#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:18:00 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179446 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/43/4334381.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_4334381
loop_
_publ_author_name
'Juan Gil-Rubio'
'Verónica Cámara'
'Delia Bautista'
'José Vicente'
_publ_section_title
;
 Mono- and Dinuclear Ag(I), Au(I), and Au(III) Metallamacrocycles
 Containing N-Heterocyclic Dicarbene Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4071
_journal_page_last               4083
_journal_paper_doi               10.1021/ic400184p
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C22 H32 Ag2 F12 N8 P2'
_chemical_formula_weight         914.24
_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                109.681(2)
_cell_angle_beta                 92.116(2)
_cell_angle_gamma                98.078(2)
_cell_formula_units_Z            1
_cell_length_a                   6.6920(7)
_cell_length_b                   10.8533(11)
_cell_length_c                   11.2870(12)
_cell_measurement_reflns_used    4403
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.55
_cell_measurement_theta_min      2.26
_cell_volume                     761.10(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.910
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       ω-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  0.0244
_diffrn_reflns_av_sigmaI/netI    0.0326
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8957
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.70
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    1.496
_exptl_absorpt_correction_T_max  0.9156
_exptl_absorpt_correction_T_min  0.7606
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.995
_exptl_crystal_description       block
_exptl_crystal_F_000             452
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.682
_refine_diff_density_min         -1.822
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.268
_refine_ls_hydrogen_treatment    'rigid methyls, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         3567
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.266
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0604
_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)+(0.0299P)²+5.4380P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1302
_refine_ls_wR_factor_ref         0.1313
_reflns_number_gt                3452
_reflns_number_total             3567
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400184p_si_002_1.cif
_cod_data_source_block           vch176s
_cod_database_code               4334381
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
Ag1 Ag 0.19917(7) 0.43303(4) 0.98783(4) 0.02336(14) Uani 1 1 d . . .
N1 N 0.2069(8) 0.6231(6) 1.2691(5) 0.0325(12) Uani 1 1 d . . .
N2 N 0.3118(8) 0.7271(5) 1.1483(5) 0.0324(12) Uani 1 1 d . . .
N3 N 0.2127(7) 0.2753(5) 0.7061(4) 0.0262(10) Uani 1 1 d . . .
N4 N 0.1448(9) 0.1377(5) 0.8010(5) 0.0340(12) Uani 1 1 d . . .
C1 C 0.2369(8) 0.6033(6) 1.1473(5) 0.0261(12) Uani 1 1 d . . .
C2 C 0.2682(10) 0.7586(7) 1.3409(6) 0.0368(16) Uani 1 1 d . . .
H2 H 0.2639 0.7983 1.4296 0.044 Uiso 1 1 calc R . .
C3 C 0.3321(10) 0.8200(7) 1.2642(7) 0.0371(15) Uani 1 1 d . . .
H3 H 0.3827 0.9118 1.2860 0.044 Uiso 1 1 calc R . .
C4 C 0.3569(11) 0.7556(7) 1.0325(8) 0.0411(17) Uani 1 1 d . . .
H4A H 0.2308 0.7614 0.9891 0.062 Uiso 1 1 calc R . .
H4B H 0.4205 0.6844 0.9766 0.062 Uiso 1 1 calc R . .
H4C H 0.4494 0.8401 1.0547 0.062 Uiso 1 1 calc R . .
C5 C 0.1076(12) 0.5241(8) 1.3155(7) 0.0417(16) Uani 1 1 d . . .
H5A H 0.2065 0.5042 1.3712 0.050 Uiso 1 1 calc R . .
H5B H 0.0593 0.4414 1.2433 0.050 Uiso 1 1 calc R . .
C11 C 0.1831(8) 0.2695(6) 0.8217(5) 0.0231(11) Uani 1 1 d . . .
C12 C 0.1908(9) 0.1500(7) 0.6154(6) 0.0329(14) Uani 1 1 d . . .
H12 H 0.2046 0.1293 0.5277 0.039 Uiso 1 1 calc R . .
C13 C 0.1471(10) 0.0652(7) 0.6744(6) 0.0359(15) Uani 1 1 d . . .
H13 H 0.1216 -0.0287 0.6369 0.043 Uiso 1 1 calc R . .
C14 C 0.1097(12) 0.0759(8) 0.8958(7) 0.0447(17) Uani 1 1 d . . .
H14A H 0.1584 0.1406 0.9796 0.067 Uiso 1 1 calc R . .
H14B H 0.1828 0.0004 0.8784 0.067 Uiso 1 1 calc R . .
H14C H -0.0357 0.0449 0.8933 0.067 Uiso 1 1 calc R . .
C15 C 0.2554(11) 0.4000(7) 0.6809(6) 0.0375(16) Uani 1 1 d . . .
H15A H 0.3732 0.3968 0.6300 0.045 Uiso 1 1 calc R . .
H15B H 0.2936 0.4738 0.7623 0.045 Uiso 1 1 calc R . .
C16 C 0.0747(11) 0.4303(7) 0.6099(6) 0.0388(16) Uani 1 1 d . . .
H16A H 0.1289 0.4998 0.5757 0.047 Uiso 1 1 calc R . .
H16B H 0.0223 0.3493 0.5368 0.047 Uiso 1 1 calc R . .
