#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:44:31 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179202 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/37/4313764.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_4313764
loop_
_publ_author_name
'Daniel L. Reger'
'Radu F. Semeniuc'
'Ioan Silaghi-Dumitrescu'
'Mark D. Smith'
_publ_contact_author_address
;
Department of Chemistry and Biochemistry
University of South Carolina
Columbia, South Carolina 29208
USA
;
_publ_contact_author_email       reger@mail.chem.sc.edu
_publ_contact_author_fax         '1 803 777 9521'
_publ_contact_author_name        'Professor Daniel L. Reger'
_publ_contact_author_phone       '1 803 777 2587'
_publ_section_title
;
 Influences of Changes in Multitopic Tris(pyrazolyl)methane Ligand
 Topology on Silver(I) Supramolecular Structures
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3751
_journal_page_last               3764
_journal_paper_doi               10.1021/ic034039r
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C62 H66 Ag2 B2 F8 N28 O4'
_chemical_formula_weight         1656.79
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                106.838(3)
_cell_angle_beta                 92.871(3)
_cell_angle_gamma                100.803(3)
_cell_formula_units_Z            1
_cell_length_a                   11.4424(19)
_cell_length_b                   11.972(2)
_cell_length_c                   13.962(2)
_cell_measurement_reflns_used    9324
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.015
_cell_measurement_theta_min      2.248
_cell_volume                     1787.1(5)
_computing_cell_refinement       'SAINT+ NT V6.02a (Bruker, 1998)'
_computing_data_collection       'SMART NT V5.619 (Bruker, 2000)'
_computing_data_reduction        'SAINT+ NT V6.02a'
_computing_molecular_graphics    'SHELXTL V5.1 (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL V5.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       '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  0.0200
_diffrn_reflns_av_sigmaI/netI    0.0363
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12727
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.53
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    0.637
_exptl_absorpt_correction_T_max  0.8943
_exptl_absorpt_correction_T_min  0.7605
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Bruker, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             842
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.843
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         6285
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0374
_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)+(0.0595P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0977
_refine_ls_wR_factor_ref         0.1005
_reflns_number_gt                5029
_reflns_number_total             6285
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034039rsi20030123_104234_1.cif
_cod_data_source_block           cmpd1
_cod_database_code               4313764
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ag Ag 0.60281(2) 0.74256(2) 0.71243(2) 0.05029(11) Uani 1 1 d . . .
C1 C 0.3967(2) 0.5092(2) 0.7421(2) 0.0258(6) Uani 1 1 d . . .
C2 C 0.3030(2) 0.4093(2) 0.7591(2) 0.0281(6) Uani 1 1 d . . .
H2A H 0.2516 0.3653 0.6972 0.034 Uiso 1 1 calc R . .
H2B H 0.3418 0.3543 0.7813 0.034 Uiso 1 1 calc R . .
C3 C 0.1431(2) 0.3772(2) 0.8537(2) 0.0263(6) Uani 1 1 d . . .
H3A H 0.1787 0.3224 0.8791 0.032 Uiso 1 1 calc R . .
H3B H 0.0918 0.3315 0.7921 0.032 Uiso 1 1 calc R . .
C4 C 0.0707(2) 0.4406(2) 0.93056(19) 0.0238(5) Uani 1 1 d . . .
C5 C 0.0695(2) 0.5609(2) 0.94689(19) 0.0254(6) Uani 1 1 d . . .
H5 H 0.1171 0.6026 0.9112 0.030 Uiso 1 1 calc R . .
C6 C 0.0003(2) 0.6209(2) 1.01433(19) 0.0239(5) Uani 1 1 d . . .
C7 C 0.0007(2) 0.7504(2) 1.0257(2) 0.0283(6) Uani 1 1 d . . .
H7A H 0.0553 0.7786 0.9827 0.034 Uiso 1 1 calc R . .
H7B H -0.0788 0.7587 1.0057 0.034 Uiso 1 1 calc R . .
C8 C 0.0179(2) 0.9377(2) 1.1512(2) 0.0276(6) Uani 1 1 d . . .
H8B H -0.0341 0.9516 1.2043 0.033 Uiso 1 1 calc R . .
H8A H -0.0206 0.9487 1.0922 0.033 Uiso 1 1 calc R . .
C9 C 0.8607(2) 0.9733(2) 0.81446(19) 0.0254(6) Uani 1 1 d . . .
C11 C 0.4685(2) 0.3406(2) 0.6198(2) 0.0343(6) Uani 1 1 d . . .
H11 H 0.4167 0.2751 0.6280 0.041 Uiso 1 1 calc R . .
C12 C 0.5592(2) 0.3380(3) 0.5607(2) 0.0387(7) Uani 1 1 d . . .
H12 H 0.5820 0.2708 0.5202 0.046 Uiso 1 1 calc R . .
