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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/4/10/93/4109311.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_4109311
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 H14 Ag F6 N4 O2 Sb'
_chemical_formula_weight         709.99
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 94.398(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8051(11)
_cell_length_b                   14.0155(17)
_cell_length_c                   19.182(2)
_cell_measurement_reflns_used    6313
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.161
_cell_measurement_theta_min      2.320
_cell_volume                     2360.2(5)
_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      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0334
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12058
_diffrn_reflns_theta_full        25.49
_diffrn_reflns_theta_max         25.49
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    2.050
_exptl_absorpt_correction_T_max  0.6846
_exptl_absorpt_correction_T_min  0.4944
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.998
_exptl_crystal_description       block
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.526
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         4374
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0266
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0287P)²+0.8397P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0602
_refine_ls_wR_factor_ref         0.0619
_reflns_number_gt                3986
_reflns_number_total             4374
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0701917si20070110_012738.cif
_cod_data_source_block           2
_cod_database_code               4109311
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Ag1 Ag 0.73187(3) 0.314668(18) 0.307122(13) 0.03253(8) Uani 1 1 d .
N1 N 0.3413(3) 0.4853(2) 0.26660(13) 0.0375(7) Uani 1 1 d .
N2 N -0.0339(3) 0.33198(18) 0.35542(13) 0.0292(6) Uani 1 1 d .
N3 N 0.5482(3) 0.2098(2) 0.31159(13) 0.0306(6) Uani 1 1 d .
N4 N 0.3076(3) -0.06742(19) 0.27381(13) 0.0309(6) Uani 1 1 d .
C1 C 0.2239(3) -0.0180(2) 0.58824(15) 0.0295(7) Uani 1 1 d .
H1 H 0.2346 -0.0032 0.6367 0.035 Uiso 1 1 calc R
C2 C 0.1294(3) -0.0912(2) 0.56395(16) 0.0342(8) Uani 1 1 d .
H2 H 0.0761 -0.1272 0.5962 0.041 Uiso 1 1 calc R
C3 C 0.1105(3) -0.1134(2) 0.49293(15) 0.0334(7) Uani 1 1 d .
H3 H 0.0470 -0.1649 0.4769 0.040 Uiso 1 1 calc R
C4 C 0.1856(3) -0.0592(2) 0.44622(15) 0.0300(7) Uani 1 1 d .
H4 H 0.1709 -0.0729 0.3977 0.036 Uiso 1 1 calc R
C5 C 0.2826(3) 0.0151(2) 0.46866(14) 0.0232(6) Uani 1 1 d .
C6 C 0.3617(3) 0.0778(2) 0.42420(14) 0.0241(6) Uani 1 1 d .
H6 H 0.4043 0.1327 0.4472 0.029 Uiso 1 1 calc R
C7 C 0.3863(3) 0.0723(2) 0.35521(14) 0.0227(6) Uani 1 1 d .
C8 C 0.3405(3) -0.0048(2) 0.30982(14) 0.0241(6) Uani 1 1 d .
C9 C 0.4748(3) 0.1476(2) 0.32777(14) 0.0244(6) Uani 1 1 d .
C10 C 0.3035(3) 0.0338(2) 0.54100(14) 0.0248(6) Uani 1 1 d .
C11 C 0.3851(3) 0.1641(2) 0.61721(14) 0.0237(6) Uani 1 1 d .
H11A H 0.4030 0.1313 0.6628 0.028 Uiso 1 1 calc R
H11B H 0.2795 0.1889 0.6128 0.028 Uiso 1 1 calc R
C12 C 0.4969(3) 0.2432(2) 0.61103(13) 0.0264(7) Uani 1 1 d .
H12A H 0.4966 0.2867 0.6517 0.032 Uiso 1 1 calc R
H12B H 0.6010 0.2175 0.6084 0.032 Uiso 1 1 calc R
C13 C 0.5458(3) 0.3481(2) 0.51512(14) 0.0237(6) Uani 1 1 d .
C14 C 0.6942(3) 0.3664(2) 0.54091(15) 0.0286(7) Uani 1 1 d .
H14 H 0.7325 0.3399 0.5844 0.034 Uiso 1 1 calc R
C15 C 0.7863(3) 0.4231(2) 0.50327(15) 0.0293(7) Uani 1 1 d .
H15 H 0.8885 0.4347 0.5207 0.035 Uiso 1 1 calc R
C16 C 0.7316(3) 0.4636(2) 0.44006(15) 0.0286(7) Uani 1 1 d .
H16 H 0.7959 0.5029 0.4147 0.034 Uiso 1 1 calc R
C17 C 0.5832(3) 0.4464(2) 0.41451(14) 0.0247(6) Uani 1 1 d .
H17 H 0.5457 0.4748 0.3716 0.030 Uiso 1 1 calc R
C18 C 0.4868(3) 0.3878(2) 0.45086(13) 0.0215(6) Uani 1 1 d .
C19 C 0.3301(3) 0.3664(2) 0.42831(14) 0.0223(6) Uani 1 1 d .
