#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/27/2222744.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_2222744
loop_
_publ_author_name
'Guan, Biao'
'Zhang, Chao-Hua'
'Song, Wen-Dong'
_publ_section_title
Poly[pentaaquatetrakis(μ₂-nicotinato-κ²N:O)(perchlorato-κO)lanthanum(III)disilver(I)]
_journal_coeditor_code           HY2200
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m896
_journal_page_last               m897
_journal_paper_doi               10.1107/S1600536809026130
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Ag2 La (C6 H4 N O2)4 (Cl O4) (H2 O)5]'
_chemical_formula_moiety         'C24 H26 Ag2 Cl La N4 O17'
_chemical_formula_sum            'C24 H26 Ag2 Cl La N4 O17'
_chemical_formula_weight         1032.59
_chemical_name_systematic
;
Poly[pentaaquatetrakis(μ₂-nicotinato-κ²N:O)(perchlorato-
κO)lanthanum(III)disilver(I)]
;
_space_group_IT_number           64
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2ac 2'
_symmetry_space_group_name_H-M   'C m c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   35.140(5)
_cell_length_b                   12.3371(16)
_cell_length_c                   15.046(2)
_cell_measurement_reflns_used    3600
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      1.36
_cell_volume                     6522.8(15)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics
'SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_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  0.0671
_diffrn_reflns_av_sigmaI/netI    0.0485
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15911
_diffrn_reflns_theta_full        25.20
_diffrn_reflns_theta_max         25.20
_diffrn_reflns_theta_min         2.21
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.639
_exptl_absorpt_correction_T_max  0.567
_exptl_absorpt_correction_T_min  0.465
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.103
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4016
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.900
_refine_diff_density_min         -0.965
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.946
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         2999
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.952
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0488
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0867
_refine_ls_wR_factor_ref         0.0896
_reflns_number_gt                2251
_reflns_number_total             2999
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hy2200.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_sg_symbol_Hall     '-C 2bc 2'
_cod_database_code               2222744
_cod_database_fobs_code          2222744
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y-1/2, -z-1/2'
'x, -y-1/2, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y, -z-1/2'
'x+1/2, -y, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
La La1 0.2500 1.08273(5) 0.2500 0.02358(16) Uani d S 1 . .
Ag Ag1 0.389767(18) 0.60965(6) 0.56481(4) 0.0465(2) Uani d . 1 . .
C C1 0.3039(2) 0.9196(6) 0.3991(4) 0.0299(18) Uani d . 1 . .
C C2 0.34312(19) 0.8866(6) 0.4214(5) 0.0318(18) Uani d . 1 . .
C C3 0.3495(2) 0.7964(6) 0.4729(4) 0.0331(19) Uani d . 1 . .
H H3 0.3287 0.7591 0.4956 0.040 Uiso calc R 1 . .
C C4 0.4138(2) 0.8140(8) 0.4627(5) 0.053(3) Uani d . 1 . .
H H4 0.4380 0.7896 0.4770 0.064 Uiso calc R 1 . .
C C5 0.4097(2) 0.9060(8) 0.4114(7) 0.071(3) Uani d . 1 . .
H H5 0.4311 0.9430 0.3913 0.085 Uiso calc R 1 . .
C C6 0.3744(2) 0.9422(7) 0.3905(5) 0.048(2) Uani d . 1 . .
H H6 0.3714 1.0039 0.3557 0.057 Uiso calc R 1 . .
C C7 0.4322(2) 0.4349(7) 0.6693(6) 0.054(3) Uani d . 1 . .
H H7 0.4534 0.4729 0.6489 0.065 Uiso calc R 1 . .
C C8 0.3685(2) 0.4135(6) 0.6768(5) 0.0313(18) Uani d . 1 . .
H H8 0.3444 0.4376 0.6605 0.038 Uiso calc R 1 . .
C C9 0.37074(19) 0.3248(6) 0.7314(4) 0.0288(18) Uani d . 1 . .
C C10 0.4064(2) 0.2925(7) 0.7546(6) 0.060(3) Uani d . 1 . .
H H10 0.4098 0.2331 0.7919 0.072 Uiso calc R 1 . .
C C11 0.4374(2) 0.3480(8) 0.7226(7) 0.078(4) Uani d . 1 . .
H H11 0.4619 0.3257 0.7375 0.094 Uiso calc R 1 . .
C C12 0.3359(2) 0.2677(6) 0.7620(5) 0.0292(17) Uani d . 1 . .
N N1 0.38410(17) 0.7606(5) 0.4913(4) 0.0369(16) Uani d . 1 . .
N N2 0.39810(17) 0.4670(5) 0.6458(4) 0.0375(16) Uani d . 1 . .
