#------------------------------------------------------------------------------
#$Date: 2016-03-24 01:35:18 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179537 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/06/4500688.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4500688
loop_
_publ_author_name
'Luo, Geng-Geng'
'Xiong, Hong-Bo'
'Sun, Di'
'Wu, Dong-Liang'
'Huang, Rong-Bin'
'Dai, Jing-Cao'
_publ_section_title
;
 A Discrete Spirocyclic (H2O)9Cluster and 1D Novel Water Chain with
 Tetrameric and Octameric Clusters in Cationic Hosts
;
_journal_issue                   5
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              1948
_journal_paper_doi               10.1021/cg200111j
_journal_volume                  11
_journal_year                    2011
_chemical_formula_sum            'C28 H46 Ag2 N4 O13'
_chemical_formula_weight         862.43
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           70
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-F 2uv 2vw'
_symmetry_space_group_name_H-M   'F d d d :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                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.600(3)
_cell_length_b                   15.107(3)
_cell_length_c                   33.000(7)
_cell_measurement_temperature    173(2)
_cell_volume                     6780(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0238
_diffrn_reflns_av_sigmaI/netI    0.0183
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            7788
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.24
_exptl_absorpt_coefficient_mu    1.224
_exptl_absorpt_correction_T_max  0.8571
_exptl_absorpt_correction_T_min  0.7745
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_crystal_density_diffrn    1.690
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3520
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.297
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     114
_refine_ls_number_reflns         1481
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0221
_refine_ls_R_factor_gt           0.0207
_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)+(0.0281P)²+16.5074P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0532
_refine_ls_wR_factor_ref         0.0540
_reflns_number_gt                1404
_reflns_number_total             1481
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg200111j_si_001.cif
_cod_data_source_block           808722
_cod_original_sg_symbol_H-M      Fddd
_cod_database_code               4500688
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/4, -y+1/4, z'
'x, -y+1/4, -z+1/4'
'-x+1/4, y, -z+1/4'
'x, y+1/2, z+1/2'
'-x+1/4, -y+3/4, z+1/2'
'x, -y+3/4, -z+3/4'
'-x+1/4, y+1/2, -z+3/4'
'x+1/2, y, z+1/2'
'-x+3/4, -y+1/4, z+1/2'
'x+1/2, -y+1/4, -z+3/4'
'-x+3/4, y, -z+3/4'
'x+1/2, y+1/2, z'
'-x+3/4, -y+3/4, z'
'x+1/2, -y+3/4, -z+1/4'
'-x+3/4, y+1/2, -z+1/4'
'-x, -y, -z'
'x-1/4, y-1/4, -z'
'-x, y-1/4, z-1/4'
'x-1/4, -y, z-1/4'
'-x, -y+1/2, -z+1/2'
'x-1/4, y+1/4, -z+1/2'
'-x, y+1/4, z+1/4'
'x-1/4, -y+1/2, z+1/4'
'-x+1/2, -y, -z+1/2'
'x+1/4, y-1/4, -z+1/2'
'-x+1/2, y-1/4, z+1/4'
'x+1/4, -y, z+1/4'
'-x+1/2, -y+1/2, -z'
'x+1/4, y+1/4, -z'
'-x+1/2, y+1/4, z-1/4'
'x+1/4, -y+1/2, z-1/4'
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
Ag1 Ag 0.2500 0.2500 0.0000 0.03056(11) Uani 1 2 d S
O1 O 0.44219(10) 0.05246(10) 0.12971(5) 0.0374(4) Uani 1 1 d .
O1W O 0.52687(13) -0.10877(10) 0.11832(5) 0.0467(4) Uani 1 1 d .
H1WC H 0.5887 -0.1014 0.1202 0.056 Uiso 0.50 1 d PR
H1WB H 0.4975 -0.0610 0.1246 0.056 Uiso 1 1 d R
H1WA H 0.5092 -0.1506 0.1339 0.056 Uiso 0.50 1 d PR
O2W O 0.26345(10) 0.01284(10) 0.16127(5) 0.0358(4) Uani 1 1 d .
