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#$Date: 2015-07-05 10:50:41 +0300 (Sun, 05 Jul 2015) $
#$Revision: 140076 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/32/4513274.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_4513274
loop_
_publ_author_name
'Durá, Gema'
'Carrión, M. Carmen'
'Jalón, Félix A.'
'Manzano, Blanca R.'
'Rodríguez, Ana M.'
'Mereiter, Kurt'
_publ_section_title
;
 Robust 2D Coordination Networks from a Two-Step Assembly Process with
 Predesigned Silver Cyclic Dimers and Hexamethylenetetramine
;
_journal_issue                   7
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              3321
_journal_paper_doi               10.1021/acs.cgd.5b00428
_journal_volume                  15
_journal_year                    2015
_chemical_formula_moiety         'C42 H45 Ag3 N19, 3(B F4)'
_chemical_formula_sum            'C42 H45 Ag3 B3 F12 N19'
_chemical_formula_weight         1400.01
_chemical_name_common            'AgBF4-eggcrate squeezed'
_chemical_name_systematic
;
Silver tetrafluoroborate / 4-[di(pyrazol-1-yl)methyl]pyridine / hexamethylene-
tetramine 3:3:1 coordination polymer, 2-dimensional, with unknown solvent 
squeezed and not contained in chemical formula and quantities derived thereof.

;
_space_group_crystal_system      trigonal
_space_group_IT_number           166
_space_group_name_Hall           '-R 3 2"'
_space_group_name_H-M_alt        'R -3 m :H'
_symmetry_space_group_name_Hall  '-R 3 2"'
_symmetry_space_group_name_H-M   'R -3 m :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   22.584(3)
_cell_length_b                   22.584(3)
_cell_length_c                   21.750(5)
_cell_measurement_reflns_used    1952
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      14.986
_cell_measurement_theta_min      2.283
_cell_volume                     9607(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX'
_computing_data_reduction        'Bruker SAINT, SADABS, XPREP'
_computing_molecular_graphics    'WINGX v2013.3 (Farrugia, 2013)'
_computing_publication_material  'WINGX v2013.3 (Farrugia, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      290(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker X8 APEX2 CCD area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0711
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_laue_measured_fraction_full 0.974
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            21518
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.143
_exptl_absorpt_coefficient_mu    0.987
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.653
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_description       block
_exptl_crystal_F_000             4164
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.374
_refine_diff_density_min         -0.587
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         2048
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0790
_refine_ls_R_factor_gt           0.0485
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0657P)²+12.9539P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1243
_refine_ls_wR_factor_ref         0.1407
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1281
_reflns_number_total             2048
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cg5b00428_si_002.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 4513274--4513276.cif.'
_cod_original_cell_volume        9608(3)
_cod_database_code               4513274
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.750
_shelx_estimated_absorpt_t_max   0.842
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'y+1/3, x+2/3, -z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z'
'x, x-y, z'
'-y, -x, z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'-y+2/3, -x+1/3, z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-x+y+1/3, y+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'
'-y+1/3, -x+2/3, z+2/3'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ag1 Ag 0.18782(3) 0.09391(2) 0.75445(3) 0.0982(3) Uani 1 2 d S T P . .
N1 N 0.2335(2) 0.1860(2) 0.8232(2) 0.0821(12) Uani 1 1 d . . . . .
N2 N 0.2839(2) 0.19463(19) 0.86240(17) 0.0707(10) Uani 1 1 d . . . . .
N3 N 0.4261(3) 0.21303(14) 0.6765(3) 0.0796(16) Uani 1 2 d S T P . .
N4 N 0.0720(2) 0.03602(12) 0.7294(2) 0.0574(12) Uani 1 2 d S T P . .
N5 N 0.0000 0.0000 0.6374(4) 0.060(2) Uani 1 6 d S T P . .
C1 C 0.2932(3) 0.2402(3) 0.9068(3) 0.1020(18) Uani 1 1 d . . . . .
H1 H 0.3250 0.2542 0.9385 0.122 Uiso 1 1 calc R U . . .
C2 C 0.2484(5) 0.2615(4) 0.8969(3) 0.135(3) Uani 1 1 d . . . . .
H2 H 0.2428 0.2930 0.9200 0.162 Uiso 1 1 calc R U . . .
C3 C 0.2119(4) 0.2265(4) 0.8449(3) 0.115(2) Uani 1 1 d . . . . .
H3 H 0.1767 0.2311 0.8275 0.138 Uiso 1 1 calc R U . . .
C4 C 0.3227(3) 0.16134(16) 0.8516(3) 0.0663(17) Uani 1 2 d S T P . .
H4 H 0.3597 0.1798 0.8820 0.080 Uiso 1 2 calc R U P . .
C5 C 0.3571(3) 0.17855(15) 0.7882(3) 0.0606(15) Uani 1 2 d S T P . .
C6 C 0.3750(2) 0.1353(3) 0.7600(2) 0.0784(14) Uani 1 1 d . . . . .
H6 H 0.3645 0.0940 0.7782 0.094 Uiso 1 1 calc R U . . .
C7 C 0.4086(3) 0.1538(3) 0.7045(3) 0.0847(15) Uani 1 1 d . . . . .
