#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/60/2206030.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_2206030
loop_
_publ_author_name
'Liu, San-Hui'
'Li, Yi-Zhi'
'Meng, Qing-Jin'
_publ_section_title
;catena-Poly[[[diaqua(6-carboxypyridine-2-carboxylato-κ³N,O,O')samarium(III)]-μ-pyridine-2,6-dicarboxylato-κ⁴N,O,O':O'']
 tetrahydrate]
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1111
_journal_page_last               m1113
_journal_paper_doi               10.1107/S1600536805012894
_journal_volume                  61
_journal_year                    2005
_chemical_formula_moiety         'C14 H11 N2 O10 Sm, 4H2 O'
_chemical_formula_sum            'C14 H19 N2 O14 Sm'
_chemical_formula_weight         589.66
_chemical_name_systematic
;
catena-Poly[[[diaqua(6-carboxypyridine-2-carboxylato-
κ³N,O,O')samarium(III)]-μ-pyridine-2,6-dicarboxylato-κ⁴N,O,O':O'']
tetrahydrate]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 102.367(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.973(3)
_cell_length_b                   11.203(2)
_cell_length_c                   12.830(3)
_cell_measurement_reflns_used    935
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.55
_cell_measurement_theta_min      2.35
_cell_volume                     1961.8(7)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_sigmaI/netI    0.0713
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10285
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.35
_exptl_absorpt_coefficient_mu    3.072
_exptl_absorpt_correction_T_max  0.69
_exptl_absorpt_correction_T_min  0.61
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.996
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1164
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.983
_refine_diff_density_min         -2.009
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         3846
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0842
_refine_ls_R_factor_gt           0.0622
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.09P)²+1.99P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1490
_refine_ls_wR_factor_ref         0.1560
_reflns_number_gt                2849
_reflns_number_total             3846
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ob6508.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 'Monoclinic' changed to 'monoclinic'
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_sg_symbol_H-M      'P 21/c'
_cod_database_code               2206030
