#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:54:45 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179430 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/27/4332754.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_4332754
loop_
_publ_author_name
'Gu, Xiaojun'
'Xue, Dongfeng'
_publ_section_title
;
 Spontaneously Resolved Homochiral 3D Lanthanide−Silver
 Heterometallic Coordination Framework with Extended Helical
 Ln−O−Ag Subunits
;
_journal_issue                   23
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9257
_journal_page_last               9261
_journal_paper_doi               10.1021/ic060806l
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C20 H15 Ag N3 Nd O8'
_chemical_formula_weight         677.46
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           178
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 61 2 (0 0 5)'
_symmetry_space_group_name_H-M   'P 61 2 2'
_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                120.00
_cell_formula_units_Z            6
_cell_length_a                   11.8241(8)
_cell_length_b                   11.8241(8)
_cell_length_c                   27.418(3)
_cell_measurement_temperature    293(2)
_cell_volume                     3319.7(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0705
_diffrn_reflns_av_sigmaI/netI    0.0487
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            20719
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    3.257
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    2.033
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1962
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.419
_refine_diff_density_min         -0.484
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_coef       0.00029(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         2746
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0323
_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)+(0.0254P)²+0.1460P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0568
_refine_ls_wR_factor_ref         0.0618
_reflns_number_gt                2239
_reflns_number_total             2746
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060806lsup2.cif
_cod_data_source_block           ds2
_cod_original_cell_volume        3319.8(5)
_cod_original_sg_symbol_H-M      P6(1)22
_cod_database_code               4332754
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'x-y, x, z+1/6'
'y, -x+y, z+5/6'
'x-y, -y, -z'
'-x, -x+y, -z+2/3'
'y, x, -z+1/3'
'-y, -x, -z+5/6'
'x, x-y, -z+1/6'
'-x+y, y, -z+1/2'
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
Nd1 Nd 1.13372(3) 1.0000 0.0000 0.02649(10) Uani 1 2 d S
Ag1 Ag 1.24115(3) 0.75885(3) -0.0833 0.04011(15) Uani 1 2 d S
O4 O 1.2837(3) 0.9175(3) -0.02469(12) 0.0426(9) Uani 1 1 d .
O3 O 1.0047(4) 1.0685(4) -0.04630(12) 0.0533(10) Uani 1 1 d .
C10 C 0.9415(3) 1.0585(3) -0.0833 0.0377(17) Uani 1 2 d S
N1 N 1.4253(4) 0.8023(5) -0.12716(15) 0.0508(13) Uani 1 1 d .
C5 C 1.5124(6) 0.7698(6) -0.11358(17) 0.0487(14) Uani 1 1 d .
H6 H 1.5077 0.7400 -0.0818 0.058 Uiso 1 1 calc R
C9 C 0.8679(3) 1.1321(3) -0.0833 0.0420(16) Uani 1 2 d S
C4 C 1.6089(6) 0.7768(6) -0.14293(17) 0.0443(15) Uani 1 1 d .
H3 H 1.6671 0.7520 -0.1312 0.053 Uiso 1 1 calc R
C8 C 0.8707(7) 1.2056(6) -0.0436(2) 0.0621(18) Uani 1 1 d .
H2 H 0.9173 1.2093 -0.0157 0.074 Uiso 1 1 calc R
C12 C 1.3796(6) 1.0000 0.0000 0.0417(17) Uani 1 2 d S
C1 C 1.4340(7) 0.8432(9) -0.1728(2) 0.093(3) Uani 1 1 d .
H9 H 1.3732 0.8652 -0.1840 0.111 Uiso 1 1 calc R
N2 N 0.7305(4) 1.2695(4) -0.0833 0.096(3) Uani 1 2 d S
C7 C 0.8036(8) 1.2736(9) -0.0457(3) 0.091(3) Uani 1 1 d .
