#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:09:40 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179315 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/12/4321265.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_4321265
loop_
_publ_author_name
'H. V. Rasika Dias'
'Ziyun Wang'
_publ_section_title
;
 Adduct Formation or Metathesis Reactions of Silver Complexes Containing
 the Fluorinated Ligands [HB(3,5-(CF3)2Pz)3]- and [CF3SO3]-: Formation of
 Silver Adducts Containing Unsupported Silver-Germanium Bonds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3890
_journal_page_last               3893
_journal_paper_doi               10.1021/ic000414t
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C25 H17 Ag B Cl3 F18 Ge N8'
_chemical_formula_weight         1069.09
_chemical_name_common            '[HB(CF3)2Tp]AgGeCl[(Me)2ATI]'
_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                 114.120(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.148(2)
_cell_length_b                   17.524(2)
_cell_length_c                   16.006(3)
_cell_measurement_reflns_used    26
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      12.49
_cell_measurement_theta_min      4.88
_cell_volume                     3621.9(10)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_method       'ω 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  0.0222
_diffrn_reflns_av_sigmaI/netI    0.0380
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5852
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.81
_diffrn_standards_decay_%        5.48
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.719
_exptl_absorpt_correction_T_max  0.9970
_exptl_absorpt_correction_T_min  0.7758
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.960
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rods
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.886
_refine_diff_density_min         -0.721
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       0.00051(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     520
_refine_ls_number_reflns         4742
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0393
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0248P)²+12.7721P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0837
_refine_ls_wR_factor_ref         0.0905
_reflns_number_gt                3772
_reflns_number_total             4742
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000414t_1.cif
_cod_data_source_block           rd183
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        3622.1(11)
_cod_database_code               4321265
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ag Ag 0.45521(3) 0.05763(3) 0.69642(3) 0.03312(15) Uani 1 1 d . . .
Ge Ge 0.29335(5) 0.05830(4) 0.56157(4) 0.03332(18) Uani 1 1 d . . .
N11 N 0.6526(3) -0.0196(3) 0.8644(3) 0.0271(11) Uani 1 1 d . . .
N12 N 0.5637(3) -0.0420(2) 0.7947(3) 0.0261(11) Uani 1 1 d . . .
N21 N 0.5768(3) 0.0940(2) 0.9144(3) 0.0271(11) Uani 1 1 d . . .
N22 N 0.4849(3) 0.1096(2) 0.8438(3) 0.0285(11) Uani 1 1 d . . .
N31 N 0.6858(3) 0.1152(2) 0.8234(3) 0.0264(10) Uani 1 1 d . . .
N32 N 0.6236(3) 0.1075(2) 0.7329(3) 0.0260(10) Uani 1 1 d . . .
C13 C 0.5726(4) -0.1172(3) 0.7879(4) 0.0264(13) Uani 1 1 d . . .
C14 C 0.6655(5) -0.1444(3) 0.8529(4) 0.0343(14) Uani 1 1 d . . .
H14 H 0.6894 -0.1956 0.8625 0.041 Uiso 1 1 calc R . .
C15 C 0.7144(4) -0.0815(3) 0.8993(4) 0.0311(14) Uani 1 1 d . . .
C16 C 0.4885(5) -0.1616(3) 0.7150(4) 0.0360(15) Uani 1 1 d . . .
C17 C 0.8203(5) -0.0769(3) 0.9749(5) 0.0462(17) Uani 1 1 d . . .
C23 C 0.4213(4) 0.1332(3) 0.8816(4) 0.0299(13) Uani 1 1 d . . .
C24 C 0.4713(5) 0.1333(3) 0.9761(4) 0.0374(15) Uani 1 1 d . . .
H24 H 0.4437 0.1477 1.0188 0.045 Uiso 1 1 calc R . .
C25 C 0.5686(4) 0.1081(3) 0.9946(4) 0.0317(14) Uani 1 1 d . . .
C26 C 0.3140(5) 0.1578(4) 0.8232(4) 0.0393(15) Uani 1 1 d . . .
C27 C 0.6538(5) 0.0979(4) 1.0862(4) 0.0444(17) Uani 1 1 d . . .
C33 C 0.6588(4) 0.1560(3) 0.6889(4) 0.0298(13) Uani 1 1 d . . .
C34 C 0.7436(4) 0.1969(3) 0.7486(4) 0.0335(14) Uani 1 1 d . . .
H34 H 0.7819 0.2352 0.7340 0.040 Uiso 1 1 calc R . .
C35 C 0.7592(4) 0.1693(3) 0.8330(4) 0.0313(14) Uani 1 1 d . . .
