#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:20:45 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179447 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/44/4334436.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_4334436
loop_
_publ_author_name
'B. Nisar Ahamed'
'Ranjan Dutta'
'Pradyut Ghosh'
_publ_section_title
;
 Role of Wingtip Substituents on Benzene-Platform-Based Tetrapodal Ligands
 toward the Formation of a Self-Assembled Silver Carbene Cage
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4269
_journal_page_last               4276
_journal_paper_doi               10.1021/ic302184h
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C60 H76 Ag4 F24 N16 P4'
_chemical_formula_weight         2032.73
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           136
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4n 2n'
_symmetry_space_group_name_H-M   'P 42/m n m'
_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            2
_cell_length_a                   18.3487(18)
_cell_length_b                   18.3487(18)
_cell_length_c                   13.0310(14)
_cell_measurement_reflns_used    9805
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.82
_cell_measurement_theta_min      2.22
_cell_volume                     4387.2(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'MERCURY 2.3'
_computing_publication_material  'ORTEP 3V.2'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0070
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2128
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    1.047
_exptl_absorpt_correction_T_max  0.9209
_exptl_absorpt_correction_T_min  0.8179
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             2024
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
The unit cell contains four diethyl ether molecules which have been treated 
as a diffuse contribution to the overall scattering without specific atom 
positions by SQUEEZE/PLATON. 
;
_refine_diff_density_max         0.838
_refine_diff_density_min         -0.508
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     143
_refine_ls_number_reflns         2128
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0334
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0848P)²+5.8484P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1194
_refine_ls_wR_factor_ref         0.1221
_reflns_number_gt                1962
_reflns_number_total             2128
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302184h_si_002_6.cif
_cod_data_source_block           Complex3
_cod_database_code               4334436
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y, x, -z'
'-y, -x, -z'
'-x, -y, -z'
'x, y, -z'
'y-1/2, -x-1/2, -z-1/2'
'-y-1/2, x-1/2, -z-1/2'
'x-1/2, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z-1/2'
'-y, -x, z'
'y, x, 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 0.942929(17) 0.247368(17) 0.0000 0.02446(19) Uani 1 2 d S
P1 P 0.21484(6) 0.21484(6) 0.0000 0.0205(4) Uani 1 4 d S
P2 P 0.66083(9) 0.33917(9) 0.0000 0.0451(5) Uani 1 4 d S
F1 F 0.15306(13) 0.15306(13) 0.0000 0.0280(8) Uani 1 4 d S
F7 F 0.7213(2) 0.2787(2) 0.0000 0.0555(12) Uani 1 4 d S
F4 F 0.21489(11) 0.21489(11) 0.1226(2) 0.0421(7) Uani 1 2 d S
F3 F 0.27674(15) 0.27674(15) 0.0000 0.0381(9) Uani 1 4 d S
F2 F 0.27679(17) 0.15387(17) 0.0000 0.0479(8) Uani 1 2 d S
F8 F 0.6618(2) 0.3382(2) 0.1218(3) 0.0881(15) Uani 1 2 d S
F6 F 0.6002(2) 0.2773(3) 0.0000 0.0797(13) Uani 1 2 d S
F5 F 0.6000(3) 0.4000(3) 0.0000 0.155(4) Uani 1 4 d S
N1 N 0.98170(13) 0.20137(12) 0.22298(19) 0.0206(5) Uani 1 1 d .
N2 N 0.89299(14) 0.27640(15) 0.2246(2) 0.0267(6) Uani 1 1 d .
C1 C 0.94028(15) 0.24321(15) 0.1603(3) 0.0212(7) Uani 1 1 d .
C6 C 1.01971(15) 0.07374(15) 0.1889(2) 0.0201(6) Uani 1 1 d .
C4 C 0.96011(18) 0.20762(18) 0.3239(2) 0.0294(7) Uani 1 1 d .
H4 H 0.9801 0.1836 0.3801 0.035 Uiso 1 1 calc R
C7 C 0.94712(16) 0.05288(16) 0.1889(3) 0.0225(9) Uani 1 2 d S
H7 H 0.9113 0.0887 0.1888 0.027 Uiso 1 2 calc SR
C5 C 1.04030(16) 0.15381(16) 0.1880(3) 0.0241(7) Uani 1 1 d .
H5A H 1.0825 0.1609 0.2318 0.029 Uiso 1 1 calc R
H5B H 1.0540 0.1676 0.1188 0.029 Uiso 1 1 calc R
C2 C 0.83921(19) 0.3313(2) 0.1933(3) 0.0418(9) Uani 1 1 d .