C13 C 0.6106(2) 0.4567(3) 0.5734(2) 0.0363(7) Uani 1 1 d . . .
H13 H 0.6752 0.4815 0.5412 0.044 Uiso 1 1 calc R . .
C21 C 0.2252(3) 0.5765(3) 0.6691(2) 0.0414(7) Uani 1 1 d . . .
H21 H 0.1660 0.5076 0.6565 0.050 Uiso 1 1 calc R . .
C22 C 0.2145(3) 0.6774(3) 0.6471(3) 0.0569(10) Uani 1 1 d . . .
H22 H 0.1471 0.6917 0.6165 0.068 Uiso 1 1 calc R . .
C23 C 0.3251(3) 0.7550(3) 0.6795(3) 0.0554(10) Uani 1 1 d . . .
H23 H 0.3431 0.8318 0.6740 0.067 Uiso 1 1 calc R . .
C31 C 0.6094(3) 0.5909(3) 0.9504(3) 0.0555(9) Uani 1 1 d . . .
H31 H 0.6755 0.5808 0.9859 0.067 Uiso 1 1 calc R . .
C32 C 0.5422(3) 0.6761(3) 0.9905(3) 0.0555(9) Uani 1 1 d . . .
H32 H 0.5540 0.7311 1.0545 0.067 Uiso 1 1 calc R . .
C33 C 0.4561(3) 0.6606(3) 0.9150(2) 0.0442(8) Uani 1 1 d . . .
H33 H 0.3949 0.7023 0.9177 0.053 Uiso 1 1 calc R . .
C41 C 0.7309(3) 1.0202(3) 1.0390(3) 0.0461(8) Uani 1 1 d . . .
H41 H 0.7285 1.0192 1.1052 0.055 Uiso 1 1 calc R . .
C42 C 0.6487(3) 1.0613(3) 0.9889(3) 0.0508(9) Uani 1 1 d . . .
H42 H 0.5840 1.0924 1.0141 0.061 Uiso 1 1 calc R . .
C43 C 0.6834(2) 1.0464(2) 0.8948(3) 0.0404(7) Uani 1 1 d . . .
H43 H 0.6468 1.0660 0.8427 0.049 Uiso 1 1 calc R . .
C51 C 0.9819(2) 0.8116(2) 0.7789(2) 0.0304(6) Uani 1 1 d . . .
H51 H 1.0559 0.8565 0.7743 0.037 Uiso 1 1 calc R . .
C52 C 0.9544(3) 0.6916(2) 0.7666(2) 0.0338(6) Uani 1 1 d . . .
H52 H 1.0056 0.6384 0.7524 0.041 Uiso 1 1 calc R . .
C53 C 0.8342(3) 0.6661(2) 0.7797(2) 0.0365(7) Uani 1 1 d . . .
H53 H 0.7912 0.5904 0.7754 0.044 Uiso 1 1 calc R . .
C61 C 0.8442(3) 1.0609(2) 0.6706(2) 0.0390(7) Uani 1 1 d . . .
H61 H 0.9149 1.1186 0.6872 0.047 Uiso 1 1 calc R . .
C62 C 0.7618(3) 1.0389(3) 0.5910(2) 0.0481(8) Uani 1 1 d . . .
H62 H 0.7643 1.0778 0.5421 0.058 Uiso 1 1 calc R . .
C63 C 0.6728(3) 0.9463(3) 0.5975(2) 0.0499(9) Uani 1 1 d . . .
H63 H 0.6042 0.9127 0.5521 0.060 Uiso 1 1 calc R . .
N11 N 0.55698(19) 0.5297(2) 0.63630(18) 0.0328(5) Uani 1 1 d . . .
N12 N 0.46802(18) 0.45681(18) 0.66446(16) 0.0265(5) Uani 1 1 d . . .
N21 N 0.4016(2) 0.7061(2) 0.7192(2) 0.0425(6) Uani 1 1 d . . .
N22 N 0.33817(19) 0.59506(19) 0.71299(17) 0.0314(5) Uani 1 1 d . . .
N31 N 0.47559(19) 0.57289(18) 0.83480(17) 0.0296(5) Uani 1 1 d . . .
N32 N 0.5692(2) 0.5263(2) 0.85648(19) 0.0409(6) Uani 1 1 d . . .
N41 N 0.78117(18) 0.99763(18) 0.89199(17) 0.0290(5) Uani 1 1 d . . .
N42 N 0.8133(2) 0.9825(2) 0.98157(18) 0.0391(6) Uani 1 1 d . . .
N51 N 0.7879(2) 0.76313(19) 0.79928(19) 0.0373(6) Uani 1 1 d . . .
N52 N 0.88064(19) 0.85229(17) 0.79884(17) 0.0279(5) Uani 1 1 d . . .