C36 C 0.6057(5) 0.1620(4) 0.5875(4) 0.0399(15) Uani 1 1 d . . .
C37 C 0.8406(5) 0.1927(4) 0.9235(4) 0.0391(15) Uani 1 1 d . . .
F16A F 0.3985(3) -0.1257(2) 0.6813(3) 0.0542(10) Uani 1 1 d . . .
F16B F 0.5124(3) -0.1778(2) 0.6448(2) 0.0523(10) Uani 1 1 d . . .
F16C F 0.4734(3) -0.2283(2) 0.7468(2) 0.0536(10) Uani 1 1 d . . .
F17A F 0.8617(3) -0.1464(2) 0.9949(3) 0.0665(12) Uani 1 1 d . . .
F17B F 0.8226(3) -0.0482(2) 1.0527(3) 0.0692(12) Uani 1 1 d . . .
F17C F 0.8841(3) -0.0339(2) 0.9523(3) 0.0654(12) Uani 1 1 d . . .
F26A F 0.3109(3) 0.2129(2) 0.7658(3) 0.0652(12) Uani 1 1 d . . .
F26B F 0.2565(3) 0.1015(2) 0.7716(3) 0.0593(11) Uani 1 1 d . . .
F26C F 0.2665(3) 0.1826(3) 0.8741(3) 0.0788(14) Uani 1 1 d . . .
F27A F 0.6856(4) 0.0267(3) 1.1027(3) 0.0745(13) Uani 1 1 d . . .
F27B F 0.6218(3) 0.1187(3) 1.1502(2) 0.0899(17) Uani 1 1 d . . .
F27C F 0.7369(3) 0.1396(2) 1.1015(2) 0.0592(11) Uani 1 1 d . . .
F36A F 0.6658(4) 0.1971(3) 0.5543(3) 0.0862(16) Uani 1 1 d . . .
F36B F 0.5179(3) 0.2009(2) 0.5596(2) 0.0639(12) Uani 1 1 d . . .
F36C F 0.5811(3) 0.0943(2) 0.5470(2) 0.0568(10) Uani 1 1 d . . .
F37A F 0.8989(3) 0.2477(2) 0.9112(3) 0.0645(12) Uani 1 1 d . . .
F37B F 0.9038(3) 0.1356(2) 0.9674(2) 0.0531(10) Uani 1 1 d . . .
F37C F 0.8011(3) 0.2201(2) 0.9800(2) 0.0568(10) Uani 1 1 d . . .
B B 0.6713(5) 0.0651(4) 0.8976(4) 0.0275(14) Uani 1 1 d . . .
N1 N 0.1927(4) -0.0185(3) 0.5393(3) 0.0349(12) Uani 1 1 d . . .
N9 N 0.2661(4) 0.0408(3) 0.4369(3) 0.0345(12) Uani 1 1 d . . .
C2 C 0.1434(4) -0.0405(3) 0.4525(4) 0.0339(14) Uani 1 1 d . . .
C3 C 0.0592(5) -0.0920(4) 0.4246(4) 0.0427(16) Uani 1 1 d . . .
H3A H 0.0410 -0.1093 0.4723 0.051 Uiso 1 1 calc R . .
C4 C -0.0006(5) -0.1210(4) 0.3392(5) 0.055(2) Uani 1 1 d . . .
H4A H -0.0524 -0.1560 0.3383 0.067 Uiso 1 1 calc R . .
C5 C 0.0013(6) -0.1085(4) 0.2552(5) 0.0571(19) Uani 1 1 d . . .
H5A H -0.0491 -0.1342 0.2042 0.069 Uiso 1 1 calc R . .
C6 C 0.0698(5) -0.0619(4) 0.2386(4) 0.0504(18) Uani 1 1 d . . .
H6A H 0.0605 -0.0600 0.1765 0.060 Uiso 1 1 calc R . .
C7 C 0.1499(5) -0.0175(4) 0.2975(4) 0.0440(16) Uani 1 1 d . . .
H7A H 0.1871 0.0097 0.2693 0.053 Uiso 1 1 calc R . .
C8 C 0.1853(4) -0.0060(3) 0.3918(4) 0.0323(14) Uani 1 1 d . . .
C10 C 0.1656(5) -0.0479(4) 0.6124(4) 0.0473(17) Uani 1 1 d . . .
H10A H 0.2140 -0.0275 0.6714 0.071 Uiso 1 1 calc R . .
H10B H 0.1699 -0.1038 0.6136 0.071 Uiso 1 1 calc R . .
H10C H 0.0949 -0.0323 0.6011 0.071 Uiso 1 1 calc R . .
