#------------------------------------------------------------------------------
#$Date: 2016-03-26 14:18:14 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180256 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/42/7114272.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_7114272
loop_
_publ_author_name
'Beauchamp, Derek A.'
'Loeb, Stephen J.'
_publ_section_title
;
 Molecular squares, rectangles and infinite helical chains utilising the
 simple ???corner??? ligand 4-(2-pyridyl)-pyrimidine
;
_journal_issue                   21
_journal_name_full               'Chemical Communications'
_journal_page_first              2484
_journal_paper_doi               10.1039/b206989j
_journal_year                    2002
_chemical_formula_sum            'C36 H28 Ag4 B4 F16 N12'
_chemical_formula_weight         1407.42
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                102.984(3)
_cell_angle_beta                 94.837(3)
_cell_angle_gamma                101.366(3)
_cell_formula_units_Z            1
_cell_length_a                   7.8407(14)
_cell_length_b                   9.2136(16)
_cell_length_c                   17.007(3)
_cell_measurement_reflns_used    'reflections from 120 data frames'
_cell_measurement_temperature    289(2)
_cell_measurement_theta_max      28.3
_cell_measurement_theta_min      1.5
_cell_volume                     1163.0(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL XPREP'
_computing_molecular_graphics    'Bruker SHELXTL XP'
_computing_publication_material  'Bruker SHELXTL XCIF'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       'hemisphere 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  0.0179
_diffrn_reflns_av_sigmaI/netI    0.0145
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4067
_diffrn_reflns_theta_full        20.81
_diffrn_reflns_theta_max         20.81
_diffrn_reflns_theta_min         2.35
_diffrn_standards_decay_%        <1
_diffrn_standards_number         '50 standard frames at start and end'
_exptl_absorpt_coefficient_mu    1.768
_exptl_absorpt_correction_T_max  0.058390
_exptl_absorpt_correction_T_min  0.036253
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.009
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.22
_refine_diff_density_max         3.489
_refine_diff_density_min         -0.645
_refine_diff_density_rms         0.183
_refine_ls_extinction_coef       0.035(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         2402
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0712
_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)+(0.1957P)²+1.7409P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2352
_refine_ls_wR_factor_ref         0.2396
_reflns_number_gt                2291
_reflns_number_total             2402
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b206989j.txt
_cod_data_source_block           '[AgL]4[BF4]4_L=4-(2-pyridyl)-pyrimidine'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        1163.1(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7114272
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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 -0.28972(10) 1.04621(8) 0.24186(5) 0.0717(7) Uani 1 1 d .
Ag2 Ag -0.11275(11) 1.37640(9) 0.62124(4) 0.0762(7) Uani 1 1 d .
N1 N -0.3993(10) 1.2309(10) 0.2001(5) 0.059(2) Uani 1 1 d .
N2 N -0.2856(10) 1.2445(8) 0.3573(4) 0.0552(19) Uani 1 1 d .
N3 N -0.2135(10) 1.3702(9) 0.4992(5) 0.062(2) Uani 1 1 d .
N4 N -0.0780(10) 1.5829(9) 0.7376(5) 0.059(2) Uani 1 1 d .
N5 N 0.0396(9) 1.3245(8) 0.7276(4) 0.0527(19) Uani 1 1 d .
N6 N 0.1742(9) 1.1539(8) 0.7835(4) 0.0551(19) Uani 1 1 d .
C1 C -0.4545(13) 1.2214(14) 0.1212(6) 0.070(3) Uani 1 1 d .
H1A H -0.4480 1.1352 0.0819 0.084 Uiso 1 1 calc R
C2 C -0.5190(14) 1.3334(14) 0.0976(7) 0.075(3) Uani 1 1 d .
H2A H -0.5534 1.3237 0.0426 0.090 Uiso 1 1 calc R
C3 C -0.5338(13) 1.4590(15) 0.1532(7) 0.078(4) Uani 1 1 d .
H3A H -0.5801 1.5352 0.1374 0.093 Uiso 1 1 calc R
C4 C -0.4754(11) 1.4715(11) 0.2383(6) 0.061(2) Uani 1 1 d .