H19 H 0.2774 0.3306 0.4609 0.027 Uiso 1 1 calc R
C20 C 0.2456(3) 0.3888(2) 0.36851(13) 0.0211(6) Uani 1 1 d .
C21 C 0.2981(3) 0.4426(2) 0.31157(14) 0.0253(6) Uani 1 1 d .
C22 C 0.0891(3) 0.3574(2) 0.36064(13) 0.0227(6) Uani 1 1 d .
O1 O 0.4102(2) 0.10029(16) 0.56086(10) 0.0300(5) Uani 1 1 d .
O2 O 0.4475(2) 0.29225(17) 0.54761(10) 0.0340(5) Uani 1 1 d .
F1 F -0.1426(2) 0.21688(15) 0.19937(10) 0.0444(5) Uani 1 1 d .
F2 F 0.0545(2) 0.20695(14) 0.10192(8) 0.0394(5) Uani 1 1 d .
F3 F -0.0182(2) 0.05241(14) 0.16633(10) 0.0446(5) Uani 1 1 d .
F4 F 0.0599(2) 0.13371(16) 0.28937(9) 0.0450(5) Uani 1 1 d .
F5 F 0.1334(2) 0.29118(15) 0.22215(10) 0.0489(5) Uani 1 1 d .
F6 F 0.25711(18) 0.12698(15) 0.19208(8) 0.0393(5) Uani 1 1 d .
Sb1 Sb 0.05696(2) 0.171002(14) 0.196016(9) 0.02321(7) Uani 1 1 d .
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'
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'
Sb Sb -0.5866 1.5461 '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
N3 Ag1 N2 136.51(10) . 1_655
N3 Ag1 N4 116.04(9) . 2_655
N2 Ag1 N4 107.17(9) 1_655 2_655
C22 N2 Ag1 157.5(2) . 1_455
C9 N3 Ag1 163.1(2) . .
C8 N4 Ag1 172.0(2) . 2_645
C2 C1 C10 119.3(3) . .
C2 C1 H1 120.4 . .
C10 C1 H1 120.4 . .
C1 C2 C3 121.3(3) . .
C1 C2 H2 119.4 . .
C3 C2 H2 119.4 . .
C4 C3 C2 119.0(3) . .
C4 C3 H3 120.5 . .
C2 C3 H3 120.5 . .
C3 C4 C5 121.5(3) . .
C3 C4 H4 119.2 . .
C5 C4 H4 119.2 . .
C4 C5 C10 118.2(3) . .
C4 C5 C6 125.8(3) . .
C10 C5 C6 115.9(3) . .
C7 C6 C5 131.5(3) . .
C7 C6 H6 114.3 . .
C5 C6 H6 114.3 . .
C6 C7 C8 125.3(3) . .
C6 C7 C9 116.5(3) . .
C8 C7 C9 118.0(2) . .
N4 C8 C7 178.2(3) . .
N3 C9 C7 174.3(3) . .
O1 C10 C1 123.2(3) . .
O1 C10 C5 116.0(2) . .
C1 C10 C5 120.7(3) . .
O1 C11 C12 105.2(2) . .
O1 C11 H11A 110.7 . .
C12 C11 H11A 110.7 . .
O1 C11 H11B 110.7 . .
C12 C11 H11B 110.7 . .
H11A C11 H11B 108.8 . .
O2 C12 C11 105.3(2) . .
O2 C12 H12A 110.7 . .
C11 C12 H12A 110.7 . .
O2 C12 H12B 110.7 . .
C11 C12 H12B 110.7 . .
H12A C12 H12B 108.8 . .
O2 C13 C14 124.2(3) . .
O2 C13 C18 115.1(2) . .
C14 C13 C18 120.8(3) . .
C15 C14 C13 119.8(3) . .
C15 C14 H14 120.1 . .
C13 C14 H14 120.1 . .
C14 C15 C16 121.0(3) . .
C14 C15 H15 119.5 . .
C16 C15 H15 119.5 . .
C17 C16 C15 119.5(3) . .
C17 C16 H16 120.2 . .
C15 C16 H16 120.2 . .
C16 C17 C18 121.2(3) . .
C16 C17 H17 119.4 . .
C18 C17 H17 119.4 . .
C17 C18 C13 117.8(2) . .
C17 C18 C19 124.9(2) . .
C13 C18 C19 117.2(2) . .
C20 C19 C18 130.9(3) . .
C20 C19 H19 114.5 . .
C18 C19 H19 114.5 . .
C19 C20 C21 125.4(3) . .
C19 C20 C22 118.4(3) . .
C21 C20 C22 116.2(2) . .
N1 C21 C20 179.3(3) . .
N2 C22 C20 178.9(3) . .
C10 O1 C11 119.8(2) . .
C13 O2 C12 120.3(2) . .
F3 Sb1 F4 91.26(9) . .
F3 Sb1 F5 177.75(8) . .
F4 Sb1 F5 90.96(9) . .
F3 Sb1 F2 88.16(9) . .
F4 Sb1 F2 179.31(9) . .
