#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:35:06 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180086 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/32/7053245.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_7053245
loop_
_publ_author_name
'Biffis, Andrea'
'Cipani, Matteo'
'Tubaro, Cristina'
'Basato, Marino'
'Costante, Michele'
'Bressan, Edoardo'
'Venzo, Alfonso'
'Graiff, Claudia'
_publ_section_title
;
 Dinuclear complexes of silver(i) and gold(i) with macrocyclic dicarbene
 ligands bearing a 2,6-lutidinyl bridge: synthesis, structural analysis
 and dynamic behaviour in solution
;
_journal_issue                   12
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              4176
_journal_paper_doi               10.1039/c3nj01000g
_journal_volume                  37
_journal_year                    2013
_chemical_formula_sum            'C50 H50 Au2 F12 N14 P2'
_chemical_formula_weight         1530.91
_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                72.9578(8)
_cell_angle_beta                 79.9609(9)
_cell_angle_gamma                69.2499(8)
_cell_formula_units_Z            1
_cell_length_a                   10.8843(6)
_cell_length_b                   11.3235(7)
_cell_length_c                   12.6353(7)
_cell_measurement_reflns_used    999
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      2
_cell_volume                     1387.99(14)
_computing_cell_refinement       'APEX II (Bruker, 2008)'
_computing_data_collection       'APEX II (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'APEX II BRUKER'
_diffrn_measurement_method       '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  0.0337
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21572
_diffrn_reflns_theta_full        30.59
_diffrn_reflns_theta_max         30.59
_diffrn_reflns_theta_min         1.69
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.426
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4348
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.832
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.469
_refine_diff_density_min         -1.181
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         8443
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0310
_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)+(0.0464P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0782
_refine_ls_wR_factor_ref         0.0810
_reflns_number_gt                7464
_reflns_number_total             8443
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3nj01000g.txt
_cod_data_source_block           Au_compound
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7053245
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
C1 C 0.0717(3) 0.6822(3) 0.5299(3) 0.0289(6) Uani 1 1 d .
C2 C 0.0922(4) 0.8550(4) 0.3945(3) 0.0384(8) Uani 1 1 d .
H2 H 0.0711 0.9321 0.3373 0.046 Uiso 1 1 calc R
C3 C 0.2106(4) 0.7883(4) 0.4353(3) 0.0358(7) Uani 1 1 d .
H3 H 0.2889 0.8090 0.4106 0.043 Uiso 1 1 calc R
C4 C 0.3018(3) 0.5761(3) 0.5751(3) 0.0336(7) Uani 1 1 d .
H4A H 0.2725 0.5463 0.6532 0.040 Uiso 1 1 calc R
H4B H 0.3774 0.6049 0.5726 0.040 Uiso 1 1 calc R
C5 C 0.3431(3) 0.4647(3) 0.5203(3) 0.0303(6) Uani 1 1 d .
C6 C 0.4036(4) 0.3343(4) 0.5791(3) 0.0381(8) Uani 1 1 d .
H6 H 0.4201 0.3136 0.6540 0.046 Uiso 1 1 calc R
C7 C 0.4375(4) 0.2390(4) 0.5224(4) 0.0439(9) Uani 1 1 d .
H7 H 0.4796 0.1515 0.5581 0.053 Uiso 1 1 calc R
C8 C 0.4097(4) 0.2718(3) 0.4135(3) 0.0383(8) Uani 1 1 d .
H8 H 0.4322 0.2072 0.3743 0.046 Uiso 1 1 calc R
C9 C 0.3480(3) 0.4014(3) 0.3624(3) 0.0316(7) Uani 1 1 d .
C10 C 0.3132(4) 0.4422(4) 0.2421(3) 0.0357(7) Uani 1 1 d .
H10A H 0.3915 0.4500 0.1926 0.043 Uiso 1 1 calc R
H10B H 0.2875 0.3741 0.2278 0.043 Uiso 1 1 calc R
C11 C 0.2235(4) 0.6797(4) 0.1492(3) 0.0373(8) Uani 1 1 d .