C11 C 0.3205(5) 0.0824(4) 0.3908(4) 0.0508(19) Uani 1 1 d . . .
H11A H 0.3764 0.1127 0.4357 0.076 Uiso 1 1 calc R . .
H11B H 0.2719 0.1162 0.3443 0.076 Uiso 1 1 calc R . .
H11C H 0.3498 0.0460 0.3613 0.076 Uiso 1 1 calc R . .
Cl1 Cl 0.19320(14) 0.16283(9) 0.54155(11) 0.0526(5) Uani 1 1 d . . .
Cl2 Cl 0.09734(17) 0.18172(13) 0.18552(18) 0.0834(7) Uani 1 1 d . . .
Cl3 Cl -0.0128(3) 0.1520(2) 0.2946(2) 0.1721(19) Uani 1 1 d . . .
C C -0.0142(8) 0.1527(7) 0.1912(6) 0.106(3) Uani 1 1 d . . .
H0A H -0.0709 0.1866 0.1519 0.128 Uiso 1 1 calc R . .
H0B H -0.0304 0.1006 0.1655 0.128 Uiso 1 1 calc R . .
H H 0.741(5) 0.068(3) 0.963(4) 0.050 Uiso 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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 '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
N32 Ag N22 82.17(15) . . ?
N32 Ag Ge 134.88(10) . . ?
N22 Ag Ge 126.60(11) . . ?
N32 Ag N12 78.48(14) . . ?
N22 Ag N12 79.96(14) . . ?
Ge Ag N12 134.23(10) . . ?
N1 Ge N9 82.7(2) . . ?
N1 Ge Cl1 99.80(16) . . ?
N9 Ge Cl1 97.80(15) . . ?
N1 Ge Ag 122.10(14) . . ?
N9 Ge Ag 130.47(15) . . ?
Cl1 Ge Ag 116.14(5) . . ?
N12 N11 C15 109.3(4) . . ?
N12 N11 B 121.8(4) . . ?
C15 N11 B 128.8(4) . . ?
C13 N12 N11 105.5(4) . . ?
C13 N12 Ag 135.5(4) . . ?
N11 N12 Ag 116.9(3) . . ?
N22 N21 C25 109.1(4) . . ?
N22 N21 B 121.4(4) . . ?
C25 N21 B 129.5(5) . . ?
C23 N22 N21 106.2(4) . . ?
C23 N22 Ag 133.0(4) . . ?
N21 N22 Ag 117.7(3) . . ?
N32 N31 C35 108.7(4) . . ?
N32 N31 B 121.8(4) . . ?
C35 N31 B 129.5(5) . . ?
C33 N32 N31 106.4(4) . . ?
C33 N32 Ag 131.5(4) . . ?
N31 N32 Ag 116.5(3) . . ?
N12 C13 C14 111.8(5) . . ?
N12 C13 C16 120.4(5) . . ?
C14 C13 C16 127.8(5) . . ?
C15 C14 C13 104.3(5) . . ?
C14 C15 N11 109.0(5) . . ?
C14 C15 C17 127.4(5) . . ?
N11 C15 C17 123.5(5) . . ?
F16A C16 F16C 107.3(5) . . ?
F16A C16 F16B 107.0(5) . . ?
F16C C16 F16B 105.8(5) . . ?
F16A C16 C13 113.3(5) . . ?
F16C C16 C13 111.1(5) . . ?
F16B C16 C13 111.9(5) . . ?
F17A C17 F17B 106.3(5) . . ?
F17A C17 F17C 107.6(5) . . ?
F17B C17 F17C 106.2(5) . . ?
F17A C17 C15 110.0(5) . . ?
F17B C17 C15 114.2(6) . . ?
F17C C17 C15 112.1(5) . . ?
N22 C23 C24 110.9(5) . . ?
N22 C23 C26 120.6(5) . . ?
C24 C23 C26 128.5(5) . . ?
C25 C24 C23 105.0(5) . . ?
C24 C25 N21 108.9(5) . . ?
C24 C25 C27 126.7(5) . . ?
N21 C25 C27 124.3(5) . . ?
F26A C26 F26C 107.8(5) . . ?
F26A C26 F26B 105.8(5) . . ?
F26C C26 F26B 106.8(5) . . ?
F26A C26 C23 112.7(5) . . ?
F26C C26 C23 110.7(5) . . ?
F26B C26 C23 112.6(5) . . ?
F27A C27 F27C 106.4(6) . . ?
F27A C27 F27B 107.6(6) . . ?
F27C C27 F27B 105.3(5) . . ?
F27A C27 C25 112.7(5) . . ?
F27C C27 C25 114.9(5) . . ?
