#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:16:27 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179369 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/66/4326651.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_4326651
loop_
_publ_author_name
'Irene Bassanetti'
'Luciano Marchiò'
_publ_contact_author_address
;
Departimento di Chimica GIAF
Università di Parma
via Usberti 17/a, 43100, Parma, Italy
;
_publ_contact_author_email       marchio@unipr.it
_publ_contact_author_fax         '0039 0521 905557'
_publ_contact_author_name        'Dr. Luciano Marchiò'
_publ_contact_author_phone       '0039 0521 905419'
_publ_section_title
;
 Structural Variability in Ag(I) and Cu(I) Coordination Polymers with
 Thioether-Functionalized Bis(pyrazolyl)methane Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10786
_journal_page_last               10797
_journal_paper_doi               10.1021/ic201338w
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C72 H60 Ag P4 1+, B F4 1-'
_chemical_formula_sum            'C72 H60 Ag B F4 P4'
_chemical_formula_weight         1243.76
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                120.00
_cell_formula_units_Z            6
_cell_length_a                   14.258(2)
_cell_length_b                   14.258(2)
_cell_length_c                   51.556(6)
_cell_measurement_reflns_used    22891
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.99
_cell_measurement_theta_min      1.18
_cell_volume                     9077(2)
_computing_cell_refinement       Saint
_computing_data_collection       Smart
_computing_data_reduction        Saint
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    Sir2004
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Smart APEXII CCD'
_diffrn_measurement_method       'theta & omega scan'
_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  0.0324
_diffrn_reflns_av_sigmaI/netI    0.0195
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       63
_diffrn_reflns_limit_l_min       -59
_diffrn_reflns_number            26894
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         1.18
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    0.494
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.827
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_description       prism
_exptl_crystal_F_000             3840
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.027
_refine_diff_density_min         -0.627
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         3986
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0563
_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)+(0.0680P)²+40.6293P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1412
_refine_ls_wR_factor_ref         0.1496
_reflns_number_gt                3382
_reflns_number_total             3986
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201338w_si_001_20.cif
_cod_data_source_block           cndhex
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4326651
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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 0.6667 0.3333 0.581350(9) 0.04844(18) Uani 1 3 d S . .
P2 P 0.6667 0.3333 0.63248(3) 0.0431(4) Uani 1 3 d S . .
P1 P 0.81008(7) 0.53170(7) 0.564086(18) 0.0430(2) Uani 1 1 d . . .
C13 C 0.8164(3) 0.5489(3) 0.52896(7) 0.0523(9) Uani 1 1 d . . .
C8 C 1.0789(4) 0.5096(4) 0.57795(12) 0.0816(15) Uani 1 1 d . . .
H8 H 1.0983 0.4568 0.5756 0.11(2) Uiso 1 1 calc R . .
C7 C 0.9785(4) 0.4899(4) 0.56980(10) 0.0665(11) Uani 1 1 d . . .
H7 H 0.9309 0.4242 0.5620 0.076(14) Uiso 1 1 calc R . .
C2 C 0.7940(3) 0.3643(3) 0.64779(7) 0.0458(8) Uani 1 1 d . . .
C3 C 0.8014(4) 0.3074(4) 0.66870(9) 0.0689(12) Uani 1 1 d . . .
H3 H 0.7392 0.2481 0.6752 0.071(14) Uiso 1 1 calc R . .
C22 C 0.8382(4) 0.7432(3) 0.56079(9) 0.0624(11) Uani 1 1 d . . .
H22 H 0.8604 0.7451 0.5437 0.077(15) Uiso 1 1 calc R . .
C18 C 0.7666(3) 0.6479(4) 0.60054(9) 0.0591(10) Uani 1 1 d . . .
H18 H 0.7409 0.5853 0.6105 0.069(13) Uiso 1 1 calc R . .
C17 C 0.8035(3) 0.6499(3) 0.57554(7) 0.0466(8) Uani 1 1 d . . .
C14 C 0.7203(4) 0.4985(4) 0.51491(9) 0.0638(11) Uani 1 1 d . . .
H14 H 0.6556 0.4532 0.5234 0.069(14) Uiso 1 1 calc R . .
C19 C 0.7675(4) 0.7373(4) 0.61080(10) 0.0721(12) Uani 1 1 d . . .
H19 H 0.7423 0.7348 0.6276 0.094(18) Uiso 1 1 calc R . .
C4 C 0.9005(5) 0.3380(5) 0.67997(11) 0.0871(16) Uani 1 1 d . . .
H4 H 0.9042 0.3003 0.6943 0.12(2) Uiso 1 1 calc R . .
