#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/99/4319924.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_4319924
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                 93.38
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.604(2)
_cell_length_b                   24.078(10)
_cell_length_c                   10.514(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      7.5
_cell_volume                     1668.9(13)
_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 0.976
_diffrn_measured_fraction_theta_max 0.976
_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  0.0382
_diffrn_reflns_av_sigmaI/netI    0.0443
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4172
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.12
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 200
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.254
_exptl_absorpt_correction_T_max  0.7203
_exptl_absorpt_correction_T_min  0.5617
_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    1.828
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             932
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.573
_refine_diff_density_min         -0.862
_refine_diff_density_rms         0.115
_refine_ls_extinction_coef       0.0207(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         3850
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0478
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0687P)²+1.8570P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1162
_refine_ls_wR_factor_ref         0.1263
_reflns_number_gt                2960
_reflns_number_total             3850
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001237z_2.cif
_cod_data_source_block           complex1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0687P)^2^+1.8570P] 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^)+(0.0687P)^2^+1.8570P] 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               4319924
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 0.13498(5) -0.236980(15) 0.74603(3) 0.03308(16) Uani 1 d . . .
O1 O 0.2668(7) -0.14715(15) 0.7121(4) 0.0534(10) Uani 1 d . . .
O2 O 0.1348(6) -0.15953(15) 0.5140(4) 0.0514(10) Uani 1 d . . .
O3 O 0.2788(7) 0.11894(17) 0.3934(4) 0.0606(12) Uani 1 d . . .
O4 O 0.3478(6) 0.13374(16) 0.5932(4) 0.0540(10) Uani 1 d . . .
N1 N 0.4490(5) -0.27857(15) 0.6698(3) 0.0264(7) Uani 1 d . . .
N2 N 0.8220(5) -0.27759(15) 0.6710(3) 0.0256(7) Uani 1 d . . .
N3 N 0.6339(6) -0.36404(15) 0.6258(3) 0.0300(8) Uani 1 d . . .
N4 N 0.6197(5) -0.28836(16) 0.4686(3) 0.0262(7) Uani 1 d . . .
N5 N 0.3024(6) 0.10275(17) 0.5036(5) 0.0407(10) Uani 1 d . . .
C1 C 0.6382(7) -0.25484(18) 0.7295(4) 0.0281(9) Uani 1 d . . .
H1A H 0.6459 -0.2632 0.8189 0.080 Uiso 1 d R . .
H1B H 0.6358 -0.2152 0.7200 0.080 Uiso 1 d R . .
C2 C 0.8196(7) -0.33894(18) 0.6867(4) 0.0302(9) Uani 1 d . . .
H2A H 0.8280 -0.3478 0.7759 0.080 Uiso 1 d R . .
H2B H 0.9359 -0.3547 0.6495 0.080 Uiso 1 d R . .
C3 C 0.4575(7) -0.33993(19) 0.6852(4) 0.0329(10) Uani 1 d . . .
H3A H 0.3354 -0.3561 0.6473 0.080 Uiso 1 d R . .
H3B H 0.4649 -0.3489 0.7744 0.080 Uiso 1 d R . .
C4 C 0.4423(6) -0.26587(19) 0.5309(4) 0.0283(9) Uani 1 d . . .
H4A H 0.4375 -0.2263 0.5193 0.080 Uiso 1 d R . .
H4B H 0.3207 -0.2813 0.4907 0.080 Uiso 1 d R . .
C5 C 0.8067(7) -0.26482(19) 0.5328(4) 0.0282(9) Uani 1 d . . .
H5A H 0.9228 -0.2797 0.4938 0.080 Uiso 1 d R . .
H5B H 0.8071 -0.2253 0.5213 0.080 Uiso 1 d R . .
C6 C 0.6217(7) -0.34975(19) 0.4889(4) 0.0314(9) Uani 1 d . . .
H6A H 0.5010 -0.3656 0.4487 0.080 Uiso 1 d R . .
H6B H 0.7363 -0.3655 0.4498 0.080 Uiso 1 d R . .
C7 C 0.2085(7) -0.1300(2) 0.6025(5) 0.0364(11) Uani 1 d . . .
C8 C 0.2327(6) -0.06836(19) 0.5787(4) 0.0310(9) Uani 1 d . . .
C9 C 0.2679(7) -0.0311(2) 0.6789(5) 0.0356(10) Uani 1 d . . .
H9A H 0.2761 -0.0447 0.7648 0.080 Uiso 1 d R . .
C10 C 0.2909(7) 0.0253(2) 0.6556(5) 0.0362(10) Uani 1 d . . .
H10A H 0.3172 0.0509 0.7245 0.080 Uiso 1 d R . .
C11 C 0.2756(6) 0.04335(19) 0.5304(5) 0.0323(10) Uani 1 d . . .
C12 C 0.2371(7) 0.0077(2) 0.4279(5) 0.0350(10) Uani 1 d . . .
H12A H 0.2251 0.0216 0.3423 0.080 Uiso 1 d R . .
C13 C 0.2153(7) -0.0482(2) 0.4545(4) 0.0326(10) Uani 1 d . . .
H13A H 0.1912 -0.0740 0.3856 0.080 Uiso 1 d R . .
O1W O 0.586(2) -0.0367(6) 1.0254(14) 0.134(6) Uani 0.50 d P . .
H1WA H 0.6797 -0.0203 0.9879 0.120 Uiso 0.50 d PR . .
