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#$Date: 2019-11-17 13:54:56 +0200 (Sun, 17 Nov 2019) $
#$Revision: 230309 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/69/7056989.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_7056989
loop_
_publ_author_name
'Lu, Taotao'
'Yang, Chu-Fan'
'Steren, Carlos A.'
'Fei, Fan'
'Chen, Xue-Tai'
'Xue, Zi-Ling'
_publ_section_title
;
 Synthesis and characterization of Ag(i) and Au(i) complexes with
 macrocyclic hybrid amine N-heterocyclic carbene ligands
;
_journal_issue                   6
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              4700
_journal_paper_doi               10.1039/C7NJ04020B
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety         'C46 H52 Ag3 N12, 3(F6 P) [+ solvent]'
_chemical_formula_sum            'C46 H52 Ag3 F18 N12 P3'
_chemical_formula_weight         1531.51
_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_Hall           '-C 2c 2'
_space_group_name_H-M_alt        'C m c m'
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-01-21 deposited with the CCDC.
2018-02-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.284(2)
_cell_length_b                   21.324(3)
_cell_length_c                   17.361(2)
_cell_measurement_reflns_used    5494
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.19
_cell_measurement_theta_min      2.24
_cell_volume                     6028.4(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'APEX2 CCD detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1132
_diffrn_reflns_av_unetI/netI     0.0665
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            25651
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.543
_diffrn_reflns_theta_min         2.242
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.143
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4972
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.687
_exptl_crystal_description       plate
_exptl_crystal_F_000             3040
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.130
_refine_diff_density_max         1.857
_refine_diff_density_min         -1.897
_refine_diff_density_rms         0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.167
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         3714
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.167
_refine_ls_R_factor_all          0.0955
_refine_ls_R_factor_gt           0.0703
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0954P)²+4.2326P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1646
_refine_ls_wR_factor_ref         0.1767
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2860
_reflns_number_total             3714
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7nj04020b2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7056979--7056989.cif.'
_cod_original_cell_volume        6028.4(15)
_cod_database_code               7056989
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.690
_shelx_estimated_absorpt_t_max   0.866
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z-1/2'
'x, -y, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z-1/2'
'x+1/2, -y+1/2, z-1/2'
'-x+1/2, y+1/2, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Ag1 Ag 0.10171(3) 0.27463(3) 0.2500 0.01673(19) Uani 1 2 d S T P
Ag2 Ag 0.0000 0.13864(5) 0.2500 0.0271(3) Uani 1 4 d S T P
C1 C 0.1116(3) 0.2764(2) 0.3704(3) 0.0169(11) Uani 1 1 d . . .
C2 C 0.1384(3) 0.2472(3) 0.4936(3) 0.0175(11) Uani 1 1 d . . .
C3 C 0.1173(3) 0.3103(3) 0.4947(3) 0.0170(11) Uani 1 1 d . . .
C4 C 0.1178(3) 0.3457(3) 0.5628(3) 0.0233(13) Uani 1 1 d . . .
H4 H 0.1056 0.3893 0.5634 0.028 Uiso 1 1 calc R U .
C5 C 0.1369(4) 0.3133(3) 0.6281(3) 0.0283(14) Uani 1 1 d . . .
H5 H 0.1363 0.3348 0.6759 0.034 Uiso 1 1 calc R U .
C6 C 0.1577(4) 0.2490(3) 0.6275(3) 0.0312(15) Uani 1 1 d . . .
H6 H 0.1706 0.2287 0.6747 0.037 Uiso 1 1 calc R U .
C7 C 0.1596(4) 0.2150(3) 0.5604(3) 0.0240(13) Uani 1 1 d . . .
H7 H 0.1746 0.1720 0.5595 0.029 Uiso 1 1 calc R U .
C8 C 0.0789(3) 0.3904(2) 0.3909(3) 0.0177(11) Uani 1 1 d . . .
H8A H 0.0744 0.3900 0.3341 0.021 Uiso 1 1 calc R U .
H8B H 0.1244 0.4191 0.4047 0.021 Uiso 1 1 calc R U .
