#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/99/4319925.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_4319925
loop_
_publ_author_name
'Shao-Liang Zheng'
'Ming-Liang Tong'
'Ruo-Wen Fu'
'Xiao-Ming Chen'
'Seik-Weng Ng'
_publ_contact_author
;
      Chen, Xiao-Ming
      School of Chemistry and Chemical Engineering
      Zhongshan University
      Guangzhou, 510275
      P. R. China
;
_publ_contact_author_email       cescxm@zsu.edu.cn
_publ_contact_author_fax         '86 20 84112245'
_publ_contact_author_phone       86-20-84113986
_publ_section_title
;
 Toward Designed Assembly of Microporous Coordination Networks Constructed
 from Silver(I)-Hexamethylenetetramine Layers
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3562
_journal_page_last               3569
_journal_paper_doi               10.1021/ic001237z
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C13 H21 Ag N5 O6.5'
_chemical_formula_weight         459.22
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 94.250(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.621(2)
_cell_length_b                   23.534(7)
_cell_length_c                   10.414(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      7.5
_cell_volume                     1618.2(8)
_computing_cell_refinement       'SHELXTL-Plus (Sheldrick, 1990)'
_computing_data_collection       'SHELXTL-Plus (Sheldrick, 1990)'
_computing_data_reduction        'SHELXTL-Plus (Sheldrick, 1990)'
_computing_molecular_graphics    'SHELXTL V. 5.0 (Sheldrick, 1995)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Siemens R3m'
_diffrn_measurement_method       'ω scan'
_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  0.0251
_diffrn_reflns_av_sigmaI/netI    0.0375
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3101
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.14
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 200
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.293
_exptl_absorpt_correction_T_max  0.6977
_exptl_absorpt_correction_T_min  0.5757
_exptl_absorpt_correction_type   semi-empirical
_exptl_absorpt_process_details   'ψ-scans (North et al., 1968)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.885
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             932
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.692
_refine_diff_density_min         -0.723
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         2842
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0531P)²+1.9869P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0906
_refine_ls_wR_factor_ref         0.0987
_reflns_number_gt                2254
_reflns_number_total             2842
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001237z_3.cif
_cod_data_source_block           complex2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0531P)^2^+1.9869P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0531P)^2^+1.9869P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'C13 H21 Ag N5 O6.50'
_cod_database_code               4319925
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, 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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ag1 Ag 0.06773(5) 0.277583(16) 0.66382(3) 0.02987(14) Uani 1 d . . .
N1 N -0.2471(6) 0.23242(16) 0.5957(3) 0.0237(8) Uani 1 d . . .
N2 N -0.4359(6) 0.14308(16) 0.5742(3) 0.0267(9) Uani 1 d . . .
N3 N -0.4526(6) 0.21122(15) 0.3957(3) 0.0238(8) Uani 1 d . . .
N4 N -0.6198(5) 0.23286(15) 0.5923(3) 0.0214(8) Uani 1 d . . .
C1 C -0.2506(7) 0.1711(2) 0.6275(4) 0.0288(10) Uani 1 d . . .
H1A H -0.2388 0.1665 0.7194 0.080 Uiso 1 d R . .
H1B H -0.1361 0.1530 0.5935 0.080 Uiso 1 d R . .
C2 C -0.2657(7) 0.23771(19) 0.4531(4) 0.0253(10) Uani 1 d . . .
H2A H -0.1514 0.2198 0.4182 0.080 Uiso 1 d R . .
H2B H -0.2643 0.2772 0.4301 0.080 Uiso 1 d R . .
C3 C -0.4294(7) 0.2594(2) 0.6452(4) 0.0248(10) Uani 1 d . . .
H3A H -0.4308 0.2991 0.6234 0.080 Uiso 1 d R . .
H3B H -0.4206 0.2565 0.7374 0.080 Uiso 1 d R . .
C4 C -0.4516(7) 0.15029(19) 0.4328(4) 0.0281(10) Uani 1 d . . .
H4A H -0.5746 0.1326 0.3983 0.080 Uiso 1 d R . .
H4B H -0.3399 0.1315 0.3970 0.080 Uiso 1 d R . .
C5 C -0.6289(7) 0.2380(2) 0.4512(4) 0.0246(10) Uani 1 d . . .