H11 H 0.8100 1.3255 -0.0191 0.109 Uiso 1 1 calc R
C11 C 1.5055(7) 1.0000 0.0000 0.089(4) Uani 1 2 d S
H12A H 1.5673 1.0695 0.0204 0.133 Uiso 0.50 1 calc PR
H12B H 1.5388 1.0126 -0.0327 0.133 Uiso 0.50 1 calc PR
H12C H 1.4915 0.9179 0.0123 0.133 Uiso 0.50 1 calc PR
C2 C 1.5297(7) 0.8540(9) -0.2043(2) 0.084(3) Uani 1 1 d .
H1A H 1.5330 0.8845 -0.2358 0.101 Uiso 1 1 calc R
C3 C 1.6194(5) 0.8211(5) -0.19014(16) 0.0337(12) Uani 1 1 d .
C6 C 1.7219(5) 0.8296(5) -0.22504(17) 0.0367(13) Uani 1 1 d .
O2 O 1.7204(3) 0.8680(4) -0.26720(11) 0.0444(9) Uani 1 1 d .
O1 O 1.8020(3) 0.7988(4) -0.20873(11) 0.0417(9) Uani 1 1 d .
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'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 '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_1
_geom_angle_site_symmetry_3
O1 Nd1 O1 161.87(18) 5_545 10_784
O1 Nd1 O3 83.20(12) 5_545 7_675
O1 Nd1 O3 82.33(12) 10_784 7_675
O1 Nd1 O3 82.33(12) 5_545 .
O1 Nd1 O3 83.20(12) 10_784 .
O3 Nd1 O3 73.83(18) 7_675 .
O1 Nd1 O4 124.28(12) 5_545 7_675
O1 Nd1 O4 73.80(12) 10_784 7_675
O3 Nd1 O4 132.61(11) 7_675 7_675
O3 Nd1 O4 139.93(13) . 7_675
O1 Nd1 O4 73.80(12) 5_545 .
O1 Nd1 O4 124.28(12) 10_784 .
O3 Nd1 O4 139.93(13) 7_675 .
O3 Nd1 O4 132.61(11) . .
O4 Nd1 O4 51.17(15) 7_675 .
O1 Nd1 O2 102.56(11) 5_545 8_874
O1 Nd1 O2 83.65(12) 10_784 8_874
O3 Nd1 O2 145.71(13) 7_675 8_874
O3 Nd1 O2 73.54(12) . 8_874
O4 Nd1 O2 71.70(12) 7_675 8_874
O4 Nd1 O2 72.64(12) . 8_874
O1 Nd1 O2 83.65(12) 5_545 3_755
O1 Nd1 O2 102.56(11) 10_784 3_755
O3 Nd1 O2 73.54(12) 7_675 3_755
O3 Nd1 O2 145.71(13) . 3_755
O4 Nd1 O2 72.64(12) 7_675 3_755
O4 Nd1 O2 71.70(12) . 3_755
O2 Nd1 O2 140.31(18) 8_874 3_755
O1 Nd1 C12 99.06(9) 5_545 .
O1 Nd1 C12 99.06(9) 10_784 .
O3 Nd1 C12 143.08(9) 7_675 .
O3 Nd1 C12 143.08(9) . .
O4 Nd1 C12 25.58(8) 7_675 .
O4 Nd1 C12 25.58(8) . .
O2 Nd1 C12 70.15(9) 8_874 .
O2 Nd1 C12 70.15(9) 3_755 .
N1 Ag1 N1 102.8(2) 10_774 .
N1 Ag1 O4 104.90(14) 10_774 .
N1 Ag1 O4 112.38(15) . .
N1 Ag1 O4 112.38(15) 10_774 10_774
N1 Ag1 O4 104.90(14) . 10_774
O4 Ag1 O4 118.55(17) . 10_774
C12 O4 Ag1 138.0(4) . .
C12 O4 Nd1 95.2(4) . .
Ag1 O4 Nd1 126.19(14) . .
C10 O3 Nd1 149.0(4) . .