_cod_database_fobs_code          2206030
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Sm1 0.73035(3) 0.79558(4) 0.35103(4) 0.03115(18) Uani d . 1 Sm
C1 0.5056(7) 0.6854(8) 0.3672(7) 0.0332(19) Uani d . 1 C
C2 0.4052(6) 0.6802(7) 0.3677(7) 0.0295(18) Uani d . 1 C
H2 0.3751 0.6067 0.3713 0.035 Uiso calc R 1 H
C3 0.3525(7) 0.7811(8) 0.3627(7) 0.0332(19) Uani d . 1 C
H3 0.2855 0.7780 0.3597 0.040 Uiso calc R 1 H
C4 0.4007(6) 0.8927(8) 0.3622(7) 0.0329(19) Uani d . 1 C
H4 0.3662 0.9640 0.3595 0.040 Uiso calc R 1 H
C5 0.4993(7) 0.8923(7) 0.3658(7) 0.0308(18) Uani d . 1 C
C6 0.5576(6) 1.0028(8) 0.3650(7) 0.0317(19) Uani d . 1 C
C7 0.5712(6) 0.5792(7) 0.3729(7) 0.0284(18) Uani d . 1 C
C8 0.8718(6) 1.0350(7) 0.4407(7) 0.0289(18) Uani d . 1 C
C9 0.9068(6) 1.1357(8) 0.5012(7) 0.0317(19) Uani d . 1 C
H9 0.9326 1.1998 0.4702 0.038 Uiso calc R 1 H
C10 0.9023(6) 1.1386(8) 0.6083(7) 0.0321(19) Uani d . 1 C
H10 0.9268 1.2036 0.6506 0.038 Uiso calc R 1 H
C11 0.8614(6) 1.0443(8) 0.6504(7) 0.0336(19) Uani d . 1 C
H11 0.8580 1.0439 0.7220 0.040 Uiso calc R 1 H
C12 0.8254(7) 0.9501(8) 0.5850(7) 0.0327(19) Uani d . 1 C
C13 0.8788(6) 1.0229(8) 0.3263(7) 0.0315(18) Uani d . 1 C
C14 0.7746(6) 0.8452(7) 0.6197(6) 0.0251(16) Uani d . 1 C
N1 0.5511(5) 0.7895(6) 0.3667(6) 0.0322(16) Uani d . 1 N
N2 0.8310(5) 0.9439(6) 0.4787(6) 0.0341(17) Uani d . 1 N
O1 0.6451(5) 0.9935(5) 0.3632(5) 0.0354(14) Uani d . 1 O
O2 0.5164(5) 1.0995(5) 0.3743(5) 0.0330(14) Uani d . 1 O
H2A 0.4741 1.1201 0.3074 0.049 Uiso d R 1 H
O3 0.6583(4) 0.6014(5) 0.3678(5) 0.0322(13) Uani d . 1 O
O4 0.5325(4) 0.4797(5) 0.3757(5) 0.0322(13) Uani d . 1 O
O5 0.7810(4) 0.8300(5) 0.7164(5) 0.0312(13) Uani d . 1 O
O6 0.7265(4) 0.7774(5) 0.5461(5) 0.0301(13) Uani d . 1 O
O7 0.8438(4) 0.9274(5) 0.2805(5) 0.0300(13) Uani d . 1 O
O8 0.9176(4) 1.1023(5) 0.2823(5) 0.0336(14) Uani d . 1 O
O9 0.8731(4) 0.6867(5) 0.4348(5) 0.0273(13) Uani d . 1 O
H9A 0.8541 0.6143 0.4650 0.041 Uiso d R 1 H
H9C 0.9109 0.6675 0.3828 0.041 Uiso d R 1 H
O10 0.6330(4) 0.8453(5) 0.1765(4) 0.0305(13) Uani d . 1 O
H10A 0.6709 0.8575 0.1338 0.037 Uiso d R 1 H
H10C 0.6000 0.9081 0.1811 0.037 Uiso d R 1 H
O11 0.9600(4) 0.8069(5) 0.1489(5) 0.0312(13) Uani d . 1 O
H11D 0.9372 0.7366 0.1494 0.037 Uiso d R 1 H
H11B 0.9186 0.8454 0.1757 0.037 Uiso d R 1 H
O12 0.8020(4) 0.4057(5) 0.4116(5) 0.0316(13) Uani d . 1 O
H12A 0.8158 0.4241 0.4773 0.038 Uiso d R 1 H
H12B 0.7402 0.3999 0.3905 0.038 Uiso d R 1 H
O13 0.6293(4) 0.2760(5) 0.3857(5) 0.0340(14) Uani d . 1 O
