#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:34:46 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179336 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/33/4323397.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_4323397
loop_
_publ_author_name
'Lucia Carlucci'
'Gianfranco Ciani'
'Davide M. Proserpio'
'Angelo Sironi'
_publ_contact_author             'Gianfranco Ciani'
_publ_contact_author_email       davide@csmtbo.mi.cnr.it
_publ_section_title
;
 A Novel 3D Three-Connected cubic Network Containing [Ag6(hmt)6]6+
 hexagonal Units (hmt = Hexamethylenetetramine)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1736
_journal_page_last               1737
_journal_paper_doi               10.1021/ic970043p
_journal_volume                  36
_journal_year                    1997
_chemical_formula_structural     '[Ag5(C6H12N4)6](PF6)5.3CH2Cl2'
_chemical_formula_sum            'C39 H78 Ag5 Cl6 F30 N24 P5'
_chemical_formula_weight         2360.15
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   16.395(2)
_cell_length_b                   16.395(2)
_cell_length_c                   16.030(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11
_cell_measurement_theta_min      8
_cell_volume                     3731.5(8)
_computing_molecular_graphics    'SCHAKAL-92  (Keller 1992)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       CAD4
_diffrn_measurement_method       omega
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1100
_diffrn_reflns_av_sigmaI/netI    0.1332
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4772
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         3
_diffrn_standards_decay_%        14
_diffrn_standards_interval_time  2h
_exptl_absorpt_coefficient_mu    1.738
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.944
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.101
_exptl_crystal_description       cube
_exptl_crystal_F_000             2324
_exptl_crystal_size_max          0.96
_exptl_crystal_size_mid          0.96
_exptl_crystal_size_min          0.96
_refine_diff_density_max         0.708
_refine_diff_density_min         -0.715
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.137
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         1220
_refine_ls_number_restraints     43
_refine_ls_restrained_S_obs      2.082
_refine_ls_R_factor_obs          0.0549
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0431P)²+19.7218P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.1035
_reflns_number_observed          1220
_reflns_number_total             2265
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic970043p_1.cif
_cod_data_source_block           compound_1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0431P)^2^+19.7218P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0431P)^2^+19.7218P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4323397
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, x, z+1/2'
'y, -x+y, z+1/2'
'-x, -y, -z'
'x, y, -z-1/2'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, -x, -z-1/2'
'-y, x-y, -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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Ag1 Ag 0.6667 0.3333 0.5250(2) 0.0337(7) Uani 1 d S .
Ag2 Ag 0.7615(2) 0.6226(2) 0.2500 0.0403(7) Uani 1 d S .
N1 N 0.7147(10) 0.4915(10) 0.4970(9) 0.027(4) Uani 1 d . .
N2 N 0.7556(11) 0.6080(10) 0.3857(8) 0.028(3) Uani 1 d . .
N3 N 0.6772(11) 0.6171(11) 0.5123(9) 0.031(4) Uani 1 d . .
N4 N 0.8407(11) 0.6540(10) 0.5185(10) 0.032(4) Uani 1 d . .
C5 C 0.7247(13) 0.5085(12) 0.4061(11) 0.028(4) Uani 1 d . .
H5A H 0.6648(13) 0.4678(12) 0.3792(11) 0.034 Uiso 1 calc R .
H5B H 0.7703(13) 0.4927(12) 0.3844(11) 0.034 Uiso 1 calc R .
C6 C 0.6470(13) 0.5195(13) 0.5304(12) 0.032(4) Uani 1 d . .
H6A H 0.5854(13) 0.4796(13) 0.5058(12) 0.039 Uiso 1 calc R .
H6B H 0.6412(13) 0.5098(13) 0.5903(12) 0.039 Uiso 1 calc R .
C7 C 0.8079(13) 0.5547(12) 0.5355(12) 0.033(5) Uani 1 d . .
H7A H 0.8035(13) 0.5447(12) 0.5954(12) 0.039 Uiso 1 calc R .
H7B H 0.8536(13) 0.5389(12) 0.5141(12) 0.039 Uiso 1 calc R .
C8 C 0.6862(14) 0.6326(14) 0.4221(11) 0.033(5) Uani 1 d . .
H8A H 0.7068(14) 0.6981(14) 0.4105(11) 0.039 Uiso 1 calc R .