H5A H -0.7497 0.2195 0.4156 0.080 Uiso 1 d R . .
H5B H -0.6369 0.2773 0.4271 0.080 Uiso 1 d R . .
C6 C -0.6111(7) 0.1712(2) 0.6255(4) 0.0277(10) Uani 1 d . . .
H6A H -0.6053 0.1666 0.7173 0.080 Uiso 1 d R . .
H6B H -0.7320 0.1530 0.5894 0.080 Uiso 1 d R . .
O1 O 0.2157(6) 0.37006(15) 0.6435(3) 0.0441(9) Uani 1 d . . .
O2 O 0.0671(6) 0.35094(15) 0.4501(4) 0.0451(9) Uani 1 d . . .
O3 O 0.4144(6) 0.62830(16) 0.6018(5) 0.0619(13) Uani 1 d . . .
O4 O 0.3526(7) 0.56931(19) 0.7489(5) 0.0648(13) Uani 1 d . . .
N5 N 0.3578(7) 0.58224(18) 0.6361(5) 0.0427(11) Uani 1 d . . .
C7 C 0.1574(7) 0.3836(2) 0.5293(5) 0.0307(11) Uani 1 d . . .
C8 C 0.2003(7) 0.44348(19) 0.4877(5) 0.0269(10) Uani 1 d . . .
C9 C 0.1757(7) 0.4592(2) 0.3587(5) 0.0348(12) Uani 1 d . . .
H9 H 0.1329 0.4314 0.2949 0.080 Uiso 1 d R . .
C10 C 0.2124(8) 0.5148(2) 0.3215(5) 0.0412(13) Uani 1 d . . .
H10 H 0.1960 0.5248 0.2320 0.080 Uiso 1 d R . .
C11 C 0.2714(7) 0.5553(2) 0.4110(6) 0.0386(13) Uani 1 d . . .
H11 H 0.2988 0.5936 0.3861 0.080 Uiso 1 d R . .
C12 C 0.2930(7) 0.5391(2) 0.5383(5) 0.0330(11) Uani 1 d . . .
C13 C 0.2602(7) 0.4843(2) 0.5791(5) 0.0285(10) Uani 1 d . . .
H13 H 0.2805 0.4747 0.6687 0.080 Uiso 1 d R . .
O1W O 0.5330(6) 0.3772(2) 0.8365(4) 0.0618(12) Uani 1 d . . .
H1WA H 0.5111 0.4104 0.8738 0.120 Uiso 1 d R . .
H1WB H 0.4340 0.3826 0.7709 0.120 Uiso 1 d R . .
O2W O 0.623(3) 0.4955(15) 1.0071(17) 0.43(2) Uani 0.75 d PU . .
H2WA H 0.5907 0.4660 0.9439 0.120 Uiso 0.75 d PR . .
H2WB H 0.6389 0.4830 1.0837 0.120 Uiso 0.75 d PR . .
O3W O 0.999(5) 0.5225(5) 0.9676(14) 0.376(17) Uani 0.75 d PU . .
H3WA H 0.8807 0.5103 0.9786 0.120 Uiso 0.75 d PR . .
H3WB H 1.0034 0.5580 0.9829 0.120 Uiso 0.75 d PR . .
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'
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
_geom_angle_publ_flag
N1 Ag1 O1 136.57(13) . . ?
N1 Ag1 N3 103.28(12) . 4_666 ?
O1 Ag1 N3 92.42(12) . 4_666 ?
N1 Ag1 N4 116.63(12) . 1_655 ?
O1 Ag1 N4 90.18(13) . 1_655 ?
N3 Ag1 N4 116.74(12) 4_666 1_655 ?
C1 N1 C2 107.7(3) . . ?
C1 N1 C3 108.2(3) . . ?
C2 N1 C3 107.5(3) . . ?
C1 N1 Ag1 113.2(3) . . ?
C2 N1 Ag1 105.3(3) . . ?
C3 N1 Ag1 114.7(3) . . ?
C1 N2 C6 108.7(3) . . ?
C1 N2 C4 108.7(4) . . ?
C6 N2 C4 108.1(3) . . ?
C2 N3 C5 108.9(3) . . ?
C2 N3 C4 108.4(3) . . ?