H13A 0.6327 0.2282 0.4379 0.041 Uiso d R 1 H
H13B 0.5815 0.3235 0.3834 0.041 Uiso d R 1 H
O14 0.9710(4) 0.0574(5) 0.0974(5) 0.0303(13) Uani d . 1 O
H14B 0.9546 0.0756 0.1640 0.036 Uiso d R 1 H
H14C 0.9845 -0.0163 0.0900 0.036 Uiso d 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'
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O9 Sm1 O10 . . 141.5(2) y
O9 Sm1 O3 . . 79.90(19) y
O10 Sm1 O3 . . 97.26(19) y
O9 Sm1 O5 . 4_575 71.6(2) y
O10 Sm1 O5 . 4_575 70.7(2) y
O3 Sm1 O5 . 4_575 74.65(19) y
O9 Sm1 O7 . . 86.04(18) y
O10 Sm1 O7 . . 78.56(19) y
O3 Sm1 O7 . . 151.38(19) y
O5 Sm1 O7 4_575 . 77.3(2) y
O9 Sm1 O6 . . 72.88(19) y
O10 Sm1 O6 . . 143.9(2) y
O3 Sm1 O6 . . 75.08(19) y
O5 Sm1 O6 4_575 . 136.45(19) y
O7 Sm1 O6 . . 124.2(2) y
O9 Sm1 N2 . . 75.5(2) y
O10 Sm1 N2 . . 124.8(2) y
O3 Sm1 N2 . . 135.5(2) y
O5 Sm1 N2 4_575 . 128.9(2) y
O7 Sm1 N2 . . 62.3(2) y
O6 Sm1 N2 . . 62.5(2) y
O9 Sm1 O1 . . 141.0(2) y
O10 Sm1 O1 . . 71.2(2) y
O3 Sm1 O1 . . 124.7(2) y
O5 Sm1 O1 4_575 . 139.1(2) y
O7 Sm1 O1 . . 81.21(18) y
O6 Sm1 O1 . . 84.23(19) y
N2 Sm1 O1 . . 65.8(2) y
O9 Sm1 N1 . . 133.5(2) y
O10 Sm1 N1 . . 73.3(2) y
O3 Sm1 N1 . . 62.4(2) y
O5 Sm1 N1 4_575 . 118.5(2) y
O7 Sm1 N1 . . 139.4(2) y
O6 Sm1 N1 . . 72.0(2) y
N2 Sm1 N1 . . 112.5(2) y
O1 Sm1 N1 . . 62.4(2) y
N1 C1 C2 . . 121.0(8) ?
N1 C1 C7 . . 114.2(8) ?
C2 C1 C7 . . 124.7(7) ?
C3 C2 C1 . . 120.1(8) ?
C3 C2 H2 . . 119.9 ?
C1 C2 H2 . . 119.9 ?
C2 C3 C4 . . 119.1(8) ?
C2 C3 H3 . . 120.5 ?
C4 C3 H3 . . 120.5 ?
C5 C4 C3 . . 118.2(8) ?
C5 C4 H4 . . 120.9 ?
C3 C4 H4 . . 120.9 ?
N1 C5 C4 . . 122.2(7) ?
N1 C5 C6 . . 114.5(8) ?
C4 C5 C6 . . 123.2(8) ?
O1 C6 O2 . . 123.9(8) ?
O1 C6 C5 . . 118.6(8) ?
O2 C6 C5 . . 117.3(8) ?
O4 C7 O3 . . 127.6(8) ?
O4 C7 C1 . . 116.7(7) ?
O3 C7 C1 . . 115.5(7) ?
N2 C8 C9 . . 123.4(8) ?
N2 C8 C13 . . 114.7(8) ?
C9 C8 C13 . . 121.9(7) ?
C10 C9 C8 . . 118.9(8) ?
C10 C9 H9 . . 120.6 ?
C8 C9 H9 . . 120.6 ?
C11 C10 C9 . . 119.0(8) ?
C11 C10 H10 . . 120.5 ?
C9 C10 H10 . . 120.5 ?
C10 C11 C12 . . 118.8(8) ?
C10 C11 H11 . . 120.6 ?
C12 C11 H11 . . 120.6 ?
C11 C12 N2 . . 123.3(8) ?
C11 C12 C14 . . 124.0(8) ?
N2 C12 C14 . . 112.7(7) ?
O8 C13 O7 . . 123.9(8) ?
O8 C13 C8 . . 120.5(8) ?
O7 C13 C8 . . 115.6(8) ?
O5 C14 O6 . . 124.8(7) ?
O5 C14 C12 . . 118.1(7) ?
O6 C14 C12 . . 117.1(7) ?
C1 N1 C5 . . 119.3(7) ?
C1 N1 Sm1 . . 120.1(6) ?
C5 N1 Sm1 . . 120.4(5) ?
C8 N2 C12 . . 116.6(8) ?
C8 N2 Sm1 . . 119.6(6) ?
C12 N2 Sm1 . . 121.9(6) ?
C6 O1 Sm1 . . 123.8(5) ?