H11 H 0.3030 0.6917 0.1134 0.045 Uiso 1 1 calc R
C12 C 0.1038(4) 0.7711(4) 0.1444(3) 0.0383(8) Uani 1 1 d .
H12 H 0.0834 0.8588 0.1038 0.046 Uiso 1 1 calc R
C13 C 0.0802(3) 0.5833(3) 0.2561(3) 0.0275(6) Uani 1 1 d .
C14 C -0.1279(4) 0.7713(4) 0.2164(4) 0.0396(8) Uani 1 1 d .
H14A H -0.1671 0.7150 0.2765 0.048 Uiso 1 1 calc R
H14B H -0.1593 0.7759 0.1467 0.048 Uiso 1 1 calc R
C15 C -0.1760(3) 0.9061(3) 0.2355(3) 0.0322(7) Uani 1 1 d .
C16 C -0.2241(4) 1.0122(4) 0.1459(3) 0.0417(8) Uani 1 1 d .
H16 H -0.2234 0.9975 0.0763 0.050 Uiso 1 1 calc R
C17 C -0.2729(4) 1.1390(4) 0.1586(4) 0.0490(10) Uani 1 1 d .
H17 H -0.3040 1.2094 0.0977 0.059 Uiso 1 1 calc R
C18 C -0.2757(4) 1.1612(4) 0.2597(4) 0.0514(10) Uani 1 1 d .
H18 H -0.3084 1.2468 0.2686 0.062 Uiso 1 1 calc R
C19 C -0.2298(4) 1.0562(4) 0.3491(3) 0.0466(9) Uani 1 1 d .
H19 H -0.2327 1.0719 0.4187 0.056 Uiso 1 1 calc R
C20 C -0.1802(3) 0.9304(3) 0.3387(3) 0.0350(7) Uani 1 1 d .
C21 C -0.1337(4) 0.8215(4) 0.4399(3) 0.0447(9) Uani 1 1 d .
H21A H -0.1850 0.8473 0.5060 0.054 Uiso 1 1 calc R
H21B H -0.1506 0.7439 0.4349 0.054 Uiso 1 1 calc R
N1 N 0.0079(3) 0.7877(3) 0.4531(2) 0.0316(6) Uani 1 1 d .
N2 N 0.1958(3) 0.6846(3) 0.5196(2) 0.0289(5) Uani 1 1 d .
N3 N 0.2073(3) 0.5647(3) 0.2170(2) 0.0296(5) Uani 1 1 d .
N4 N 0.0160(3) 0.7108(3) 0.2111(2) 0.0314(6) Uani 1 1 d .
N5 N 0.3170(3) 0.4963(3) 0.4144(2) 0.0302(5) Uani 1 1 d .
F1 F 0.7633(3) 0.5580(3) 0.1545(2) 0.0672(8) Uani 1 1 d .
F2 F 0.7364(4) 0.6185(8) -0.0224(3) 0.193(4) Uani 1 1 d .
F3 F 0.6465(7) 0.4826(4) 0.0785(7) 0.213(4) Uani 1 1 d .
F4 F 0.5448(4) 0.6129(9) 0.1824(3) 0.191(4) Uani 1 1 d .
F5 F 0.5220(3) 0.6741(4) 0.0063(3) 0.0960(12) Uani 1 1 d .
F6 F 0.6391(6) 0.7482(4) 0.0843(7) 0.199(4) Uani 1 1 d .
P P 0.64220(10) 0.61460(10) 0.07920(8) 0.0388(2) Uani 1 1 d .
Au1 Au -0.004465(12) 0.548858(11) 0.636269(9) 0.02860(5) Uani 1 1 d .
N1S N 0.3126(7) 0.0601(6) 0.3244(5) 0.100(2) Uani 1 1 d .
N2S N 0.0965(5) 0.0784(4) 0.1083(4) 0.0720(12) Uani 1 1 d .
C1S C 0.3595(6) 0.0359(5) 0.2449(5) 0.0623(13) Uani 1 1 d .
C2S C 0.4220(7) 0.0037(7) 0.1410(6) 0.092(2) Uani 1 1 d .