H7 H 0.4197 0.1237 0.6855 0.102 Uiso 1 1 calc R U . . .
C8 C 0.0694(3) 0.03470(17) 0.6609(3) 0.0683(17) Uani 1 2 d S T P . .
H8A H 0.0931 0.0813 0.6456 0.082 Uiso 0.5 1 calc R U P . .
H8B H 0.0931 0.0119 0.6456 0.082 Uiso 0.5 1 calc R U P . .
C9 C 0.03535(16) -0.03535(16) 0.7511(3) 0.0640(16) Uani 1 2 d S T P . .
H9A H 0.0359 -0.0359 0.7957 0.077 Uiso 1 2 calc R U P . .
H9B H 0.0588 -0.0588 0.7365 0.077 Uiso 1 2 calc R U P . .
B1 B 0.1285(3) 0.2570(5) 0.6838(5) 0.091(2) Uani 1 2 d DS TU P . .
F1 F 0.16204(14) 0.3241(3) 0.6764(3) 0.155(2) Uani 1 2 d DS TU P A 1
F2 F 0.1133(3) 0.2267(5) 0.6247(4) 0.186(7) Uani 0.654(17) 2 d S TU P A 1
F3 F 0.0703(4) 0.2321(4) 0.7109(5) 0.162(6) Uani 0.654(17) 1 d D U P A 1
F2A F 0.1361(11) 0.272(2) 0.7450(8) 0.227(18) Uani 0.346(17) 2 d DS TU P A 2
F3A F 0.0681(9) 0.2337(12) 0.6701(13) 0.274(17) Uani 0.346(17) 1 d D U P A 2
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'
F F 0.0171 0.0103 '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'
B B 0.0013 0.0007 '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
N4 Ag1 N1 121.36(13) . 23
N4 Ag1 N1 121.36(13) . .
N1 Ag1 N1 83.8(2) 23 .
N4 Ag1 N3 102.42(18) . 25_556
N1 Ag1 N3 114.05(14) 23 25_556
N1 Ag1 N3 114.05(14) . 25_556
C3 N1 N2 104.5(5) . .
C3 N1 Ag1 133.8(5) . .
N2 N1 Ag1 119.7(3) . .
C1 N2 N1 111.0(4) . .
C1 N2 C4 128.0(5) . .
N1 N2 C4 120.8(4) . .
C7 N3 C7 117.1(6) 23 .
C7 N3 Ag1 121.4(3) 23 25_556
C7 N3 Ag1 121.4(3) . 25_556
C9 N4 C9 108.7(6) 2 .
C9 N4 C8 107.6(3) 2 .
C9 N4 C8 107.6(3) . .
C9 N4 Ag1 113.5(3) 2 .
C9 N4 Ag1 113.5(3) . .
C8 N4 Ag1 105.5(3) . .
C8 N5 C8 108.3(4) 3 2
C8 N5 C8 108.3(4) 3 .
C8 N5 C8 108.3(4) 2 .
C2 C1 N2 107.6(6) . .
C1 C2 C3 105.5(6) . .
N1 C3 C2 111.3(6) . .
N2 C4 N2 112.6(5) . 23
N2 C4 C5 112.3(3) . .
N2 C4 C5 112.3(3) 23 .
C6 C5 C6 118.0(6) . 23
C6 C5 C4 120.9(3) . .
C6 C5 C4 120.9(3) 23 .
C7 C6 C5 119.4(5) . .
N3 C7 C6 123.0(5) . .
N5 C8 N4 112.6(5) . .
N4 C9 N4 111.8(5) . 3
F3A B1 F3A 127(3) 22 .
F3 B1 F3 107.1(14) . 22
F3 B1 F1 115.6(7) . .
F3 B1 F1 115.6(7) 22 .
F3A B1 F2A 108.6(17) 22 .
F3A B1 F2A 108.6(17) . .
F3 B1 F2 104.9(8) . .
F3 B1 F2 104.9(8) 22 .
F1 B1 F2 107.8(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ag1 N4 2.329(5) .
Ag1 N1 2.341(4) 23
Ag1 N1 2.341(5) .
Ag1 N3 2.361(6) 25_556
N1 C3 1.322(7) .
N1 N2 1.356(5) .
N2 C1 1.348(6) .
N2 C4 1.430(5) .
N3 C7 1.337(6) 23
N3 C7 1.337(6) .
N3 Ag1 2.361(6) 25_556
N4 C9 1.473(4) 2
N4 C9 1.473(4) .
N4 C8 1.491(7) .
N5 C8 1.450(7) 3
N5 C8 1.450(7) 2
N5 C8 1.450(7) .
C1 C2 1.337(9) .
C2 C3 1.391(10) .
C4 N2 1.430(5) 23
C4 C5 1.534(9) .
C5 C6 1.375(6) .
C5 C6 1.375(6) 23
C6 C7 1.374(7) .
C9 N4 1.474(4) 3
B1 F3A 1.228(16) 22
B1 F3A 1.228(16) .
B1 F3 1.285(9) .
B1 F3 1.285(9) 22
B1 F1 1.322(10) .
B1 F2A 1.36(2) .
B1 F2 1.417(14) .