C6 O2 H2A . . 109.5 ?
C7 O3 Sm1 . . 127.3(5) ?
C14 O5 Sm1 . 4_576 144.9(5) ?
C14 O6 Sm1 . . 124.2(5) ?
C13 O7 Sm1 . . 123.2(5) ?
Sm1 O9 H9A . . 109.7 ?
Sm1 O9 H9C . . 109.4 ?
H9A O9 H9C . . 109.5 ?
Sm1 O10 H10A . . 109.2 ?
Sm1 O10 H10C . . 109.4 ?
H10A O10 H10C . . 109.5 ?
H11D O11 H11B . . 100.3 ?
H12A O12 H12B . . 109.5 ?
H13A O13 H13B . . 109.5 ?
H14B O14 H14C . . 113.9 ?
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
Sm1 O9 . 2.388(5) y
Sm1 O10 . 2.423(6) y
Sm1 O3 . 2.426(6) y
Sm1 O5 4_575 2.446(6) y
Sm1 O7 . 2.476(6) y
Sm1 O6 . 2.524(6) y
Sm1 N2 . 2.537(8) y
Sm1 O1 . 2.537(6) y
Sm1 N1 . 2.556(7) y
C1 N1 . 1.330(11) ?
C1 C2 . 1.406(12) ?
C1 C7 . 1.493(12) ?
C2 C3 . 1.343(12) ?
C2 H2 . 0.9300 ?
C3 C4 . 1.421(12) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.369(12) ?
C4 H4 . 0.9300 ?
C5 N1 . 1.359(11) ?
C5 C6 . 1.483(11) ?
C6 O1 . 1.231(10) ?
C6 O2 . 1.244(11) ?
C7 O4 . 1.243(10) ?
C7 O3 . 1.257(10) ?
C8 N2 . 1.312(11) ?
C8 C9 . 1.397(12) ?
C8 C13 . 1.498(12) ?
C9 C10 . 1.389(12) ?
C9 H9 . 0.9300 ?
C10 C11 . 1.366(13) ?
C10 H10 . 0.9300 ?
C11 C12 . 1.374(12) ?
C11 H11 . 0.9300 ?
C12 N2 . 1.385(11) ?
C12 C14 . 1.489(12) ?
C13 O8 . 1.240(11) ?
C13 O7 . 1.267(11) ?
C14 O5 . 1.237(10) ?
C14 O6 . 1.283(10) ?
O2 H2A . 0.9600 ?
O5 Sm1 4_576 2.446(6) no
O9 H9A . 0.9601 ?
O9 H9C . 0.9600 ?
O10 H10A . 0.8501 ?
O10 H10C . 0.8500 ?
O11 H11D . 0.8500 ?
O11 H11B . 0.8500 ?
O12 H12A . 0.8500 ?
O12 H12B . 0.8501 ?
O13 H13A . 0.8500 ?
O13 H13B . 0.8499 ?
O14 H14B . 0.9539 ?
O14 H14C . 0.8566 ?
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 H2A O3 2_655 0.96 2.60 3.515(9) 161
O9 H9A O12 . 0.96 2.50 3.295(8) 140
O9 H9C O14 2_755 0.96 2.03 2.720(7) 127
O10 H10A O6 4_575 0.85 2.13 2.707(8) 125
O10 H10C O1 . 0.85 2.48 2.889(8) 111
O10 H10C O4 2_655 0.85 2.01 2.720(9) 141
O11 H11B O7 . 0.85 2.08 2.912(8) 164
O12 H12A O14 4_566 0.85 2.39 3.004(9) 130
O12 H12B O3 . 0.85 2.52 2.945(8) 112
O12 H12B O13 . 0.85 2.07 2.775(8) 140
O13 H13B O4 . 0.85 1.87 2.642(8) 150
O14 H14B O8 1_545 0.95 1.73 2.683(8) 176
O14 H14C O11 1_545 0.86 2.17 2.895(8) 142