H2S1 H 0.4074 -0.0744 0.1366 0.138 Uiso 1 1 calc R
H2S2 H 0.5159 -0.0116 0.1378 0.138 Uiso 1 1 calc R
H2S3 H 0.3845 0.0755 0.0792 0.138 Uiso 1 1 calc R
C3C C 0.0513(5) 0.1819(5) 0.1098(4) 0.0537(10) Uani 1 1 d .
C4S C -0.0087(7) 0.3180(7) 0.1076(9) 0.130(4) Uani 1 1 d .
H4S1 H 0.0338 0.3692 0.0471 0.195 Uiso 1 1 calc R
H4S2 H 0.0012 0.3318 0.1774 0.195 Uiso 1 1 calc R
H4S3 H -0.1017 0.3447 0.0968 0.195 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'
Au Au -2.0133 8.8022 '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
N2 C1 N1 105.3(3) . .
N2 C1 Au1 127.8(2) . .
N1 C1 Au1 126.8(2) . .
C3 C2 N1 106.4(3) . .
C3 C2 H2 126.8 . .
N1 C2 H2 126.8 . .
C2 C3 N2 107.2(3) . .
C2 C3 H3 126.4 . .
N2 C3 H3 126.4 . .
N2 C4 C5 110.9(3) . .
N2 C4 H4A 109.5 . .
C5 C4 H4A 109.5 . .
N2 C4 H4B 109.5 . .
C5 C4 H4B 109.5 . .
H4A C4 H4B 108.1 . .
N5 C5 C6 122.4(3) . .
N5 C5 C4 116.0(3) . .
C6 C5 C4 121.6(3) . .
C7 C6 C5 117.5(3) . .
C7 C6 H6 121.2 . .
C5 C6 H6 121.2 . .
C8 C7 C6 119.9(4) . .
C8 C7 H7 120.0 . .
C6 C7 H7 120.0 . .
C7 C8 C9 119.0(3) . .
C7 C8 H8 120.5 . .
C9 C8 H8 120.5 . .
N5 C9 C8 122.3(3) . .
N5 C9 C10 116.8(3) . .
C8 C9 C10 120.9(3) . .
N3 C10 C9 112.6(3) . .
N3 C10 H10A 109.1 . .
C9 C10 H10A 109.1 . .
N3 C10 H10B 109.1 . .
C9 C10 H10B 109.1 . .
H10A C10 H10B 107.8 . .
C12 C11 N3 107.0(3) . .
C12 C11 H11 126.5 . .
N3 C11 H11 126.5 . .
C11 C12 N4 106.7(3) . .
C11 C12 H12 126.6 . .
N4 C12 H12 126.6 . .
N3 C13 N4 105.2(3) . .
N3 C13 Au1 127.1(2) . 2_566
N4 C13 Au1 127.6(2) . 2_566
N4 C14 C15 114.4(3) . .
N4 C14 H14A 108.7 . .
C15 C14 H14A 108.7 . .
N4 C14 H14B 108.7 . .
C15 C14 H14B 108.7 . .
H14A C14 H14B 107.6 . .
C20 C15 C16 118.5(3) . .
C20 C15 C14 123.5(3) . .
C16 C15 C14 117.9(3) . .
C17 C16 C15 120.8(4) . .
C17 C16 H16 119.6 . .
C15 C16 H16 119.6 . .
C18 C17 C16 120.1(4) . .
C18 C17 H17 120.0 . .
C16 C17 H17 120.0 . .
C17 C18 C19 119.3(4) . .
C17 C18 H18 120.3 . .
C19 C18 H18 120.3 . .
C20 C19 C18 121.9(4) . .
C20 C19 H19 119.1 . .
C18 C19 H19 119.1 . .
C19 C20 C15 119.4(3) . .
C19 C20 C21 118.7(4) . .
C15 C20 C21 121.8(3) . .
N1 C21 C20 113.3(3) . .
N1 C21 H21A 108.9 . .
C20 C21 H21A 108.9 . .
N1 C21 H21B 108.9 . .
C20 C21 H21B 108.9 . .
H21A C21 H21B 107.7 . .