H2A H 0.7925 0.3202 0.2245 0.050 Uiso 1 1 calc R
H2B H 0.8332 0.3297 0.1194 0.050 Uiso 1 1 calc R
C3 C 0.90442(19) 0.25536(18) 0.3249(3) 0.0314(7) Uani 1 1 d .
H3 H 0.8786 0.2711 0.3822 0.038 Uiso 1 1 calc R
C8 C 0.8627(4) 0.4063(3) 0.2247(6) 0.098(2) Uani 1 1 d .
H8A H 0.8743 0.4065 0.2965 0.147 Uiso 1 1 calc R
H8B H 0.8239 0.4402 0.2117 0.147 Uiso 1 1 calc R
H8C H 0.9050 0.4202 0.1859 0.147 Uiso 1 1 calc R
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'
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
C1 Ag1 C1 175.04(15) 10 .
F2 P1 F2 179.1(3) 7 .
F2 P1 F4 90.000(1) 7 .
F2 P1 F4 90.000(1) . .
F2 P1 F4 90.000(1) 7 10
F2 P1 F4 90.000(1) . 10
F4 P1 F4 179.9(3) . 10
F2 P1 F1 90.46(13) 7 .
F2 P1 F1 90.46(13) . .
F4 P1 F1 90.05(12) . .
F4 P1 F1 90.05(12) 10 .
F2 P1 F3 89.54(13) 7 .
F2 P1 F3 89.54(13) . .
F4 P1 F3 89.95(12) . .
F4 P1 F3 89.95(12) 10 .
F1 P1 F3 180.0(2) . .
F5 P2 F7 180.0(3) . .
F5 P2 F8 90.9(2) . .
F7 P2 F8 89.1(2) . .
F5 P2 F8 90.9(2) . 10
F7 P2 F8 89.1(2) . 10
F8 P2 F8 178.1(4) . 10
F5 P2 F6 90.56(19) . 15_665
F7 P2 F6 89.44(19) . 15_665
F8 P2 F6 89.991(4) . 15_665
F8 P2 F6 89.991(4) 10 15_665
F5 P2 F6 90.56(19) . .
F7 P2 F6 89.44(19) . .
F8 P2 F6 89.991(4) . .
F8 P2 F6 89.991(4) 10 .
F6 P2 F6 178.9(4) 15_665 .
C1 N1 C4 111.5(3) . .
C1 N1 C5 124.4(3) . .
C4 N1 C5 124.1(3) . .
C1 N2 C3 111.4(3) . .
C1 N2 C2 124.6(3) . .
C3 N2 C2 123.9(3) . .
N2 C1 N1 104.0(3) . .
N2 C1 Ag1 128.2(2) . .
N1 C1 Ag1 127.6(2) . .
C7 C6 C6 118.97(19) . 16_645
C7 C6 C5 120.5(3) . .
C6 C6 C5 120.58(15) 16_645 .
C3 C4 N1 106.4(3) . .
C6 C7 C6 122.1(4) 15_665 .
N1 C5 C6 113.2(2) . .
N2 C2 C8 111.1(3) . .
C4 C3 N2 106.8(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ag1 C1 2.091(4) 10
Ag1 C1 2.091(4) .
P1 F2 1.595(3) 7
P1 F2 1.595(3) .
P1 F4 1.598(3) .
P1 F4 1.598(3) 10
P1 F1 1.603(4) .
P1 F3 1.606(4) .
P2 F5 1.580(7) .
P2 F7 1.570(5) .
P2 F8 1.587(4) .
P2 F8 1.587(4) 10
P2 F6 1.590(4) 15_665
P2 F6 1.590(4) .
N1 C1 1.354(4) .
N1 C4 1.378(4) .
N1 C5 1.458(4) .
N2 C1 1.351(4) .
N2 C3 1.379(4) .
N2 C2 1.468(4) .
C6 C7 1.386(3) .
C6 C6 1.402(6) 16_645
C6 C5 1.517(4) .
C4 C3 1.346(5) .
C7 C6 1.386(3) 15_665
C2 C8 1.499(7) .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.500 0.000 136 59 ' '
2 0.500 0.000 0.000 136 59 ' '
3 0.500 0.500 0.000 73 29 ' '
4 0.000 0.500 0.500 136 59 ' '
5 0.500 1.000 0.500 136 59 ' '
6 0.000 0.000 0.500 73 29 ' '