F27B C27 C25 109.5(6) . . ?
N32 C33 C34 111.8(5) . . ?
N32 C33 C36 119.6(5) . . ?
C34 C33 C36 128.6(5) . . ?
C35 C34 C33 104.1(5) . . ?
C34 C35 N31 109.0(5) . . ?
C34 C35 C37 127.7(5) . . ?
N31 C35 C37 123.3(5) . . ?
F36A C36 F36B 107.0(5) . . ?
F36A C36 F36C 107.7(5) . . ?
F36B C36 F36C 105.9(5) . . ?
F36A C36 C33 110.4(5) . . ?
F36B C36 C33 112.9(5) . . ?
F36C C36 C33 112.6(5) . . ?
F37C C37 F37B 106.8(5) . . ?
F37C C37 F37A 107.2(5) . . ?
F37B C37 F37A 107.4(5) . . ?
F37C C37 C35 112.6(5) . . ?
F37B C37 C35 113.0(5) . . ?
F37A C37 C35 109.5(5) . . ?
N21 B N31 109.9(4) . . ?
N21 B N11 109.3(5) . . ?
N31 B N11 109.5(4) . . ?
C2 N1 C10 122.4(5) . . ?
C2 N1 Ge 115.8(4) . . ?
C10 N1 Ge 121.7(4) . . ?
C8 N9 C11 122.5(5) . . ?
C8 N9 Ge 115.1(4) . . ?
C11 N9 Ge 121.9(4) . . ?
N1 C2 C3 121.9(6) . . ?
N1 C2 C8 113.2(5) . . ?
C3 C2 C8 124.9(5) . . ?
C4 C3 C2 130.3(6) . . ?
C5 C4 C3 131.4(7) . . ?
C4 C5 C6 125.6(6) . . ?
C5 C6 C7 130.6(7) . . ?
C6 C7 C8 130.6(7) . . ?
N9 C8 C7 121.1(6) . . ?
N9 C8 C2 112.3(5) . . ?
C7 C8 C2 126.6(6) . . ?
Cl3 C Cl2 115.3(6) . . ?
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 N32 2.375(4) . ?
Ag N22 2.400(4) . ?
Ag Ge 2.4215(9) . ?
Ag N12 2.431(4) . ?
Ge N1 1.885(5) . ?
Ge N9 1.896(5) . ?
Ge Cl1 2.2573(18) . ?
N11 N12 1.354(6) . ?
N11 C15 1.362(7) . ?
N11 B 1.563(8) . ?
N12 C13 1.331(7) . ?
N21 N22 1.358(6) . ?
N21 C25 1.357(7) . ?
N21 B 1.552(8) . ?
N22 C23 1.339(7) . ?
N31 N32 1.360(6) . ?
N31 C35 1.367(7) . ?
N31 B 1.556(8) . ?
N32 C33 1.325(7) . ?
C13 C14 1.385(8) . ?
C13 C16 1.500(8) . ?
C14 C15 1.351(8) . ?
C15 C17 1.495(9) . ?
C16 F16A 1.321(7) . ?
C16 F16C 1.327(6) . ?
C16 F16B 1.330(6) . ?
C17 F17A 1.332(7) . ?
C17 F17B 1.332(8) . ?
C17 F17C 1.334(8) . ?
C23 C24 1.383(8) . ?
C23 C26 1.484(8) . ?
C24 C25 1.357(8) . ?
C25 C27 1.481(8) . ?
C26 F26A 1.321(7) . ?
C26 F26C 1.324(7) . ?
C26 F26B 1.330(7) . ?
C27 F27A 1.316(8) . ?
C27 F27C 1.319(7) . ?
C27 F27B 1.329(7) . ?
C33 C34 1.389(8) . ?
C33 C36 1.488(8) . ?
C34 C35 1.366(8) . ?
C35 C37 1.493(8) . ?
C36 F36A 1.323(7) . ?
C36 F36B 1.324(7) . ?
C36 F36C 1.328(7) . ?
C37 F37C 1.332(7) . ?
C37 F37B 1.334(7) . ?
C37 F37A 1.333(7) . ?
N1 C2 1.332(7) . ?
N1 C10 1.465(7) . ?
N9 C8 1.351(7) . ?
N9 C11 1.461(7) . ?
C2 C3 1.414(8) . ?
C2 C8 1.460(8) . ?
C3 C4 1.378(9) . ?
C4 C5 1.374(10) . ?
C5 C6 1.373(10) . ?
C6 C7 1.381(9) . ?
C7 C8 1.396(8) . ?
Cl2 C 1.695(10) . ?
Cl3 C 1.647(10) . ?
