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#$Date: 2016-03-21 17:44:03 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178791 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/45/4104546.cif $
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#
# 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_4104546
loop_
_publ_author_name
'Ming-Liang Ma'
'Xiao-Yan Li'
'Ke Wen'
_publ_section_title
;
 Coordination-Driven Self-Assembly of a Discrete Molecular Cage and an
 Infinite Chain of Coordination Cages Based on ortho-Linked
 Oxacalix[2]benzene[2]pyrazine and Oxacalix[2]arene[2]pyrazine
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8338
_journal_page_last               8339
_journal_paper_doi               10.1021/ja900291w
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C11.75 H7.75 Ag0.25 B0.25 F1.25 N2 O2'
_chemical_formula_weight         262.37
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           59
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2a'
_symmetry_space_group_name_H-M   'P m m n :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.6692(3)
_cell_length_b                   21.3336(5)
_cell_length_c                   7.9208(2)
_cell_measurement_temperature    173(2)
_cell_volume                     2140.83(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0225
_diffrn_reflns_av_sigmaI/netI    0.0096
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            23876
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    0.561
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.875511
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.628
_exptl_crystal_description       block
_exptl_crystal_F_000             1060
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.334
_exptl_crystal_size_min          0.268
_refine_diff_density_max         1.165
_refine_diff_density_min         -1.470
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         2023
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0424
_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)+(0.0541P)²+6.1567P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1120
_refine_ls_wR_factor_ref         0.1160
_reflns_number_gt                1929
_reflns_number_total             2023
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja900291w_si_002.cif
_cod_data_source_block           z
_cod_original_sg_symbol_H-M      'P m m n'
_cod_database_code               4104546
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'x+1/2, -y, -z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'-x-1/2, y, z'
'x, -y-1/2, z'
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 -0.2500 0.2500 0.28951(7) 0.0271(2) Uani 1 4 d S
O1 O 0.0615(2) 0.11952(14) 0.6464(3) 0.0412(7) Uani 1 1 d .
O2 O 0.06167(19) 0.07739(12) 0.0758(3) 0.0332(6) Uani 1 1 d .
N1 N -0.1127(2) 0.17190(15) 0.3210(4) 0.0356(7) Uani 1 1 d .
N2 N 0.0645(2) 0.09794(13) 0.3612(4) 0.0262(6) Uani 1 1 d .
C1 C 0.0193(3) 0.12642(17) 0.4904(4) 0.0306(8) Uani 1 1 d .
C2 C -0.0707(3) 0.16337(19) 0.4732(5) 0.0368(9) Uani 1 1 d .
H2A H -0.1018 0.1824 0.5695 0.044 Uiso 1 1 calc R
C3 C -0.0691(3) 0.14381(17) 0.1885(5) 0.0311(8) Uani 1 1 d .
H3A H -0.0983 0.1491 0.0789 0.037 Uiso 1 1 calc R
C4 C 0.0199(3) 0.10652(16) 0.2123(4) 0.0265(7) Uani 1 1 d .
C5 C 0.2500 -0.0092(3) 0.6896(7) 0.0376(13) Uani 1 2 d S
H5A H 0.2500 -0.0533 0.7065 0.045 Uiso 1 2 calc SR
C6 C 0.1552(3) 0.02249(18) 0.6774(5) 0.0346(8) Uani 1 1 d .
H6A H 0.0901 0.0006 0.6850 0.041 Uiso 1 1 calc R
C7 C 0.1570(3) 0.08624(17) 0.6540(4) 0.0293(8) Uani 1 1 d .
C8 C 0.2500 0.1191(2) 0.6415(6) 0.0300(11) Uani 1 2 d S
H8A H 0.2500 0.1632 0.6247 0.036 Uiso 1 2 calc SR
C9 C 0.2500 -0.0500(2) 0.1525(7) 0.0339(12) Uani 1 2 d S
H9A H 0.2500 -0.0937 0.1755 0.041 Uiso 1 2 calc SR
C10 C 0.1551(3) -0.01848(17) 0.1360(4) 0.0307(8) Uani 1 1 d .
H10A H 0.0899 -0.0400 0.1478 0.037 Uiso 1 1 calc R
C11 C 0.1574(3) 0.04511(16) 0.1018(4) 0.0262(7) Uani 1 1 d .
C12 C 0.2500 0.0780(2) 0.0849(6) 0.0256(10) Uani 1 2 d S
H12A H 0.2500 0.1218 0.0625 0.031 Uiso 1 2 calc SR
F1 F -0.3652(10) 0.2500 -0.1403(13) 0.307(9) Uani 1 2 d SU
F3 F -0.2500 0.2500 -0.3231(7) 0.079(2) Uani 1 4 d SU
F2 F -0.2500 0.1998(2) -0.0683(8) 0.112(2) Uani 1 2 d SU
B1 B -0.2500 0.2500 -0.1584(12) 0.047(3) Uani 1 4 d SU
C30 C 0.2500 0.2500 0.279(2) 0.129(8) Uani 1 4 d SDU
H30A H 0.2500 0.2500 0.3988 0.155 Uiso 1 4 calc SR
C31 C 0.1491(9) 0.2500 0.2438(19) 0.180(9) Uani 1 2 d SDU
H31A H 0.0923 0.2500 0.3220 0.216 Uiso 1 2 calc SR
C32 C 0.1425(9) 0.2500 0.0784(17) 0.122(5) Uani 1 2 d SDU
H32A H 0.0704 0.2500 0.0456 0.146 Uiso 1 2 calc SR
C33 C 0.2009(9) 0.2500 -0.0529(16) 0.100(4) Uani 1 2 d SDU
H33A H 0.1665 0.2500 -0.1595 0.120 Uiso 1 2 calc SR
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'
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'
F F 0.0171 0.0103 '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'
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
N1 Ag1 N1 86.96(15) 8_565 .
