
O51 N51 . 1.307(5) ?
N51 C51 . 1.343(7) ?
N51 C55 . 1.354(7) ?
C51 C52 . 1.359(7) ?
C51 H51 . 0.9300 ?
C52 C53 . 1.390(6) ?
C52 H52 . 0.9300 ?
C53 C54 . 1.388(7) ?
C53 C53 2_775 1.478(10) ?
C54 C55 . 1.378(8) ?
C54 H54 . 0.9300 ?
C55 H55 . 0.9300 ?
O1W H1WA . 0.85(5) ?
O1W H1WB . 0.85(5) ?
O2W H2WA . 0.85(5) ?
O2W H2WB . 0.85(5) ?
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
O2W H2WA O21 2_776 0.85(5) 1.88(5) 2.703(4) 164(5)
O1W H1WB O32 . 0.85(5) 1.81(5) 2.650(6) 167(5)
O1W H1WA O11 2_676 0.85(5) 1.97(5) 2.819(5) 176(5)
O2W H2WB O51 2_676 0.85(5) 1.94(5) 2.769(5) 166(5)