N61 N 0.6980(2) 0.9117(2) 0.67639(19) 0.0437(6) Uani 1 1 d . . .
N62 N 0.80486(19) 0.98361(18) 0.72177(17) 0.0304(5) Uani 1 1 d . . .
O1 O 0.23512(15) 0.46417(14) 0.83396(14) 0.0305(4) Uani 1 1 d . . .
O2 O 0.03738(15) 0.81945(14) 1.12838(13) 0.0269(4) Uani 1 1 d . . .
B1 B 0.2716(5) 0.0714(3) 0.6962(3) 0.0591(12) Uani 1 1 d . . .
F1 F 0.2049(3) 0.1316(2) 0.65328(19) 0.1213(12) Uani 1 1 d . . .
F2 F 0.3599(2) 0.0409(3) 0.6384(2) 0.1218(12) Uani 1 1 d . . .
F3 F 0.3136(4) 0.1408(2) 0.79155(19) 0.1310(14) Uani 1 1 d . . .
F4 F 0.19994(18) -0.03171(16) 0.69956(19) 0.0688(6) Uani 1 1 d . . .
C1S C 0.8768(4) 0.7454(3) 0.5180(3) 0.0594(10) Uani 1 1 d . . .
C2S C 0.9798(4) 0.8300(3) 0.5101(3) 0.0706(11) Uani 1 1 d . . .
H2S1 H 1.0209 0.8723 0.5760 0.106 Uiso 1 1 calc R . .
H2S2 H 0.9548 0.8857 0.4801 0.106 Uiso 1 1 calc R . .
H2S3 H 1.0325 0.7887 0.4689 0.106 Uiso 1 1 calc R . .
N1S N 0.7978(4) 0.6787(4) 0.5241(3) 0.0984(13) Uani 1 1 d . . .
C3S C 0.8421(4) 0.3576(3) 0.7227(3) 0.0569(10) Uani 1 1 d . . .
C4S C 0.7480(5) 0.3317(4) 0.7879(4) 0.0919(15) Uani 1 1 d . . .
H4S1 H 0.6986 0.2540 0.7559 0.138 Uiso 1 1 calc R . .
H4S2 H 0.6996 0.3907 0.7980 0.138 Uiso 1 1 calc R . .
H4S3 H 0.7852 0.3338 0.8517 0.138 Uiso 1 1 calc R . .
N2S N 0.9106(4) 0.3744(3) 0.6715(4) 0.0853(12) 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'
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
_geom_angle_publ_flag
N21 Ag N61 120.33(9) . . ?
N21 Ag N51 144.78(10) . . ?
N61 Ag N51 83.03(8) . . ?
N21 Ag N11 80.60(8) . . ?
N61 Ag N11 138.74(9) . . ?
N51 Ag N11 99.03(7) . . ?
N12 C1 N31 108.8(2) . . ?
N12 C1 N22 110.8(2) . . ?
N31 C1 N22 108.0(2) . . ?
N12 C1 C2 108.98(19) . . ?
N31 C1 C2 110.0(2) . . ?
N22 C1 C2 110.3(2) . . ?
O1 C2 C1 107.06(19) . . ?
O1 C3 C4 108.82(19) . . ?
C5 C4 C6 118.1(2) . 2_567 ?
C5 C4 C3 121.2(2) . . ?
C6 C4 C3 120.6(2) 2_567 . ?
C6 C5 C4 122.7(2) . . ?
C5 C6 C4 119.2(2) . 2_567 ?
C5 C6 C7 119.7(2) . . ?
C4 C6 C7 121.1(2) 2_567 . ?
O2 C7 C6 109.0(2) . . ?
O2 C8 C9 109.07(19) . 2_677 ?
N41 C9 N62 108.7(2) . . ?
N41 C9 N52 108.5(2) . . ?
N62 C9 N52 110.5(2) . . ?
N41 C9 C8 109.8(2) . 2_677 ?
N62 C9 C8 110.6(2) . 2_677 ?
N52 C9 C8 108.7(2) . 2_677 ?
N12 C11 C12 106.8(2) . . ?
C11 C12 C13 105.5(2) . . ?
N11 C13 C12 111.8(3) . . ?
N22 C21 C22 107.0(3) . . ?
C21 C22 C23 105.7(3) . . ?
N21 C23 C22 111.5(3) . . ?
N32 C31 C32 112.8(3) . . ?
C33 C32 C31 104.3(3) . . ?
C32 C33 N31 107.3(3) . . ?
N42 C41 C42 112.3(3) . . ?
C43 C42 C41 105.1(3) . . ?
N41 C43 C42 106.7(3) . . ?
N52 C51 C52 106.7(2) . . ?
C51 C52 C53 105.4(2) . . ?
N51 C53 C52 111.7(2) . . ?