H1WB H 0.5786 -0.0649 0.9742 0.120 Uiso 0.50 d PR . .
O2W O 0.6029(8) -0.1190(3) 0.8805(6) 0.113(2) Uani 1 d . . .
H2WC H 0.4975 -0.1386 0.8887 0.080 Uiso 1 d R . .
H2WB H 0.6101 -0.1108 0.8022 0.120 Uiso 1 d R . .
O3W O 0.8390(16) 0.0149(3) 0.9082(7) 0.154(4) Uani 1 d . . .
H3WA H 0.8649 0.0471 0.9385 0.120 Uiso 1 d R . .
H3WB H 0.9479 -0.0033 0.9013 0.120 Uiso 1 d R . .
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
O1 Ag1 N2 130.24(14) . 1_455 ?
O1 Ag1 N4 87.26(13) . 4_556 ?
N2 Ag1 N4 109.78(12) 1_455 4_556 ?
O1 Ag1 N1 89.90(14) . . ?
N2 Ag1 N1 117.00(12) 1_455 . ?
N4 Ag1 N1 119.78(11) 4_556 . ?
C7 O1 Ag1 109.9(3) . . ?
C7 O1 O2W 132.6(3) . . ?
Ag1 O1 O2W 113.92(19) . . ?
C1 N1 C3 108.2(3) . . ?
C1 N1 C4 108.2(3) . . ?
C3 N1 C4 108.0(3) . . ?
C1 N1 Ag1 114.1(2) . . ?
C3 N1 Ag1 113.2(3) . . ?
C4 N1 Ag1 104.9(2) . . ?
C5 N2 C2 108.3(3) . . ?
C5 N2 C1 108.4(3) . . ?
C2 N2 C1 107.7(3) . . ?
C5 N2 Ag1 104.3(2) . 1_655 ?
C2 N2 Ag1 112.7(2) . 1_655 ?
C1 N2 Ag1 115.1(2) . 1_655 ?
C3 N3 C6 108.8(3) . . ?
C3 N3 C2 108.2(3) . . ?
C6 N3 C2 108.8(3) . . ?
C4 N4 C5 108.5(3) . . ?
C4 N4 C6 107.5(3) . . ?
C5 N4 C6 108.2(3) . . ?
C4 N4 Ag1 114.5(2) . 4_655 ?
C5 N4 Ag1 105.2(2) . 4_655 ?
C6 N4 Ag1 112.7(2) . 4_655 ?
O3 N5 O4 123.1(5) . . ?
O3 N5 C11 118.8(4) . . ?
O4 N5 C11 118.1(4) . . ?
N1 C1 N2 111.7(3) . . ?
N3 C2 N2 111.8(3) . . ?
N3 C3 N1 111.8(3) . . ?
N4 C4 N1 112.4(3) . . ?
N2 C5 N4 111.9(3) . . ?
N3 C6 N4 111.7(3) . . ?
O2 C7 O1 125.5(5) . . ?
O2 C7 C8 118.4(4) . . ?
O1 C7 C8 116.1(4) . . ?
C13 C8 C9 119.1(4) . . ?
C13 C8 C7 119.5(4) . . ?
C9 C8 C7 121.4(4) . . ?
C10 C9 C8 120.7(4) . . ?
C11 C10 C9 118.2(4) . . ?
C10 C11 C12 122.9(4) . . ?
C10 C11 N5 119.0(4) . . ?
C12 C11 N5 118.1(4) . . ?
C13 C12 C11 117.4(4) . . ?
C12 C13 C8 121.7(4) . . ?
O3W O1W O2W 92.3(6) . . ?
O1W O2W O1 120.5(4) . . ?
O1W O2W O3 127.0(4) . 3_656 ?
O1W O3W O3W 92.0(5) . 3_757 ?
O1W O3W N3 127.4(5) . 2_656 ?
O3W O3W N3 106.3(4) 3_757 2_656 ?
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 O1 2.367(4) . ?
Ag1 N2 2.378(3) 1_455 ?
Ag1 N4 2.426(4) 4_556 ?
Ag1 N1 2.478(4) . ?
O1 C7 1.262(6) . ?
O1 O2W 2.838(8) . ?
O2 C7 1.246(6) . ?
O3 N5 1.224(6) . ?
O4 N5 1.225(6) . ?
N1 C1 1.479(5) . ?
N1 C3 1.487(6) . ?
N1 C4 1.490(5) . ?
N2 C5 1.483(5) . ?
N2 C2 1.487(5) . ?
N2 C1 1.497(5) . ?
N2 Ag1 2.378(3) 1_655 ?
N3 C3 1.473(6) . ?
N3 C6 1.478(5) . ?
N3 C2 1.479(6) . ?
N4 C4 1.478(5) . ?
N4 C5 1.485(5) . ?
N4 C6 1.493(6) . ?
N4 Ag1 2.426(4) 4_655 ?
N5 C11 1.470(6) . ?
C7 C8 1.516(6) . ?
C8 C13 1.391(6) . ?
C8 C9 1.393(7) . ?
C9 C10 1.389(7) . ?
C10 C11 1.384(7) . ?
C11 C12 1.389(7) . ?
C12 C13 1.384(7) . ?
O1W O3W 2.468(18) . ?
O1W O2W 2.506(15) . ?
O2W O3 3.028(8) 3_656 ?
O3W O3W 2.877(17) 3_757 ?
O3W N3 2.943(7) 2_656 ?