O3 C10 O3 127.4(7) . 10_774
O3 C10 C9 116.3(3) . .
O3 C10 C9 116.3(3) 10_774 .
C5 N1 C1 116.3(5) . .
C5 N1 Ag1 125.1(4) . .
C1 N1 Ag1 117.7(4) . .
N1 C5 C4 124.5(5) . .
N1 C5 H6 117.8 . .
C4 C5 H6 117.8 . .
C8 C9 C8 116.9(7) . 10_774
C8 C9 C10 121.5(4) . .
C8 C9 C10 121.5(4) 10_774 .
C5 C4 C3 119.4(5) . .
C5 C4 H3 120.3 . .
C3 C4 H3 120.3 . .
C9 C8 C7 119.4(6) . .
C9 C8 H2 120.3 . .
C7 C8 H2 120.3 . .
O4 C12 O4 118.4(7) . 7_675
O4 C12 C11 120.8(3) . .
O4 C12 C11 120.8(3) 7_675 .
O4 C12 Nd1 59.2(3) . .
O4 C12 Nd1 59.2(3) 7_675 .
C11 C12 Nd1 180.000(1) . .
N1 C1 C2 122.3(5) . .
N1 C1 H9 118.8 . .
C2 C1 H9 118.8 . .
C7 N2 C7 115.9(9) . 10_774
N2 C7 C8 124.1(7) . .
N2 C7 H11 117.9 . .
C8 C7 H11 117.9 . .
C12 C11 H12A 109.5 . .
C12 C11 H12B 109.5 . .
H12A C11 H12B 109.5 . .
C12 C11 H12C 109.5 . .
H12A C11 H12C 109.5 . .
H12B C11 H12C 109.5 . .
C3 C2 C1 121.3(5) . .
C3 C2 H1A 119.4 . .
C1 C2 H1A 119.4 . .
C2 C3 C4 116.3(5) . .
C2 C3 C6 121.1(5) . .
C4 C3 C6 122.6(5) . .
O2 C6 O1 125.9(5) . .
O2 C6 C3 117.2(5) . .
O1 C6 C3 116.9(4) . .
C6 O2 Nd1 122.2(3) . 4_774
C6 O1 Nd1 147.2(3) . 6_664
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Nd1 O1 2.362(3) 5_545
Nd1 O1 2.362(3) 10_784
Nd1 O3 2.414(3) 7_675
Nd1 O3 2.414(3) .
Nd1 O4 2.507(3) 7_675
Nd1 O4 2.507(3) .
Nd1 O2 2.510(3) 8_874
Nd1 O2 2.510(3) 3_755
Nd1 C12 2.907(7) .
Ag1 N1 2.309(4) 10_774
Ag1 N1 2.309(4) .
Ag1 O4 2.327(3) .
Ag1 O4 2.327(3) 10_774
O4 C12 1.260(5) .
O3 C10 1.231(4) .
C10 O3 1.231(4) 10_774
C10 C9 1.507(9) .
N1 C5 1.320(7) .
N1 C1 1.328(6) .
C5 C4 1.365(7) .
C5 H6 0.9300 .
C9 C8 1.383(6) .
C9 C8 1.383(6) 10_774
C4 C3 1.378(6) .
C4 H3 0.9300 .
C8 C7 1.386(9) .
C8 H2 0.9300 .
C12 O4 1.260(5) 7_675
C12 C11 1.489(10) .
C1 C2 1.377(7) .
C1 H9 0.9300 .
N2 C7 1.331(8) .
N2 C7 1.331(8) 10_774
C7 H11 0.9300 .
C11 H12A 0.9600 .
C11 H12B 0.9600 .
C11 H12C 0.9600 .
C2 C3 1.356(7) .
C2 H1A 0.9300 .
C3 C6 1.507(7) .
C6 O2 1.245(5) .
C6 O1 1.256(6) .
O2 Nd1 2.510(3) 4_774
O1 Nd1 2.362(3) 6_664
