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#$Date: 2016-03-21 19:11:46 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178839 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/93/4109312.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_4109312
loop_
_publ_author_name
'Yu-Bin Dong'
'You-Yun Jiang'
'Jie Li'
'Jian-Ping Ma'
'Feng-Ling Liu'
'Bo Tang'
'Ru-Qi Huang'
'Stuart R. Batten'
_publ_section_title
;
 Temperature-Dependent Synthesis of Metal-Organic Frameworks Based on a
 Flexible Tetradentate Ligand with Bidirectional Coordination Donors
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4520
_journal_page_last               4521
_journal_paper_doi               10.1021/ja0701917
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C22 H18 Ag2 B2 F8 N4 O4'
_chemical_formula_weight         791.76
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 110.326(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.042(4)
_cell_length_b                   12.199(3)
_cell_length_c                   15.050(4)
_cell_measurement_temperature    298(2)
_cell_volume                     2761.8(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.925
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0375
_diffrn_reflns_av_sigmaI/netI    0.0473
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            8138
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    1.509
_exptl_absorpt_correction_T_max  0.7523
_exptl_absorpt_correction_T_min  0.5836
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.904
_exptl_crystal_description       block
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.294
_refine_diff_density_min         -0.968
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         3175
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.1059
_refine_ls_R_factor_gt           0.0701
_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)+(0.0826P)²+11.3297P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1745
_refine_ls_wR_factor_ref         0.1945
_reflns_number_gt                2037
_reflns_number_total             3175
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0701917si20070110_012813.cif
_cod_data_source_block           3
_cod_original_cell_volume        2762.0(12)
_cod_database_code               4109312
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
C3 C 0.2965(4) 0.3326(5) 0.2098(4) 0.0469(14) Uani 1 1 d .
Ag1 Ag 0.0000 0.14240(6) 0.2500 0.0715(3) Uani 1 2 d S
Ag2 Ag 0.5000 0.25349(13) 0.2500 0.1201(5) Uani 1 2 d S
C10 C 0.1191(4) 0.6451(5) 0.0721(4) 0.0490(14) Uani 1 1 d .
C5 C 0.1165(4) 0.5481(4) 0.1216(4) 0.0426(12) Uani 1 1 d .
C4 C 0.1948(4) 0.4809(5) 0.1494(4) 0.0453(13) Uani 1 1 d .
H4 H 0.2427 0.5113 0.1369 0.054 Uiso 1 1 calc R
N2 N 0.3654(4) 0.2982(5) 0.2255(4) 0.0601(14) Uani 1 1 d .
O1 O 0.1978(3) 0.6670(4) 0.0621(4) 0.0639(13) Uani 1 1 d .
B1 B 0.3034(6) 0.5521(8) 0.4222(8) 0.071(2) Uani 1 1 d .
C1 C 0.1507(4) 0.3175(5) 0.2194(5) 0.0497(14) Uani 1 1 d .
C6 C 0.0377(4) 0.5240(5) 0.1378(5) 0.0538(15) Uani 1 1 d .
H6 H 0.0352 0.4614 0.1720 0.065 Uiso 1 1 calc R
C2 C 0.2106(4) 0.3810(4) 0.1906(4) 0.0428(13) Uani 1 1 d .
F1 F 0.3638(5) 0.4813(7) 0.4084(7) 0.156(3) Uani 1 1 d .
C7 C -0.0361(4) 0.5897(6) 0.1048(5) 0.0601(17) Uani 1 1 d .
H7 H -0.0877 0.5718 0.1165 0.072 Uiso 1 1 calc R
C9 C 0.0439(5) 0.7111(5) 0.0379(5) 0.0572(16) Uani 1 1 d .
H9 H 0.0456 0.7744 0.0042 0.069 Uiso 1 1 calc R
N1 N 0.1043(4) 0.2634(5) 0.2434(5) 0.0742(18) Uani 1 1 d .
C8 C -0.0326(5) 0.6832(6) 0.0536(5) 0.0609(17) Uani 1 1 d .
H8 H -0.0827 0.7274 0.0298 0.073 Uiso 1 1 calc R
O2 O -0.0122(5) 0.0073(8) 0.1390(6) 0.137(3) Uani 1 1 d D
H2A H -0.0629 0.0069 0.1002 0.205 Uiso 1 1 calc RD
F2 F 0.2249(4) 0.4985(7) 0.3833(5) 0.132(2) Uani 1 1 d .
C11 C 0.2026(5) 0.7515(5) -0.0014(5) 0.0597(17) Uani 1 1 d .
H11A H 0.1886 0.8223 0.0193 0.072 Uiso 1 1 calc R
H11B H 0.1616 0.7373 -0.0650 0.072 Uiso 1 1 calc R
F4 F 0.3219(5) 0.5529(6) 0.5180(5) 0.140(3) Uani 1 1 d .
F3 F 0.3027(7) 0.6444(6) 0.3856(9) 0.234(6) Uani 1 1 d .
H2B H 0.0322 0.0184 0.1228 0.351 Uiso 1 1 d RD
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'
B B 0.0013 0.0007 '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'
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'
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
N2 C3 C2 177.6(7) . .