H4A H -0.4828 1.5557 0.2789 0.073 Uiso 1 1 calc R
C5 C -0.4108(11) 1.3571(10) 0.2558(5) 0.053(2) Uani 1 1 d .
C6 C -0.3399(11) 1.3648(10) 0.3422(6) 0.049(2) Uani 1 1 d .
C7 C -0.3287(15) 1.4958(11) 0.4049(6) 0.068(3) Uani 1 1 d .
H7A H -0.3639 1.5813 0.3949 0.081 Uiso 1 1 calc R
C8 C -0.2648(16) 1.4922(11) 0.4801(7) 0.073(3) Uani 1 1 d .
H8A H -0.2550 1.5791 0.5219 0.088 Uiso 1 1 calc R
C9 C -0.2226(12) 1.2511(11) 0.4331(6) 0.060(2) Uani 1 1 d .
H9A H -0.1809 1.1677 0.4422 0.071 Uiso 1 1 calc R
C10 C -0.1253(13) 1.7122(11) 0.7386(6) 0.063(3) Uani 1 1 d .
H10A H -0.1712 1.7283 0.6899 0.076 Uiso 1 1 calc R
C11 C -0.1088(14) 1.8288(10) 0.8115(8) 0.079(4) Uani 1 1 d .
H11A H -0.1419 1.9200 0.8106 0.094 Uiso 1 1 calc R
C12 C -0.0453(13) 1.8040(12) 0.8804(7) 0.068(3) Uani 1 1 d .
H12A H -0.0349 1.8777 0.9290 0.081 Uiso 1 1 calc R
C13 C 0.0068(13) 1.6661(11) 0.8806(7) 0.066(3) Uani 1 1 d .
H13A H 0.0515 1.6470 0.9287 0.079 Uiso 1 1 calc R
C14 C -0.0106(10) 1.5611(9) 0.8076(5) 0.047(2) Uani 1 1 d .
C15 C 0.0509(10) 1.4154(9) 0.8035(5) 0.049(2) Uani 1 1 d .
C16 C 0.1209(12) 1.3773(11) 0.8676(5) 0.062(2) Uani 1 1 d .
H16A H 0.1291 1.4397 0.9197 0.074 Uiso 1 1 calc R
C17 C 0.1820(12) 1.2425(11) 0.8562(6) 0.060(2) Uani 1 1 d .
H17A H 0.2294 1.2152 0.9013 0.072 Uiso 1 1 calc R
C18 C 0.0992(13) 1.1984(11) 0.7215(6) 0.065(3) Uani 1 1 d .
H18A H 0.0883 1.1346 0.6696 0.078 Uiso 1 1 calc R
B1 B 0.2492(16) 1.0979(14) 0.4510(10) 0.080(4) Uani 1 1 d .
B2 B -0.3015(15) 1.1942(12) 0.9059(7) 0.065(3) Uani 1 1 d .
F1 F 0.221(3) 1.1308(15) 0.5328(8) 0.225(7) Uani 1 1 d .
F2 F 0.2328(18) 0.9487(10) 0.4309(8) 0.170(4) Uani 1 1 d .
F3 F 0.1032(13) 1.1334(12) 0.4159(8) 0.160(4) Uani 1 1 d .
F4 F 0.3762(15) 1.1959(15) 0.4414(11) 0.178(6) Uani 1 1 d .
F5 F -0.2827(12) 1.1695(10) 0.8262(4) 0.118(3) Uani 1 1 d .
F6 F -0.4758(8) 1.1487(8) 0.9162(4) 0.097(2) Uani 1 1 d .
F7 F -0.2052(12) 1.1141(9) 0.9424(5) 0.107(2) Uani 1 1 d .
F8 F -0.2415(10) 1.3493(7) 0.9446(4) 0.0882(19) 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'
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'
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
N6 Ag1 N1 150.8(3) 2_576 .
N6 Ag1 N2 135.3(3) 2_576 .
N1 Ag1 N2 71.8(3) . .
N3 Ag2 N5 160.8(3) . .
N3 Ag2 N4 126.8(3) . .
N5 Ag2 N4 70.8(3) . .