O O1 0.30034(13) 0.9960(4) 0.3448(3) 0.0366(13) Uani d . 1 . .
O O2 0.27688(13) 0.8707(4) 0.4351(3) 0.0331(13) Uani d . 1 . .
O O3 0.30462(12) 0.3020(4) 0.7338(3) 0.0328(12) Uani d . 1 . .
O O4 0.33989(13) 0.1890(5) 0.8112(3) 0.0432(15) Uani d . 1 . .
O O1W 0.28251(13) 0.9406(4) 0.1593(3) 0.0373(14) Uani d . 1 . .
H H1W 0.2679 0.9115 0.1204 0.056 Uiso d R 1 . .
H H2W 0.2983 0.8959 0.1795 0.056 Uiso d R 1 . .
O O2W 0.24825(13) 1.1647(4) 0.4015(3) 0.0478(14) Uani d . 1 . .
H H3W 0.2385 1.2269 0.4029 0.072 Uiso d R 1 . .
H H4W 0.2620 1.1535 0.4461 0.072 Uiso d R 1 . .
O O3W 0.32305(14) 0.5000 0.5000 0.074(3) Uani d SDU 1 . .
H H5W 0.3086 0.5297 0.5356 0.111 Uiso d RD 1 . .
Cl Cl1 0.5030(4) 0.6862(4) 0.5923(4) 0.0816(15) Uani d PRDU 0.50 A -1
O O5 0.5071(4) 0.8007(6) 0.5862(9) 0.118(3) Uani d PRDU 0.50 A -1
O O6 0.4640(3) 0.6544(14) 0.5835(10) 0.118(3) Uani d PRDU 0.50 A -1
O O7 0.5133(4) 0.6545(12) 0.6849(7) 0.118(3) Uani d PRDU 0.50 A -1
O O8 0.5275(4) 0.6292(12) 0.5351(9) 0.118(3) Uani d PRDU 0.50 A -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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -0.2871 2.4523 '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
O3 La1 O3 13_566 11_575 107.4(2) ?
O3 La1 O2W 13_566 7_545 82.65(16) ?
O3 La1 O2W 11_575 7_545 69.35(15) ?
O3 La1 O2W 13_566 . 69.35(15) ?
O3 La1 O2W 11_575 . 82.65(16) ?
O2W La1 O2W 7_545 . 132.1(2) ?
O3 La1 O1W 13_566 . 146.78(15) ?
O3 La1 O1W 11_575 . 89.71(15) ?
O2W La1 O1W 7_545 . 76.96(16) ?
O2W La1 O1W . . 142.66(15) ?
O3 La1 O1W 13_566 7_545 89.71(15) ?
O3 La1 O1W 11_575 7_545 146.78(15) ?
O2W La1 O1W 7_545 7_545 142.66(15) ?
O2W La1 O1W . 7_545 76.96(16) ?
O1W La1 O1W . 7_545 90.8(2) ?
O3 La1 O1 13_566 7_545 75.34(16) ?
O3 La1 O1 11_575 7_545 139.26(15) ?
O2W La1 O1 7_545 7_545 70.81(16) ?
O2W La1 O1 . 7_545 132.40(16) ?
O1W La1 O1 . 7_545 73.32(16) ?
O1W La1 O1 7_545 7_545 71.89(16) ?
O3 La1 O1 13_566 . 139.26(15) ?
O3 La1 O1 11_575 . 75.34(16) ?
O2W La1 O1 7_545 . 132.40(16) ?
O2W La1 O1 . . 70.81(16) ?
O1W La1 O1 . . 71.89(16) ?
O1W La1 O1 7_545 . 73.32(16) ?
O1 La1 O1 7_545 . 129.6(2) ?
N2 Ag1 N1 . . 175.3(2) ?
N2 Ag1 Ag1 . 4_566 70.66(16) ?
N1 Ag1 Ag1 . 4_566 113.42(17) ?
O6 Ag1 N2 . . 88.67(6) ?
O6 Ag1 N1 . . 88.06(7) ?
O3W Ag1 N1 . . 98.95(17) ?
O3W Ag1 N2 . . 85.33(16) ?
O3W Ag1 O6 . . 157.70(7) ?
O1 C1 O2 . . 124.7(7) ?
O1 C1 C2 . . 116.7(7) ?
O2 C1 C2 . . 118.6(7) ?
C6 C2 C3 . . 117.6(7) ?
C6 C2 C1 . . 122.1(7) ?
C3 C2 C1 . . 120.3(7) ?
N1 C3 C2 . . 122.5(7) ?
N1 C3 H3 . . 118.7 ?
C2 C3 H3 . . 118.7 ?
N1 C4 C5 . . 121.1(8) ?