P1 P 0.4563(7) 0.2253(3) 0.2894(2) 0.0226(8) Uani 0.804(17) 1 d PD A 1
F1 F 0.4997(18) 0.1317(9) 0.3737(8) 0.054(2) Uani 0.804(17) 1 d P A 1
F2 F 0.3914(16) 0.3092(6) 0.2075(6) 0.058(2) Uani 0.804(17) 1 d P A 1
F3 F 0.4181(14) 0.0944(5) 0.1657(5) 0.0401(16) Uani 0.804(17) 1 d PD A 1
F4 F 0.6864(10) 0.2521(7) 0.2601(7) 0.058(3) Uani 0.804(17) 1 d PD A 1
F5 F 0.2295(9) 0.1976(7) 0.3197(7) 0.0520(19) Uani 0.804(17) 1 d PD A 1
F6 F 0.4923(15) 0.3551(7) 0.4114(6) 0.045(2) Uani 0.804(17) 1 d PD A 1
P1' P 0.508(3) 0.2102(15) 0.3005(14) 0.031(4) Uiso 0.196(17) 1 d PD A 2
F1' F 0.558(4) 0.148(3) 0.365(3) 0.021(6) Uiso 0.196(17) 1 d P A 2
F2' F 0.511(5) 0.313(3) 0.226(3) 0.053(8) Uiso 0.196(17) 1 d P A 2
F3' F 0.502(5) 0.091(3) 0.172(2) 0.048(9) Uiso 0.196(17) 1 d PD A 2
F4' F 0.745(3) 0.232(3) 0.319(4) 0.067(9) Uiso 0.196(17) 1 d PD A 2
F5' F 0.268(4) 0.189(4) 0.276(4) 0.078(13) Uiso 0.196(17) 1 d PD A 2
F6' F 0.512(8) 0.329(3) 0.430(3) 0.056(13) Uiso 0.196(17) 1 d PD A 2
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 C11 175.0(2) . .
C1 Ag1 Ag1 69.95(16) . 2_567
C11 Ag1 Ag1 112.51(15) . 2_567
C1 N1 C2 109.1(6) . .
C1 N1 C5 124.9(6) . .
C2 N1 C5 125.6(6) . .
C3 N2 C1 113.2(6) . .
C3 N2 C4 124.0(6) . .
C1 N2 C4 122.8(6) . .
C11 N3 C12 111.6(5) . .
C11 N3 C15 123.4(5) . .
C12 N3 C15 125.0(5) . .
C11 N4 C13 110.9(5) . .
C11 N4 C14 126.5(6) . .
C13 N4 C14 122.6(6) . .
N1 C1 N2 103.3(5) . .
N1 C1 Ag1 132.3(5) . .
N2 C1 Ag1 124.4(4) . .
C3 C2 N1 108.1(6) . .
C2 C3 N2 106.3(6) . .
N1 C5 C16 112.2(6) . 2_567
N3 C11 N4 103.6(5) . .
N3 C11 Ag1 125.5(4) . .
N4 C11 Ag1 131.0(4) . .
C13 C12 N3 106.6(6) . .
C12 C13 N4 107.4(6) . .
N3 C15 C16 114.2(5) . .
C5 C16 C15 118.3(6) 2_567 .
F5 P1 F6 89.0(4) . .
F5 P1 F2 90.0(5) . .
F6 P1 F2 89.8(5) . .
F5 P1 F4 179.2(5) . .
F6 P1 F4 91.0(4) . .
F2 P1 F4 90.9(4) . .
F5 P1 F3 90.7(4) . .
F6 P1 F3 179.5(5) . .
F2 P1 F3 89.8(4) . .
F4 P1 F3 89.4(4) . .
F5 P1 F1 84.5(5) . .
F6 P1 F1 91.7(5) . .
F2 P1 F1 174.3(6) . .
F4 P1 F1 94.6(5) . .
F3 P1 F1 88.7(4) . .
F1' P1' F4' 71.7(18) . .
F1' P1' F3' 94(2) . .
F4' P1' F3' 92.3(17) . .
F1' P1' F6' 86(2) . .
F4' P1' F6' 88(2) . .
F3' P1' F6' 179(2) . .
F1' P1' F5' 111(2) . .
F4' P1' F5' 177(2) . .
F3' P1' F5' 86.4(19) . .
F6' P1' F5' 93(2) . .
F1' P1' F2' 163.1(19) . .
F4' P1' F2' 92.0(17) . .
F3' P1' F2' 90.6(17) . .
F6' P1' F2' 89.9(19) . .
F5' P1' F2' 86(2) . .
P1' F1' F4' 64.1(17) . .
P1' F4' F1' 44.3(14) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ag1 C1 2.077(6) .
Ag1 C11 2.090(6) .
Ag1 Ag1 3.1888(9) 2_567
N1 C1 1.345(7) .
N1 C2 1.411(9) .
N1 C5 1.440(9) .
N2 C3 1.343(9) .
N2 C1 1.363(8) .
N2 C4 1.474(9) .
N3 C11 1.347(7) .
N3 C12 1.383(8) .
N3 C15 1.467(8) .
N4 C11 1.355(8) .
N4 C13 1.381(8) .
N4 C14 1.452(9) .
C2 C3 1.309(11) .
C5 C16 1.551(10) 2_567
C12 C13 1.314(10) .
C15 C16 1.559(10) .
C16 C5 1.551(10) 2_567
P1 F5 1.578(6) .
P1 F6 1.585(5) .
P1 F2 1.589(6) .
P1 F4 1.595(6) .
P1 F3 1.603(5) .
P1 F1 1.653(10) .
P1' F1' 1.22(4) .
P1' F4' 1.565(15) .
P1' F3' 1.579(15) .
P1' F6' 1.586(15) .
P1' F5' 1.591(15) .
P1' F2' 1.61(3) .
F1' F4' 1.65(4) .