F5 Sb1 F2 89.62(9) . .
F3 Sb1 F6 90.41(9) . .
F4 Sb1 F6 90.14(8) . .
F5 Sb1 F6 89.25(9) . .
F2 Sb1 F6 89.49(8) . .
F3 Sb1 F1 90.26(9) . .
F4 Sb1 F1 90.42(8) . .
F5 Sb1 F1 90.05(9) . .
F2 Sb1 F1 89.95(8) . .
F6 Sb1 F1 179.12(9) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ag1 N3 2.192(3) .
Ag1 N2 2.208(3) 1_655
Ag1 N4 2.276(3) 2_655
N1 C21 1.139(4) .
N2 C22 1.137(4) .
N2 Ag1 2.208(3) 1_455
N3 C9 1.142(4) .
N4 C8 1.141(3) .
N4 Ag1 2.276(3) 2_645
C1 C2 1.379(4) .
C1 C10 1.392(4) .
C1 H1 0.9500 .
C2 C3 1.395(4) .
C2 H2 0.9500 .
C3 C4 1.381(4) .
C3 H3 0.9500 .
C4 C5 1.394(4) .
C4 H4 0.9500 .
C5 C10 1.410(4) .
C5 C6 1.440(4) .
C6 C7 1.359(4) .
C6 H6 0.9500 .
C7 C8 1.426(4) .
C7 C9 1.436(4) .
C10 O1 1.357(4) .
C11 O1 1.433(3) .
C11 C12 1.493(4) .
C11 H11A 0.9900 .
C11 H11B 0.9900 .
C12 O2 1.435(3) .
C12 H12A 0.9900 .
C12 H12B 0.9900 .
C13 O2 1.353(4) .
C13 C14 1.386(4) .
C13 C18 1.414(4) .
C14 C15 1.378(4) .
C14 H14 0.9500 .
C15 C16 1.391(4) .
C15 H15 0.9500 .
C16 C17 1.381(4) .
C16 H16 0.9500 .
C17 C18 1.405(4) .
C17 H17 0.9500 .
C18 C19 1.445(4) .
C19 C20 1.355(4) .
C19 H19 0.9500 .
C20 C21 1.433(4) .
C20 C22 1.444(4) .
F1 Sb1 1.8765(17) .
F2 Sb1 1.8725(16) .
F3 Sb1 1.8621(18) .
F4 Sb1 1.8637(17) .
F5 Sb1 1.8682(19) .
F6 Sb1 1.8742(16) .
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
N2 Ag1 N3 C9 13.1(9) 1_655
N4 Ag1 N3 C9 -174.0(8) 2_655
C10 C1 C2 C3 -0.8(5) .
C1 C2 C3 C4 -1.5(5) .
C2 C3 C4 C5 1.8(5) .
C3 C4 C5 C10 0.4(5) .
C3 C4 C5 C6 -177.6(3) .
C4 C5 C6 C7 -13.4(5) .
C10 C5 C6 C7 168.6(3) .
C5 C6 C7 C8 -3.0(5) .
C5 C6 C7 C9 -178.4(3) .
Ag1 N4 C8 C7 -60(10) 2_645
C6 C7 C8 N4 -96(10) .
C9 C7 C8 N4 79(10) .
Ag1 N3 C9 C7 41(4) .
C6 C7 C9 N3 11(3) .
C8 C7 C9 N3 -165(3) .
C2 C1 C10 O1 -173.1(3) .
C2 C1 C10 C5 3.0(5) .
C4 C5 C10 O1 173.6(3) .
C6 C5 C10 O1 -8.2(4) .
C4 C5 C10 C1 -2.8(4) .
C6 C5 C10 C1 175.4(3) .
O1 C11 C12 O2 67.6(3) .
O2 C13 C14 C15 179.0(3) .
C18 C13 C14 C15 -0.7(5) .
C13 C14 C15 C16 1.0(5) .
C14 C15 C16 C17 -0.3(5) .
C15 C16 C17 C18 -0.7(4) .
C16 C17 C18 C13 1.0(4) .
C16 C17 C18 C19 179.6(3) .
O2 C13 C18 C17 -180.0(3) .
C14 C13 C18 C17 -0.3(4) .
O2 C13 C18 C19 1.3(4) .
C14 C13 C18 C19 -179.0(3) .
C17 C18 C19 C20 5.8(5) .
C13 C18 C19 C20 -175.6(3) .
C18 C19 C20 C21 -0.4(5) .
C18 C19 C20 C22 -179.8(3) .
C19 C20 C21 N1 10(29) .
C22 C20 C21 N1 -170(100) .
Ag1 N2 C22 C20 178(100) 1_455
C19 C20 C22 N2 -1(19) .
C21 C20 C22 N2 180(100) .
C1 C10 O1 C11 -40.5(4) .
C5 C10 O1 C11 143.2(3) .
C12 C11 O1 C10 -163.6(2) .
C14 C13 O2 C12 -3.5(4) .
C18 C13 O2 C12 176.2(2) .
C11 C12 O2 C13 -159.7(3) .