H2WA H 0.3214 0.0255 0.1535 0.043 Uiso 1 1 d R
H2WB H 0.2228 0.0523 0.1537 0.043 Uiso 0.50 1 d PR
H2WC H 0.2446 -0.0361 0.1512 0.043 Uiso 0.50 1 d PR
O3W O 0.1250 0.1250 0.1250 0.0350(7) Uani 1 4 d S
H3WA H 0.1670 0.0902 0.1355 0.042 Uiso 0.50 1 d PR
N1 N 0.40780(12) 0.26482(10) -0.00504(5) 0.0232(3) Uani 1 1 d .
C1 C 0.72350(14) 0.28099(15) -0.01445(7) 0.0312(4) Uani 1 1 d .
H1A H 0.7452 0.3424 -0.0090 0.037 Uiso 1 1 calc R
H1B H 0.7427 0.2661 -0.0426 0.037 Uiso 1 1 calc R
C2 C 0.61350(14) 0.27667(13) -0.01101(6) 0.0251(4) Uani 1 1 d .
C3 C 0.56424(13) 0.29561(12) 0.02513(6) 0.0246(4) Uani 1 1 d .
H3A H 0.6003 0.3132 0.0484 0.030 Uiso 1 1 calc R
C4 C 0.46332(13) 0.28867(12) 0.02690(6) 0.0232(4) Uani 1 1 d .
H4A H 0.4314 0.3013 0.0518 0.028 Uiso 1 1 calc R
C5 C 0.45495(15) 0.24753(13) -0.03985(6) 0.0298(5) Uani 1 1 d .
H5A H 0.4171 0.2312 -0.0629 0.036 Uiso 1 1 calc R
C6 C 0.55597(16) 0.25237(14) -0.04380(6) 0.0320(5) Uani 1 1 d .
H6A H 0.5860 0.2390 -0.0691 0.038 Uiso 1 1 calc R
C7 C 0.5922(3) 0.1258(3) 0.14296(12) 0.0333(10) Uani 0.50 1 d P
H7A H 0.5819 0.0810 0.1632 0.040 Uiso 0.50 1 d PR
H7B H 0.5859 0.1801 0.1578 0.040 Uiso 0.50 1 d PR
C8 C 0.4832(2) 0.1250 0.1250 0.0436(8) Uani 1 2 d S
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'
Ag Ag -0.8971 1.1015 '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'
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
N1 Ag1 N1 180.00(12) . 29
H1WC O1W H1WB 109.5 . .
H1WC O1W H1WA 109.5 . .
H1WB O1W H1WA 110.6 . .
H2WA O2W H2WB 110.9 . .
H2WA O2W H2WC 110.9 . .
H2WB O2W H2WC 107.4 . .
C5 N1 C4 117.05(17) . .
C5 N1 Ag1 121.32(13) . .
C4 N1 Ag1 121.59(13) . .
C2 C1 C1 113.5(2) . 29_655
C2 C1 H1A 108.9 . .
C1 C1 H1A 108.9 29_655 .
C2 C1 H1B 108.9 . .
C1 C1 H1B 108.9 29_655 .
H1A C1 H1B 107.7 . .
C6 C2 C3 116.76(18) . .
C6 C2 C1 121.01(18) . .
C3 C2 C1 122.23(18) . .
C4 C3 C2 119.89(17) . .
C4 C3 H3A 120.1 . .
C2 C3 H3A 120.1 . .
N1 C4 C3 123.09(17) . .
N1 C4 H4A 118.5 . .
C3 C4 H4A 118.5 . .
N1 C5 C6 123.08(18) . .
N1 C5 H5A 118.5 . .
C6 C5 H5A 118.5 . .
C5 C6 C2 120.12(18) . .
C5 C6 H6A 119.9 . .
C2 C6 H6A 119.9 . .