C5 C 0.9934(4) 0.4234(5) 0.67021(11) 0.0792(14) Uani 1 1 d . . .
H5 H 1.0600 0.4433 0.6778 0.14(3) Uiso 1 1 calc R . .
C1 C 0.8896(3) 0.4511(3) 0.63812(9) 0.0603(10) Uani 1 1 d . . .
H1 H 0.8868 0.4903 0.6240 0.080(15) Uiso 1 1 calc R . .
C15 C 0.7197(5) 0.5145(5) 0.48871(10) 0.0819(15) Uani 1 1 d . . .
H15 H 0.6550 0.4786 0.4795 0.10(2) Uiso 1 1 calc R . .
C21 C 0.8399(4) 0.8341(4) 0.57143(12) 0.0773(14) Uani 1 1 d . . .
H21 H 0.8643 0.8968 0.5616 0.078(15) Uiso 1 1 calc R . .
C20 C 0.8054(4) 0.8303(4) 0.59643(12) 0.0757(14) Uani 1 1 d . . .
H20 H 0.8076 0.8911 0.6037 0.072(14) Uiso 1 1 calc R . .
C10 C 1.1221(3) 0.6846(4) 0.59236(10) 0.0715(13) Uani 1 1 d . . .
H10 H 1.1709 0.7506 0.5999 0.088(17) Uiso 1 1 calc R . .
C16 C 0.8121(6) 0.5818(7) 0.47631(10) 0.106(2) Uani 1 1 d . . .
H16 H 0.8105 0.5944 0.4587 0.12(2) Uiso 1 1 calc R . .
C9 C 1.1500(4) 0.6058(4) 0.58939(11) 0.0755(14) Uani 1 1 d . . .
H9 H 1.2170 0.6179 0.5951 0.101(18) Uiso 1 1 calc R . .
C6 C 0.9481(3) 0.5678(3) 0.57319(7) 0.0453(8) Uani 1 1 d . . .
C12 C 0.9122(4) 0.6150(5) 0.51582(10) 0.0896(18) Uani 1 1 d . . .
H12 H 0.9778 0.6474 0.5247 0.090(17) Uiso 1 1 calc R . .
C11 C 1.0222(3) 0.6662(3) 0.58427(8) 0.0570(10) Uani 1 1 d . . .
H11 H 1.0042 0.7201 0.5863 0.056(11) Uiso 1 1 calc R . .
C24 C 0.9878(4) 0.4791(4) 0.64926(10) 0.0704(12) Uani 1 1 d . . .
H24 H 1.0509 0.5364 0.6425 0.084(16) Uiso 1 1 calc R . .
C23 C 0.9093(6) 0.6324(8) 0.48937(12) 0.129(3) Uani 1 1 d . . .
H23 H 0.9730 0.6782 0.4805 0.14(3) Uiso 1 1 calc R . .
B2 B 0.3333 0.6667 0.6667 0.087(5) Uani 1 6 d SD . .
F3 F 0.2403(7) 0.6290(14) 0.6793(3) 0.189(5) Uani 0.50 1 d PDU . 1
F4 F 0.3333 0.6667 0.6912(3) 0.36(2) Uani 0.50 3 d SPDU . 2
B1 B 0.0000 0.0000 0.5000 0.118(7) Uani 1 6 d SD . .
F2 F 0.0000 0.0000 0.5242(3) 0.232(14) Uani 0.50 3 d SPDU A 3
F1 F 0.010(2) -0.0783(15) 0.5114(3) 0.246(7) Uani 0.50 1 d PDU . 4
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'
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'
B B 0.0013 0.0007 '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
P2 Ag P1 109.39(2) . 3_665
P2 Ag P1 109.39(2) . .
P1 Ag P1 109.56(2) 3_665 .
P2 Ag P1 109.39(2) . 2_655
P1 Ag P1 109.56(2) 3_665 2_655
P1 Ag P1 109.56(2) . 2_655
C2 P2 C2 102.59(14) . 3_665
C2 P2 C2 102.59(14) . 2_655
C2 P2 C2 102.59(14) 3_665 2_655
C2 P2 Ag 115.70(12) . .
C2 P2 Ag 115.70(12) 3_665 .
C2 P2 Ag 115.70(12) 2_655 .
C13 P1 C6 104.09(18) . .
C13 P1 C17 102.58(18) . .
C6 P1 C17 101.60(17) . .
C13 P1 Ag 115.59(14) . .
C6 P1 Ag 110.95(12) . .
C17 P1 Ag 120.03(12) . .
C12 C13 C14 118.5(4) . .