C62 C61 N62 107.4(3) . . ?
C61 C62 C63 105.5(3) . . ?
N61 C63 C62 111.4(3) . . ?
C13 N11 N12 104.7(2) . . ?
C13 N11 Ag 132.71(18) . . ?
N12 N11 Ag 122.20(16) . . ?
C11 N12 N11 111.3(2) . . ?
C11 N12 C1 129.2(2) . . ?
N11 N12 C1 119.2(2) . . ?
C23 N21 N22 104.6(3) . . ?
C23 N21 Ag 125.4(2) . . ?
N22 N21 Ag 121.63(16) . . ?
C21 N22 N21 111.1(2) . . ?
C21 N22 C1 127.9(2) . . ?
N21 N22 C1 120.7(2) . . ?
C33 N31 N32 111.9(2) . . ?
C33 N31 C1 128.4(2) . . ?
N32 N31 C1 118.2(2) . . ?
C31 N32 N31 103.5(3) . . ?
C43 N41 N42 111.9(2) . . ?
C43 N41 C9 130.3(2) . . ?
N42 N41 C9 117.3(2) . . ?
C41 N42 N41 103.9(2) . . ?
C53 N51 N52 104.6(2) . . ?
C53 N51 Ag 116.27(18) . . ?
N52 N51 Ag 120.30(17) . . ?
C51 N52 N51 111.7(2) . . ?
C51 N52 C9 128.6(2) . . ?
N51 N52 C9 119.7(2) . . ?
C63 N61 N62 105.1(2) . . ?
C63 N61 Ag 127.54(19) . . ?
N62 N61 Ag 126.35(17) . . ?
C61 N62 N61 110.6(2) . . ?
C61 N62 C9 128.5(2) . . ?
N61 N62 C9 120.9(2) . . ?
C2 O1 C3 111.07(18) . . ?
C8 O2 C7 113.33(19) . . ?
F3 B1 F2 113.2(4) . . ?
F3 B1 F4 108.9(3) . . ?
F2 B1 F4 107.5(3) . . ?
F3 B1 F1 108.2(3) . . ?
F2 B1 F1 109.9(4) . . ?
F4 B1 F1 109.0(4) . . ?
N1S C1S C2S 179.1(5) . . ?
N2S C3S C4S 177.9(5) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ag N21 2.274(2) . ?
Ag N61 2.315(2) . ?
Ag N51 2.322(2) . ?
Ag N11 2.403(2) . ?
C1 N12 1.456(3) . ?
C1 N31 1.457(3) . ?
C1 N22 1.464(3) . ?
C1 C2 1.532(3) . ?
C2 O1 1.415(3) . ?
C3 O1 1.433(3) . ?
C3 C4 1.506(3) . ?
C4 C5 1.393(3) . ?
C4 C6 1.400(3) 2_567 ?
C5 C6 1.388(3) . ?
C6 C4 1.400(3) 2_567 ?
C6 C7 1.511(3) . ?
C7 O2 1.428(3) . ?
C8 O2 1.421(3) . ?
C8 C9 1.542(3) 2_677 ?
C9 N41 1.449(3) . ?
C9 N62 1.462(3) . ?
C9 N52 1.465(3) . ?
C9 C8 1.542(3) 2_677 ?
C11 N12 1.351(3) . ?
C11 C12 1.357(4) . ?
C12 C13 1.389(4) . ?
C13 N11 1.312(4) . ?
C21 N22 1.353(4) . ?
C21 C22 1.355(4) . ?
C22 C23 1.389(5) . ?
C23 N21 1.323(4) . ?
C31 N32 1.322(4) . ?
C31 C32 1.398(5) . ?
C32 C33 1.352(5) . ?
C33 N31 1.356(4) . ?
C41 N42 1.327(4) . ?
C41 C42 1.386(5) . ?
C42 C43 1.362(5) . ?
C43 N41 1.353(3) . ?
C51 N52 1.350(3) . ?
C51 C52 1.370(4) . ?
C52 C53 1.385(4) . ?
C53 N51 1.329(3) . ?
C61 C62 1.351(4) . ?
C61 N62 1.352(3) . ?
C62 C63 1.386(4) . ?
C63 N61 1.321(4) . ?
N11 N12 1.363(3) . ?
N21 N22 1.366(3) . ?
N31 N32 1.356(3) . ?
N41 N42 1.358(3) . ?
N51 N52 1.358(3) . ?
N61 N62 1.360(3) . ?
B1 F3 1.356(5) . ?
B1 F2 1.361(5) . ?
B1 F4 1.362(4) . ?
B1 F1 1.368(5) . ?
C1S N1S 1.113(5) . ?
C1S C2S 1.434(5) . ?
C3S N2S 1.117(5) . ?
C3S C4S 1.489(7) . ?