N1 C4 H4 . . 119.5 ?
C5 C4 H4 . . 119.5 ?
C4 C5 C6 . . 119.8(8) ?
C4 C5 H5 . . 120.1 ?
C6 C5 H5 . . 120.1 ?
C2 C6 C5 . . 119.2(8) ?
C2 C6 H6 . . 120.4 ?
C5 C6 H6 . . 120.4 ?
N2 C7 C11 . . 121.5(8) ?
N2 C7 H7 . . 119.2 ?
C11 C7 H7 . . 119.2 ?
N2 C8 C9 . . 124.5(7) ?
N2 C8 H8 . . 117.8 ?
C9 C8 H8 . . 117.8 ?
C10 C9 C8 . . 116.2(7) ?
C10 C9 C12 . . 122.7(7) ?
C8 C9 C12 . . 121.1(6) ?
C9 C10 C11 . . 119.7(8) ?
C9 C10 H10 . . 120.2 ?
C11 C10 H10 . . 120.2 ?
C7 C11 C10 . . 119.7(8) ?
C7 C11 H11 . . 120.1 ?
C10 C11 H11 . . 120.1 ?
O4 C12 O3 . . 124.7(7) ?
O4 C12 C9 . . 117.9(7) ?
O3 C12 C9 . . 117.4(7) ?
C4 N1 C3 . . 119.7(7) ?
C4 N1 Ag1 . . 121.8(5) ?
C3 N1 Ag1 . . 118.5(5) ?
C7 N2 C8 . . 118.4(7) ?
C7 N2 Ag1 . . 121.4(5) ?
C8 N2 Ag1 . . 120.0(5) ?
C1 O1 La1 . . 139.5(5) ?
C12 O3 La1 . 13_566 150.2(5) ?
La1 O1W H1W . . 113.1 ?
La1 O1W H2W . . 124.4 ?
H1W O1W H2W . . 111.6 ?
La1 O2W H3W . . 113.8 ?
La1 O2W H4W . . 130.5 ?
H3W O2W H4W . . 111.4 ?
O8 Cl1 O5 . . 113.3 ?
O8 Cl1 O6 . . 113.1 ?
O5 Cl1 O6 . . 111.3 ?
O8 Cl1 O7 . . 106.8 ?
O5 Cl1 O7 . . 107.2 ?
O6 Cl1 O7 . . 104.5 ?
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
La1 O1 . 2.511(5) y
La1 O3 11_575 2.401(4) y
La1 O1W . 2.498(5) y
La1 O2W . 2.494(4) y
Ag1 N1 . 2.175(6) y
Ag1 N2 . 2.161(6) y
Ag1 O6 . 2.681(2) y
Ag1 O3W . 2.877(6) y
Ag1 Ag1 4_566 3.3352(14) y
C1 O1 . 1.254(8) ?
C1 O2 . 1.249(8) ?
C1 C2 . 1.475(9) ?
C2 C6 . 1.378(10) ?
C2 C3 . 1.373(10) ?
C3 N1 . 1.324(8) ?
C3 H3 . 0.9300 ?
C4 N1 . 1.306(9) ?
C4 C5 . 1.379(11) ?
C4 H4 . 0.9300 ?
C5 C6 . 1.354(10) ?
C5 H5 . 0.9300 ?
C6 H6 . 0.9300 ?
C7 N2 . 1.312(9) ?
C7 C11 . 1.352(11) ?
C7 H7 . 0.9300 ?
C8 N2 . 1.317(8) ?
C8 C9 . 1.371(10) ?
C8 H8 . 0.9300 ?
C9 C10 . 1.360(9) ?
C9 C12 . 1.484(10) ?
C10 C11 . 1.375(11) ?
C10 H10 . 0.9300 ?
C11 H11 . 0.9300 ?
C12 O4 . 1.230(8) ?
C12 O3 . 1.253(8) ?
O3 La1 13_566 2.401(4) ?
O1W H1W . 0.8564 ?
O1W H2W . 0.8388 ?
O2W H3W . 0.8404 ?
O2W H4W . 0.8395 ?
O3W H5W . 0.8241 ?
Cl1 O8 . 1.4076 ?
Cl1 O5 . 1.4226 ?
Cl1 O6 . 1.4309 ?
Cl1 O7 . 1.4925 ?
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
_geom_hbond_publ_flag
O1W H1W O2 7_545 0.86 1.85 2.667(6) 159 y
O1W H2W O4 4_566 0.84 1.80 2.611(7) 161 y
O2W H3W O2 16 0.84 1.92 2.738(7) 165 y
O2W H4W O2 4_576 0.84 1.89 2.693(7) 161 y
O3W H5W O1W 11_576 0.82 2.11 2.883(5) 157 y