C12 C13 P1 122.8(3) . .
C14 C13 P1 118.6(3) . .
C9 C8 C7 120.7(5) . .
C9 C8 H8 119.7 . .
C7 C8 H8 119.7 . .
C8 C7 C6 120.3(4) . .
C8 C7 H7 119.8 . .
C6 C7 H7 119.8 . .
C3 C2 C1 118.1(4) . .
C3 C2 P2 123.7(3) . .
C1 C2 P2 118.2(3) . .
C4 C3 C2 120.6(5) . .
C4 C3 H3 119.7 . .
C2 C3 H3 119.7 . .
C17 C22 C21 120.4(4) . .
C17 C22 H22 119.8 . .
C21 C22 H22 119.8 . .
C19 C18 C17 120.8(4) . .
C19 C18 H18 119.6 . .
C17 C18 H18 119.6 . .
C18 C17 C22 118.5(4) . .
C18 C17 P1 118.3(3) . .
C22 C17 P1 123.1(3) . .
C15 C14 C13 120.9(5) . .
C15 C14 H14 119.5 . .
C13 C14 H14 119.5 . .
C20 C19 C18 120.3(5) . .
C20 C19 H19 119.8 . .
C18 C19 H19 119.8 . .
C5 C4 C3 120.5(5) . .
C5 C4 H4 119.8 . .
C3 C4 H4 119.8 . .
C24 C5 C4 119.7(5) . .
C24 C5 H5 120.2 . .
C4 C5 H5 120.2 . .
C24 C1 C2 120.6(4) . .
C24 C1 H1 119.7 . .
C2 C1 H1 119.7 . .
C16 C15 C14 120.1(5) . .
C16 C15 H15 119.9 . .
C14 C15 H15 119.9 . .
C20 C21 C22 119.6(5) . .
C20 C21 H21 120.2 . .
C22 C21 H21 120.2 . .
C21 C20 C19 120.4(4) . .
C21 C20 H20 119.8 . .
C19 C20 H20 119.8 . .
C9 C10 C11 120.3(5) . .
C9 C10 H10 119.8 . .
C11 C10 H10 119.8 . .
C15 C16 C23 120.9(5) . .
C15 C16 H16 119.6 . .
C23 C16 H16 119.6 . .
C8 C9 C10 119.7(4) . .
C8 C9 H9 120.2 . .
C10 C9 H9 120.2 . .
C11 C6 C7 118.4(4) . .
C11 C6 P1 123.9(3) . .
C7 C6 P1 117.6(3) . .
C13 C12 C23 119.6(6) . .
C13 C12 H12 120.2 . .
C23 C12 H12 120.2 . .
C10 C11 C6 120.6(4) . .
C10 C11 H11 119.7 . .
C6 C11 H11 119.7 . .
C5 C24 C1 120.6(5) . .
C5 C24 H24 119.7 . .
C1 C24 H24 119.7 . .
C16 C23 C12 119.8(6) . .
C16 C23 H23 120.1 . .
C12 C23 H23 120.1 . .
F4 B2 F4 179.997(6) 13_566 .
F4 B2 F3 60.7(6) 13_566 13_566
F4 B2 F3 119.3(6) . 13_566
F4 B2 F3 60.7(6) 13_566 15_556
F4 B2 F3 119.3(6) . 15_556
F3 B2 F3 98.1(7) 13_566 15_556
F4 B2 F3 119.3(6) 13_566 .
F4 B2 F3 60.7(6) . .
F3 B2 F3 179.995(10) 13_566 .
F3 B2 F3 81.9(7) 15_556 .
F4 B2 F3 119.3(6) 13_566 3_565
F4 B2 F3 60.7(6) . 3_565
F3 B2 F3 81.9(7) 13_566 3_565
F3 B2 F3 180.0(10) 15_556 3_565
F3 B2 F3 98.1(7) . 3_565
F4 B2 F3 60.7(6) 13_566 14_456
F4 B2 F3 119.3(6) . 14_456
F3 B2 F3 98.1(7) 13_566 14_456
F3 B2 F3 98.1(7) 15_556 14_456
F3 B2 F3 81.9(7) . 14_456
F3 B2 F3 81.9(7) 3_565 14_456
F4 B2 F3 119.3(6) 13_566 2_665
F4 B2 F3 60.7(6) . 2_665
F3 B2 F3 81.9(7) 13_566 2_665
F3 B2 F3 81.9(7) 15_556 2_665
F3 B2 F3 98.1(7) . 2_665
F3 B2 F3 98.1(7) 3_565 2_665
F3 B2 F3 180.0(12) 14_456 2_665
B2 F3 F3 49.0(4) . 15_556
B2 F3 F3 49.0(4) . 14_456
F3 F3 F3 70.3(10) 15_556 14_456
F2 B1 F2 180.000(6) 10_556 .