N1 Ag1 N1 98.4(3) . 2
N1 Ag1 O2 128.4(3) . 2
N1 Ag1 O2 108.2(3) 2 2
N1 Ag1 O2 108.2(3) . .
N1 Ag1 O2 128.4(3) 2 .
O2 Ag1 O2 88.8(5) 2 .
N2 Ag2 N2 150.4(3) 2_655 .
O1 C10 C9 124.6(6) . .
O1 C10 C5 115.3(5) . .
C9 C10 C5 120.0(6) . .
C6 C5 C10 117.7(5) . .
C6 C5 C4 125.6(5) . .
C10 C5 C4 116.8(5) . .
C2 C4 C5 130.9(5) . .
C2 C4 H4 114.5 . .
C5 C4 H4 114.5 . .
C3 N2 Ag2 172.5(5) . .
C10 O1 C11 119.3(5) . .
F3 B1 F2 112.2(9) . .
F3 B1 F4 115.1(10) . .
F2 B1 F4 106.7(8) . .
F3 B1 F1 113.5(9) . .
F2 B1 F1 103.3(8) . .
F4 B1 F1 105.0(8) . .
N1 C1 C2 177.7(7) . .
C7 C6 C5 122.2(6) . .
C7 C6 H6 118.9 . .
C5 C6 H6 118.9 . .
C4 C2 C1 126.5(5) . .
C4 C2 C3 118.6(5) . .
C1 C2 C3 114.9(5) . .
C6 C7 C8 119.0(6) . .
C6 C7 H7 120.5 . .
C8 C7 H7 120.5 . .
C8 C9 C10 120.4(6) . .
C8 C9 H9 119.8 . .
C10 C9 H9 119.8 . .
C1 N1 Ag1 164.7(7) . .
C9 C8 C7 120.7(6) . .
C9 C8 H8 119.7 . .
C7 C8 H8 119.7 . .
Ag1 O2 H2A 109.5 . .
Ag1 O2 H2B 103.2 . .
H2A O2 H2B 121.7 . .
O1 C11 C11 104.6(7) . 7_565
O1 C11 H11A 110.8 . .
C11 C11 H11A 110.8 7_565 .
O1 C11 H11B 110.8 . .
C11 C11 H11B 110.8 7_565 .
H11A C11 H11B 108.9 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C3 N2 1.128(8) .
C3 C2 1.433(8) .
Ag1 N1 2.259(6) .
Ag1 N1 2.259(6) 2
Ag1 O2 2.306(7) 2
Ag1 O2 2.306(7) .
Ag2 N2 2.131(5) 2_655
Ag2 N2 2.131(5) .
C10 O1 1.348(7) .
C10 C9 1.392(9) .
C10 C5 1.407(8) .
C5 C6 1.399(8) .
C5 C4 1.435(8) .
C4 C2 1.351(8) .
C4 H4 0.9300 .
O1 C11 1.427(7) .
B1 F3 1.251(10) .
B1 F2 1.358(11) .
B1 F4 1.367(12) .
B1 F1 1.367(11) .
C1 N1 1.144(8) .
C1 C2 1.415(8) .
C6 C7 1.371(9) .
C6 H6 0.9300 .
C7 C8 1.389(10) .
C7 H7 0.9300 .
C9 C8 1.372(9) .
C9 H9 0.9300 .
C8 H8 0.9300 .
O2 H2A 0.8200 .
O2 H2B 0.8401 .
C11 C11 1.508(14) 7_565
C11 H11A 0.9700 .
C11 H11B 0.9700 .
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
O2 H2B F1 0.84 1.94 2.730(9) 157.1 4_545
O2 H2A F4 0.82 1.97 2.752(10) 158.5 8_455
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
O1 C10 C5 C6 177.1(6) . .
C9 C10 C5 C6 -2.5(9) . .
O1 C10 C5 C4 -4.2(8) . .
C9 C10 C5 C4 176.1(6) . .
C6 C5 C4 C2 4.0(11) . .
C10 C5 C4 C2 -174.5(6) . .
C2 C3 N2 Ag2 -24(20) . .
N2 Ag2 N2 C3 18(5) 2_655 .
C9 C10 O1 C11 -12.0(9) . .
C5 C10 O1 C11 168.4(5) . .
C10 C5 C6 C7 1.9(10) . .
C4 C5 C6 C7 -176.6(6) . .
C5 C4 C2 C1 -1.7(11) . .
C5 C4 C2 C3 179.5(6) . .
N1 C1 C2 C4 175(100) . .
N1 C1 C2 C3 -6(19) . .
N2 C3 C2 C4 33(16) . .
N2 C3 C2 C1 -145(16) . .
C5 C6 C7 C8 0.0(10) . .
O1 C10 C9 C8 -178.4(6) . .
C5 C10 C9 C8 1.2(9) . .
C2 C1 N1 Ag1 -90(19) . .
N1 Ag1 N1 C1 -105(2) 2 .
O2 Ag1 N1 C1 133(2) 2 .
O2 Ag1 N1 C1 30(2) . .
C10 C9 C8 C7 0.8(10) . .
C6 C7 C8 C9 -1.4(10) . .
C10 O1 C11 C11 -176.9(7) . 7_565