H8B H 0.6253(14) 0.5943(14) 0.3960(11) 0.039 Uiso 1 calc R .
C9 C 0.8480(13) 0.6681(13) 0.4281(11) 0.032(5) Uani 1 d . .
H9A H 0.8940(13) 0.6530(13) 0.4063(11) 0.038 Uiso 1 calc R .
H9B H 0.8698(13) 0.7338(13) 0.4159(11) 0.038 Uiso 1 calc R .
C10 C 0.7716(15) 0.6769(14) 0.5497(12) 0.040(5) Uani 1 d . .
H10A H 0.7926(15) 0.7425(14) 0.5376(12) 0.048 Uiso 1 calc R .
H10B H 0.7669(15) 0.6690(14) 0.6098(12) 0.048 Uiso 1 calc R .
P1 P 1.0000 0.0000 0.5000 0.051(4) Uani 1 d SD .
F11 F 0.9428(27) -0.0838(18) 0.4472(19) 0.249(16) Uani 1 d D .
P2 P 0.4780(6) 0.4290(6) 0.2500 0.041(2) Uani 1 d SD .
F21 F 0.4795(9) 0.4278(10) 0.3480(7) 0.069(4) Uani 1 d D .
F22 F 0.3964(16) 0.4480(18) 0.2500 0.097(8) Uani 1 d SD .
F23 F 0.4079(17) 0.3216(13) 0.2500 0.096(8) Uani 1 d SD .
F24 F 0.5617(17) 0.4078(21) 0.2500 0.108(10) Uani 1 d SD .
F25 F 0.5529(17) 0.5353(14) 0.2500 0.103(9) Uani 1 d SD .
P3 P 0.6667 0.3333 0.7500 0.071(5) Uani 1 d SD .
F31 F 0.6668(57) 0.2676(31) 0.6933(11) 0.448(40) Uani 1 d D .
C1S C 0.9283(31) -0.1650(36) 0.7500 0.153(25) Uani 1 d SD .
H1S1 H 0.9617(31) -0.1290(36) 0.7989 0.183 Uiso 0.50 calc PR .
H1S2 H 0.9617(31) -0.1291(36) 0.7011 0.183 Uiso 0.50 calc PR .
Cl1 Cl 0.8146(9) -0.1820(9) 0.7500 0.102(4) Uani 1 d SD .
Cl2 Cl 0.9269(12) -0.2731(16) 0.7500 0.158(8) Uani 1 d SD .
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'
Cl Cl 0.1484 0.1585 '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
N1 Ag1 N1 116.4(2) 4_665 . ?
N1 Ag1 N1 116.4(2) 4_665 3_655 ?
N1 Ag1 N1 116.4(2) . 3_655 ?
N2 Ag2 N2 169.1(7) 8_556 . ?
C5 N1 C7 107.4(15) . . ?
C5 N1 C6 108.9(14) . . ?
C7 N1 C6 107.4(14) . . ?
C5 N1 Ag1 110.0(10) . . ?
C7 N1 Ag1 110.6(10) . . ?
C6 N1 Ag1 112.4(11) . . ?
C5 N2 C9 107.5(14) . . ?
C5 N2 C8 108.7(14) . . ?
C9 N2 C8 107.5(13) . . ?
C5 N2 Ag2 108.2(10) . . ?
C9 N2 Ag2 114.0(10) . . ?
C8 N2 Ag2 110.8(11) . . ?
C6 N3 C8 109.8(14) . . ?
C6 N3 C10 108.5(15) . . ?
C8 N3 C10 107.7(16) . . ?
C10 N4 C7 108.9(15) . . ?
C10 N4 C9 108.3(15) . . ?
C7 N4 C9 108.4(15) . . ?
N1 C5 N2 111.7(14) . . ?
N3 C6 N1 111.8(15) . . ?
N4 C7 N1 112.2(14) . . ?
N3 C8 N2 111.3(15) . . ?
N4 C9 N2 111.8(15) . . ?
N4 C10 N3 112.4(14) . . ?
F11 P1 F11 89.4(18) 10_546 3_645 ?
F11 P1 F11 89.4(18) 10_546 . ?
F11 P1 F11 90.6(18) 3_645 . ?
F11 P1 F11 90.6(18) 10_546 7_756 ?