F2 B1 F1 116.1(7) 10_556 2
F2 B1 F1 63.9(7) . 2
F2 B1 F1 116.1(7) 10_556 3
F2 B1 F1 63.9(7) . 3
F1 B1 F1 102.1(9) 2 3
F2 B1 F1 63.9(7) 10_556 11_556
F2 B1 F1 116.1(7) . 11_556
F1 B1 F1 180.0(11) 2 11_556
F1 B1 F1 77.9(9) 3 11_556
F2 B1 F1 116.1(7) 10_556 .
F2 B1 F1 63.9(7) . .
F1 B1 F1 102.1(8) 2 .
F1 B1 F1 102.1(9) 3 .
F1 B1 F1 77.9(9) 11_556 .
F2 B1 F1 63.9(7) 10_556 12_556
F2 B1 F1 116.1(7) . 12_556
F1 B1 F1 77.9(9) 2 12_556
F1 B1 F1 180.0(11) 3 12_556
F1 B1 F1 102.1(9) 11_556 12_556
F1 B1 F1 77.9(9) . 12_556
F2 B1 F1 63.9(7) 10_556 10_556
F2 B1 F1 116.1(7) . 10_556
F1 B1 F1 77.9(9) 2 10_556
F1 B1 F1 77.9(9) 3 10_556
F1 B1 F1 102.1(9) 11_556 10_556
F1 B1 F1 180.0(11) . 10_556
F1 B1 F1 102.1(9) 12_556 10_556
B1 F1 F1 51.0(4) . 11_556
B1 F1 F1 51.0(4) . 12_556
F1 F1 F1 76.4(14) 11_556 12_556
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ag P2 2.6360(16) .
Ag P1 2.6812(9) 3_665
Ag P1 2.6812(10) .
Ag P1 2.6813(10) 2_655
P2 C2 1.820(4) .
P2 C2 1.820(4) 3_665
P2 C2 1.820(4) 2_655
P1 C13 1.824(4) .
P1 C6 1.829(4) .
P1 C17 1.831(4) .
C13 C12 1.387(6) .
C13 C14 1.390(6) .
C8 C9 1.366(8) .
C8 C7 1.379(6) .
C8 H8 0.9300 .
C7 C6 1.391(6) .
C7 H7 0.9300 .
C2 C3 1.384(6) .
C2 C1 1.397(6) .
C3 C4 1.381(7) .
C3 H3 0.9300 .
C22 C17 1.392(5) .
C22 C21 1.396(7) .
C22 H22 0.9300 .
C18 C19 1.374(6) .
C18 C17 1.387(6) .
C18 H18 0.9300 .
C14 C15 1.371(7) .
C14 H14 0.9300 .
C19 C20 1.372(7) .
C19 H19 0.9300 .
C4 C5 1.370(8) .
C4 H4 0.9300 .
C5 C24 1.367(7) .
C5 H5 0.9300 .
C1 C24 1.375(6) .
C1 H1 0.9300 .
C15 C16 1.343(9) .
C15 H15 0.9300 .
C21 C20 1.371(8) .
C21 H21 0.9300 .
C20 H20 0.9300 .
C10 C9 1.376(7) .
C10 C11 1.377(6) .
C10 H10 0.9300 .
C16 C23 1.377(10) .
C16 H16 0.9300 .
C9 H9 0.9300 .
C6 C11 1.388(5) .
C12 C23 1.390(8) .
C12 H12 0.9300 .
C11 H11 0.9300 .
C24 H24 0.9300 .
C23 H23 0.9300 .
B2 F4 1.266(18) 13_566
B2 F4 1.266(18) .
B2 F3 1.326(9) 13_566
B2 F3 1.326(9) 15_556
B2 F3 1.326(9) .
B2 F3 1.326(10) 3_565
B2 F3 1.326(9) 14_456
B2 F3 1.326(9) 2_665
F3 F3 1.74(2) 15_556
F3 F3 1.74(2) 14_456
B1 F2 1.248(14) 10_556
B1 F2 1.248(14) .
B1 F1 1.332(12) 2
B1 F1 1.332(12) 3
B1 F1 1.332(12) 11_556
B1 F1 1.332(12) .
B1 F1 1.332(12) 12_556
B1 F1 1.332(12) 10_556
F1 F1 1.675(19) 11_556
F1 F1 1.675(19) 12_556