N1 Ag1 N1 168.16(16) 8_565 7
N1 Ag1 N1 91.83(15) . 7
N1 Ag1 N1 91.83(15) 8_565 2_455
N1 Ag1 N1 168.16(16) . 2_455
N1 Ag1 N1 86.96(15) 7 2_455
C1 O1 C7 115.8(3) . .
C4 O2 C11 116.3(3) . .
C3 N1 C2 119.2(3) . .
C3 N1 Ag1 121.8(3) . .
C2 N1 Ag1 118.4(2) . .
C1 N2 C4 116.3(3) . .
N2 C1 O1 119.0(3) . .
N2 C1 C2 122.7(3) . .
O1 C1 C2 118.3(3) . .
N1 C2 C1 119.6(3) . .
N1 C2 H2A 120.2 . .
C1 C2 H2A 120.2 . .
N1 C3 C4 119.1(3) . .
N1 C3 H3A 120.4 . .
C4 C3 H3A 120.4 . .
N2 C4 O2 118.9(3) . .
N2 C4 C3 123.1(3) . .
O2 C4 C3 118.0(3) . .
C6 C5 C6 120.7(5) 7_655 .
C6 C5 H5A 119.7 7_655 .
C6 C5 H5A 119.7 . .
C7 C6 C5 118.7(4) . .
C7 C6 H6A 120.6 . .
C5 C6 H6A 120.6 . .
C6 C7 C8 121.9(4) . .
C6 C7 O1 119.6(3) . .
C8 C7 O1 118.5(3) . .
C7 C8 C7 118.0(5) . 7_655
C7 C8 H8A 121.0 . .
C7 C8 H8A 121.0 7_655 .
C10 C9 C10 120.6(5) 7_655 .
C10 C9 H9A 119.7 7_655 .
C10 C9 H9A 119.7 . .
C11 C10 C9 118.5(3) . .
C11 C10 H10A 120.8 . .
C9 C10 H10A 120.8 . .
C12 C11 C10 122.6(3) . .
C12 C11 O2 118.1(3) . .
C10 C11 O2 119.3(3) . .
C11 C12 C11 117.3(4) . 7_655
C11 C12 H12A 121.4 . .
C11 C12 H12A 121.4 7_655 .
F2 B1 F2 112.7(10) 2_455 .
F2 B1 F3 123.6(5) 2_455 .
F2 B1 F3 123.6(5) . .
F2 B1 F1 86.9(3) 2_455 .
F2 B1 F1 86.9(3) . .
F3 B1 F1 95.6(6) . .
F2 B1 F1 86.9(3) 2_455 2_455
F2 B1 F1 86.9(3) . 2_455
F3 B1 F1 95.6(6) . 2_455
F1 B1 F1 168.8(11) . 2_455
C31 C30 C31 155.5(16) . 2
C31 C30 H30A 102.3 . .
C31 C30 H30A 102.3 2 .
C30 C31 C32 105.9(11) . .
C30 C31 H31A 127.0 . .
C32 C31 H31A 127.0 . .
C33 C32 C31 140.9(12) . .
C33 C32 H32A 109.6 . .
C31 C32 H32A 109.6 . .
C33 C33 C32 125.4(8) 2 .
C33 C33 H33A 117.3 2 .
C32 C33 H33A 117.3 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ag1 N1 2.421(3) 8_565
Ag1 N1 2.421(3) .
Ag1 N1 2.421(3) 7
Ag1 N1 2.421(3) 2_455
O1 C1 1.355(4) .
O1 C7 1.403(4) .
O2 C4 1.355(4) .
O2 C11 1.410(4) .
N1 C3 1.329(5) .
N1 C2 1.330(5) .
N2 C1 1.320(4) .
N2 C4 1.321(4) .
C1 C2 1.392(5) .
C2 H2A 0.9500 .
C3 C4 1.393(5) .
C3 H3A 0.9500 .
C5 C6 1.381(5) 7_655
C5 C6 1.381(5) .
C5 H5A 0.9500 .
C6 C7 1.373(5) .
C6 H6A 0.9500 .
C7 C8 1.375(4) .
C8 C7 1.375(4) 7_655
C8 H8A 0.9500 .
C9 C10 1.384(4) 7_655
C9 C10 1.384(4) .
C9 H9A 0.9500 .
C10 C11 1.384(5) .
C10 H10A 0.9500 .
C11 C12 1.374(4) .
C12 C11 1.374(4) 7_655
C12 H12A 0.9500 .
F1 B1 1.466(13) .
F3 B1 1.305(11) .
F2 B1 1.287(7) .
B1 F2 1.287(7) 2_455
B1 F1 1.466(13) 2_455
C30 C31 1.308(10) .
C30 C31 1.308(10) 2
C30 H30A 0.9500 .
C31 C32 1.313(10) .
C31 H31A 0.9500 .
C32 C33 1.277(9) .
C32 H32A 0.9500 .
C33 C33 1.24(2) 2
C33 H33A 0.9500 .