C7 C7 C7 89.97(3) 2_655 3
C7 C7 C7 53.1(3) 2_655 4_655
C7 C7 C7 37.0(3) 3 4_655
C7 C7 C8 158.13(17) 2_655 .
C7 C7 C8 68.21(14) 3 .
C7 C7 C8 105.2(4) 4_655 .
C7 C7 H7A 97.4 2_655 .
C7 C7 H7A 132.9 3 .
C7 C7 H7A 130.1 4_655 .
C8 C7 H7A 96.7 . .
C7 C7 H7B 96.4 2_655 .
C7 C7 H7B 121.8 3 .
C7 C7 H7B 117.5 4_655 .
C8 C7 H7B 96.5 . .
H7A C7 H7B 103.5 . .
O1 C8 O1 126.5(3) . 3
O1 C8 C7 112.2(2) . .
O1 C8 C7 117.2(2) 3 .
O1 C8 C7 117.2(2) . 3
O1 C8 C7 112.2(2) 3 3
C7 C8 C7 43.6(3) . 3
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ag1 N1 2.1642(17) .
Ag1 N1 2.1642(17) 29
O1 C8 1.2392(19) .
O1W H1WC 0.8501 .
O1W H1WB 0.8501 .
O1W H1WA 0.8499 .
O2W H2WA 0.8500 .
O2W H2WB 0.8499 .
O2W H2WC 0.8499 .
O3W H3WA 0.8501 .
N1 C5 1.341(3) .
N1 C4 1.346(2) .
C1 C2 1.502(3) .
C1 C1 1.519(4) 29_655
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C2 C6 1.385(3) .
C2 C3 1.397(3) .
C3 C4 1.378(3) .
C3 H3A 0.9500 .
C4 H4A 0.9500 .
C5 C6 1.382(3) .
C5 H5A 0.9500 .
C6 H6A 0.9500 .
C7 C7 0.892(7) 2_655
C7 C7 1.186(8) 3
C7 C7 1.484(7) 4_655
C7 C8 1.597(4) .
C7 H7A 0.9600 .
C7 H7B 0.9600 .
C8 O1 1.2392(19) 3
C8 C7 1.597(4) 3
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1WC O1W 0.85 1.87 2.705(4) 166.7 4_655
O1W H1WB O1 0.85 1.88 2.720(2) 169.8 .
O1W H1WA O2W 0.85 1.94 2.780(2) 167.0 14_545
O2W H2WA O1 0.85 1.87 2.712(2) 172.6 .
O3W H3WA O2W 0.85 1.95 2.8015(15) 178.1 .
O2W H2WC O1W 0.85 1.95 2.780(2) 166.7 14_545
O3W H3WA O2W 0.85 1.95 2.8015(15) 178.1 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
N1 Ag1 N1 C5 -61(100) 29 .
N1 Ag1 N1 C4 121(100) 29 .
C1 C1 C2 C6 -119.8(3) 29_655 .
C1 C1 C2 C3 59.4(3) 29_655 .
C6 C2 C3 C4 0.7(3) . .
C1 C2 C3 C4 -178.50(18) . .
C5 N1 C4 C3 -0.1(3) . .
Ag1 N1 C4 C3 177.59(13) . .
C2 C3 C4 N1 -0.6(3) . .
C4 N1 C5 C6 0.7(3) . .
Ag1 N1 C5 C6 -177.03(15) . .
N1 C5 C6 C2 -0.5(3) . .
C3 C2 C6 C5 -0.2(3) . .
C1 C2 C6 C5 179.04(19) . .
C7 C7 C8 O1 103(2) 2_655 .
C7 C7 C8 O1 106.8(4) 3 .
C7 C7 C8 O1 107.71(12) 4_655 .
C7 C7 C8 O1 -98(2) 2_655 3
C7 C7 C8 O1 -94.3(5) 3 3
C7 C7 C8 O1 -93.37(14) 4_655 3
C7 C7 C8 C7 -4.0(17) 2_655 3
C7 C7 C8 C7 0.9(4) 4_655 3