C5 N1 C1 117.5(9) . .
C5 N1 Ag1 119.3(6) . .
C1 N1 Ag1 123.2(8) . .
C9 N2 C6 118.4(8) . .
C9 N2 Ag1 126.1(6) . .
C6 N2 Ag1 115.3(6) . .
C8 N3 C9 113.6(8) . .
C8 N3 Ag2 121.6(6) . .
C9 N3 Ag2 124.7(7) . .
C10 N4 C14 118.5(8) . .
C10 N4 Ag2 125.3(7) . .
C14 N4 Ag2 116.2(6) . .
C18 N5 C15 117.1(8) . .
C18 N5 Ag2 123.1(6) . .
C15 N5 Ag2 119.2(5) . .
C17 N6 C18 115.9(8) . .
C17 N6 Ag1 124.3(6) . 2_576
C18 N6 Ag1 119.7(6) . 2_576
N1 C1 C2 122.3(11) . .
C3 C2 C1 120.6(10) . .
C2 C3 C4 118.1(10) . .
C5 C4 C3 117.2(10) . .
C4 C5 N1 124.4(9) . .
C4 C5 C6 120.4(8) . .
N1 C5 C6 115.2(8) . .
N2 C6 C7 120.7(8) . .
N2 C6 C5 118.2(8) . .
C7 C6 C5 121.1(8) . .
C8 C7 C6 117.0(9) . .
C7 C8 N3 124.5(9) . .
N2 C9 N3 125.6(9) . .
N4 C10 C11 122.5(9) . .
C12 C11 C10 118.2(9) . .
C11 C12 C13 120.2(9) . .
C14 C13 C12 117.8(10) . .
N4 C14 C13 122.8(8) . .
N4 C14 C15 117.0(7) . .
C13 C14 C15 120.2(8) . .
C16 C15 N5 120.2(8) . .
C16 C15 C14 124.2(8) . .
N5 C15 C14 115.5(7) . .
C15 C16 C17 119.3(9) . .
N6 C17 C16 121.5(8) . .
N5 C18 N6 125.8(9) . .
F4 B1 F2 126.2(14) . .
F4 B1 F3 104.8(12) . .
F2 B1 F3 109.3(13) . .
F4 B1 F1 109.4(14) . .
F2 B1 F1 104.2(13) . .
F3 B1 F1 100.0(13) . .
F5 B2 F7 109.8(9) . .
F5 B2 F6 111.0(9) . .
F7 B2 F6 108.7(10) . .
F5 B2 F8 110.3(9) . .
F7 B2 F8 108.2(8) . .
F6 B2 F8 108.9(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ag1 N6 2.184(7) 2_576
Ag1 N1 2.270(8) .
Ag1 N2 2.356(7) .
Ag2 N3 2.141(8) .
Ag2 N5 2.276(7) .
Ag2 N4 2.372(8) .
N1 C5 1.349(12) .
N1 C1 1.353(13) .
N2 C9 1.325(12) .
N2 C6 1.331(12) .
N3 C8 1.361(13) .
N3 C9 1.369(12) .
N4 C10 1.312(13) .
N4 C14 1.334(12) .
N5 C18 1.322(12) .
N5 C15 1.356(11) .
N6 C17 1.309(12) .
N6 C18 1.347(13) .
N6 Ag1 2.184(7) 2_576
C1 C2 1.357(17) .
C2 C3 1.352(17) .
C3 C4 1.453(15) .
C4 C5 1.335(13) .
C5 C6 1.508(13) .
C6 C7 1.402(14) .
C7 C8 1.343(16) .
C10 C11 1.424(16) .
C11 C12 1.319(15) .
C12 C13 1.410(15) .
C13 C14 1.369(14) .
C14 C15 1.503(13) .
C15 C16 1.328(13) .
C16 C17 1.396(13) .
B1 F4 1.254(16) .
B1 F2 1.317(16) .
B1 F3 1.376(16) .
B1 F1 1.402(19) .
B2 F5 1.349(14) .
B2 F7 1.359(14) .
B2 F6 1.386(14) .
B2 F8 1.399(13) .