C5 N3 C4 107.3(3) . . ?
C2 N3 Ag1 104.4(2) . 4_565 ?
C5 N3 Ag1 116.3(3) . 4_565 ?
C4 N3 Ag1 111.2(2) . 4_565 ?
C5 N4 C3 107.9(3) . . ?
C5 N4 C6 108.0(3) . . ?
C3 N4 C6 108.0(3) . . ?
C5 N4 Ag1 106.9(2) . 1_455 ?
C3 N4 Ag1 114.6(3) . 1_455 ?
C6 N4 Ag1 111.2(2) . 1_455 ?
N2 C1 N1 112.3(3) . . ?
N3 C2 N1 112.0(3) . . ?
N4 C3 N1 112.4(3) . . ?
N2 C4 N3 111.6(3) . . ?
N4 C5 N3 112.3(3) . . ?
N2 C6 N4 111.8(3) . . ?
C7 O1 Ag1 102.3(3) . . ?
C7 O1 O1W 145.2(3) . . ?
Ag1 O1 O1W 106.25(16) . . ?
O3 N5 O4 122.7(5) . . ?
O3 N5 C12 119.5(5) . . ?
O4 N5 C12 117.7(4) . . ?
O2 C7 O1 124.4(5) . . ?
O2 C7 C8 118.5(4) . . ?
O1 C7 C8 117.0(4) . . ?
C13 C8 C9 119.0(4) . . ?
C13 C8 C7 120.0(4) . . ?
C9 C8 C7 121.0(4) . . ?
C10 C9 C8 120.6(5) . . ?
C11 C10 C9 120.8(5) . . ?
C10 C11 C12 117.8(5) . . ?
C11 C12 C13 123.2(5) . . ?
C11 C12 N5 118.4(5) . . ?
C13 C12 N5 118.3(5) . . ?
C12 C13 C8 118.6(5) . . ?
O1 O1W O2W 121.8(4) . . ?
O1 O1W O2W 98.6(3) . 3_667 ?
O2W O1W O2W 26.9(5) . 3_667 ?
O2W O2W O3W 154(3) 3_667 . ?
O2W O2W O4 97.8(16) 3_667 3_667 ?
O3W O2W O4 105.4(7) . 3_667 ?
O2W O2W O1W 86(2) 3_667 . ?
O3W O2W O1W 104.6(9) . . ?
O4 O2W O1W 91.3(9) 3_667 . ?
O3W O3W O2W 72(3) 3_767 . ?
O3W O3W N2 155(2) 3_767 2_556 ?
O2W O3W N2 97.6(12) . 2_556 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ag1 N1 2.400(4) . ?
Ag1 O1 2.403(4) . ?
Ag1 N3 2.442(3) 4_666 ?
Ag1 N4 2.484(4) 1_655 ?
N1 C1 1.482(6) . ?
N1 C2 1.487(5) . ?
N1 C3 1.490(6) . ?
N2 C1 1.465(6) . ?
N2 C6 1.470(6) . ?
N2 C4 1.478(6) . ?
N3 C2 1.472(6) . ?
N3 C5 1.481(6) . ?
N3 C4 1.485(6) . ?
N3 Ag1 2.442(3) 4_565 ?
N4 C5 1.472(5) . ?
N4 C3 1.477(5) . ?
N4 C6 1.492(6) . ?
N4 Ag1 2.484(3) 1_455 ?
O1 C7 1.264(6) . ?
O1 O1W 2.803(6) . ?
O2 C7 1.246(6) . ?
O3 N5 1.210(6) . ?
O4 N5 1.217(6) . ?
N5 C12 1.479(7) . ?
C7 C8 1.508(6) . ?
C8 C13 1.390(7) . ?
C8 C9 1.391(7) . ?
C9 C10 1.390(7) . ?
C10 C11 1.370(8) . ?
C11 C12 1.377(7) . ?
C12 C13 1.379(7) . ?
O1W O2W 3.33(3) . ?
O1W O2W 3.60(3) 3_667 ?
O2W O2W 1.63(4) 3_667 ?
O2W O3W 2.63(4) . ?
O2W O4 2.96(2) 3_667 ?
O3W O3W 1.26(2) 3_767 ?
O3W N2 2.896(12) 2_556 ?