C1 N1 C2 110.5(3) . .
C1 N1 C21 122.0(3) . .
C2 N1 C21 127.4(3) . .
C1 N2 C3 110.5(3) . .
C1 N2 C4 122.5(3) . .
C3 N2 C4 125.8(3) . .
C13 N3 C11 110.7(3) . .
C13 N3 C10 125.1(3) . .
C11 N3 C10 124.2(3) . .
C13 N4 C12 110.3(3) . .
C13 N4 C14 124.8(3) . .
C12 N4 C14 124.2(3) . .
C5 N5 C9 118.8(3) . .
F3 P F2 89.9(5) . .
F3 P F6 177.9(4) . .
F2 P F6 91.3(5) . .
F3 P F4 90.8(5) . .
F2 P F4 179.1(5) . .
F6 P F4 88.0(5) . .
F3 P F5 89.0(3) . .
F2 P F5 91.0(2) . .
F6 P F5 92.7(3) . .
F4 P F5 88.5(2) . .
F3 P F1 92.6(2) . .
F2 P F1 89.6(2) . .
F6 P F1 85.7(2) . .
F4 P F1 90.9(2) . .
F5 P F1 178.3(2) . .
C13 Au1 C1 179.28(11) 2_566 .
N1S C1S C2S 179.5(7) . .
C1S C2S H2S1 109.5 . .
C1S C2S H2S2 109.5 . .
H2S1 C2S H2S2 109.5 . .
C1S C2S H2S3 109.5 . .
H2S1 C2S H2S3 109.5 . .
H2S2 C2S H2S3 109.5 . .
N2S C3C C4S 178.0(7) . .
C3C C4S H4S1 109.5 . .
C3C C4S H4S2 109.5 . .
H4S1 C4S H4S2 109.5 . .
C3C C4S H4S3 109.5 . .
H4S1 C4S H4S3 109.5 . .
H4S2 C4S H4S3 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N2 1.343(4) .
C1 N1 1.349(4) .
C1 Au1 2.020(3) .
C2 C3 1.346(5) .
C2 N1 1.378(4) .
C2 H2 0.9400 .
C3 N2 1.371(4) .
C3 H3 0.9400 .
C4 N2 1.451(4) .
C4 C5 1.508(5) .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C5 N5 1.334(4) .
C5 C6 1.415(5) .
C6 C7 1.376(6) .
C6 H6 0.9400 .
C7 C8 1.374(5) .
C7 H7 0.9400 .
C8 C9 1.386(5) .
C8 H8 0.9400 .
C9 N5 1.333(4) .
C9 C10 1.527(5) .
C10 N3 1.446(5) .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C11 C12 1.344(6) .
C11 N3 1.384(4) .
C11 H11 0.9400 .
C12 N4 1.390(5) .
C12 H12 0.9400 .
C13 N3 1.348(4) .
C13 N4 1.356(4) .
C13 Au1 2.015(3) 2_566
C14 N4 1.469(5) .
C14 C15 1.506(5) .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C15 C20 1.399(5) .
C15 C16 1.402(5) .
C16 C17 1.391(6) .
C16 H16 0.9400 .
C17 C18 1.365(6) .
C17 H17 0.9400 .
C18 C19 1.389(6) .
C18 H18 0.9400 .
C19 C20 1.371(5) .
C19 H19 0.9400 .
C20 C21 1.507(5) .
C21 N1 1.477(5) .
C21 H21A 0.9800 .
C21 H21B 0.9800 .
F1 P 1.592(3) .
F2 P 1.497(4) .
F3 P 1.481(4) .
F4 P 1.530(4) .
F5 P 1.564(3) .
F6 P 1.521(4) .
Au1 C13 2.015(3) 2_566
N1S C1S 1.108(7) .
N2S C3C 1.103(6) .
C1S C2S 1.454(8) .
C2S H2S1 0.9700 .
C2S H2S2 0.9700 .
C2S H2S3 0.9700 .
C3C C4S 1.439(8) .
C4S H4S1 0.9700 .
C4S H4S2 0.9700 .
C4S H4S3 0.9700 .