F11 P1 F11 89.4(18) 3_645 7_756 ?
F11 P1 F11 179.998(5) . 7_756 ?
F11 P1 F11 90.6(18) 10_546 9_666 ?
F11 P1 F11 179.996(5) 3_645 9_666 ?
F11 P1 F11 89.4(18) . 9_666 ?
F11 P1 F11 90.6(18) 7_756 9_666 ?
F11 P1 F11 179.997(9) 10_546 4_765 ?
F11 P1 F11 90.6(18) 3_645 4_765 ?
F11 P1 F11 90.6(18) . 4_765 ?
F11 P1 F11 89.4(18) 7_756 4_765 ?
F11 P1 F11 89.4(18) 9_666 4_765 ?
F22 P2 F23 90.2(14) . . ?
F22 P2 F25 93.0(16) . . ?
F23 P2 F25 176.8(16) . . ?
F22 P2 F21 91.3(6) . . ?
F23 P2 F21 89.6(6) . . ?
F25 P2 F21 90.3(6) . . ?
F22 P2 F21 91.3(6) . 8_556 ?
F23 P2 F21 89.6(6) . 8_556 ?
F25 P2 F21 90.3(6) . 8_556 ?
F21 P2 F21 177.2(12) . 8_556 ?
F22 P2 F24 179.2(17) . . ?
F23 P2 F24 89.0(15) . . ?
F25 P2 F24 87.7(15) . . ?
F21 P2 F24 88.7(6) . . ?
F21 P2 F24 88.7(6) 8_556 . ?
F31 P3 F31 80.3(17) . 8_557 ?
F31 P3 F31 82.9(12) . 3_655 ?
F31 P3 F31 135.0(6) 8_557 3_655 ?
F31 P3 F31 135.0(6) . 12_657 ?
F31 P3 F31 82.9(12) 8_557 12_657 ?
F31 P3 F31 80.3(17) 3_655 12_657 ?
F31 P3 F31 135.0(6) . 11_667 ?
F31 P3 F31 82.9(12) 8_557 11_667 ?
F31 P3 F31 135.0(6) 3_655 11_667 ?
F31 P3 F31 82.9(12) 12_657 11_667 ?
F31 P3 F31 82.9(12) . 4_665 ?
F31 P3 F31 135.0(6) 8_557 4_665 ?
F31 P3 F31 82.9(13) 3_655 4_665 ?
F31 P3 F31 135.0(6) 12_657 4_665 ?
F31 P3 F31 80.3(17) 11_667 4_665 ?
Cl1 C1S Cl2 111.4(29) . . ?
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
Ag1 N1 2.345(15) 4_665 ?
Ag1 N1 2.345(15) . ?
Ag1 N1 2.345(15) 3_655 ?
Ag2 N2 2.185(13) 8_556 ?
Ag2 N2 2.185(13) . ?
N1 C5 1.48(2) . ?
N1 C7 1.48(2) . ?
N1 C6 1.50(2) . ?
N2 C5 1.48(2) . ?
N2 C9 1.49(2) . ?
N2 C8 1.50(2) . ?
N3 C6 1.45(2) . ?
N3 C8 1.46(2) . ?
N3 C10 1.48(2) . ?
N4 C10 1.45(2) . ?
N4 C7 1.46(2) . ?
N4 C9 1.46(2) . ?
P1 F11 1.48(2) 10_546 ?
P1 F11 1.48(2) 3_645 ?
P1 F11 1.48(2) . ?
P1 F11 1.48(2) 7_756 ?
P1 F11 1.48(2) 9_666 ?
P1 F11 1.48(2) 4_765 ?
P2 F22 1.52(2) . ?
P2 F23 1.55(2) . ?
P2 F25 1.55(2) . ?
P2 F21 1.572(11) . ?
P2 F21 1.572(11) 8_556 ?
P2 F24 1.57(2) . ?
P3 F31 1.41(2) . ?
P3 F31 1.41(2) 8_557 ?
P3 F31 1.41(2) 3_655 ?
P3 F31 1.41(2) 12_657 ?
P3 F31 1.41(2) 11_667 ?
P3 F31 1.41(2) 4_665 ?
C1S Cl1 1.74(4) . ?
C1S Cl2 1.76(4) . ?