C9 C 0.0000 0.4168(3) 0.4236(4) 0.0184(16) Uani 1 2 d S T P
H9A H 0.0000 0.4627 0.4153 0.022 Uiso 1 2 calc R U P
H9B H 0.0000 0.4096 0.4800 0.022 Uiso 1 2 calc R U P
C10 C 0.1480(4) 0.1635(3) 0.3916(3) 0.0223(12) Uani 1 1 d . . .
H10A H 0.1978 0.1468 0.4172 0.027 Uiso 1 1 calc R U .
H10B H 0.1575 0.1628 0.3353 0.027 Uiso 1 1 calc R U .
C11 C 0.0757(4) 0.1222(3) 0.4107(3) 0.0231(13) Uani 1 1 d . . .
H11A H 0.0857 0.0792 0.3911 0.028 Uiso 1 1 calc R U .
H11B H 0.0688 0.1198 0.4673 0.028 Uiso 1 1 calc R U .
F1 F 1.0000 0.4668(3) 0.2500 0.043(2) Uani 1 4 d S T P
F2 F 1.0000 0.6165(4) 0.2500 0.061(3) Uani 1 4 d S T P
F3 F 0.9310(3) 0.5414(2) 0.3158(2) 0.0490(11) Uani 1 1 d . . .
F4 F 0.1360(3) 0.0000 0.5000 0.0461(15) Uani 1 2 d S T P
F5 F 0.3319(3) 0.0000 0.5000 0.0315(12) Uani 1 2 d S T P
F6 F 0.2334(2) 0.03228(17) 0.4173(2) 0.0402(10) Uani 1 1 d . . .
F7 F 0.2335(2) 0.06808(16) 0.5388(2) 0.0379(9) Uani 1 1 d . . .
N1 N 0.1004(3) 0.3265(2) 0.4172(3) 0.0170(9) Uani 1 1 d . . .
N2 N 0.1345(3) 0.2283(2) 0.4165(3) 0.0160(9) Uani 1 1 d . . .
N3 N 0.0000 0.1480(3) 0.3752(4) 0.0203(14) Uani 1 2 d S T P
H3 H 0.0000 0.1940 0.3864 0.024 Uiso 1 2 calc R U P
P3 P 0.23368(13) 0.0000 0.5000 0.0220(5) Uani 1 2 d S T P
P4 P 1.0000 0.54227(16) 0.2500 0.0305(8) Uani 1 4 d S T P
N4 N 0.1160(7) 0.0509(6) 0.2500 0.077(3) Uani 1 2 d S TU P
C12 C 0.1810(10) 0.0224(7) 0.2500 0.080(4) Uani 1 2 d S TU P
C13 C 0.2407(10) -0.0274(7) 0.2500 0.096(4) Uani 1 2 d S TU P
H13A H 0.2692 -0.0262 0.2997 0.145 Uiso 0.5 1 d R U P
H13B H 0.2796 -0.0174 0.2087 0.145 Uiso 0.5 1 d R U P
H13C H 0.2180 -0.0694 0.2416 0.145 Uiso 0.5 1 d R U P
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 170.9(3) . 10_556
C1 Ag1 Ag1 94.41(14) . 3
C1 Ag1 Ag1 94.41(14) 10_556 3
C1 Ag1 Ag2 93.06(14) . .
C1 Ag1 Ag2 93.06(14) 10_556 .
Ag1 Ag1 Ag2 60.267(14) 3 .
N3 Ag2 N3 169.5(3) 10_556 .
N3 Ag2 N4 93.69(12) 10_556 .
N3 Ag2 N4 93.69(12) . .
N3 Ag2 Ag1 85.45(15) 10_556 .
N3 Ag2 Ag1 85.45(15) . .
N4 Ag2 Ag1 105.0(3) . .
N3 Ag2 Ag1 85.45(15) 10_556 3
N3 Ag2 Ag1 85.45(15) . 3
N4 Ag2 Ag1 164.5(3) . 3
Ag1 Ag2 Ag1 59.47(3) . 3
N2 C1 N1 106.3(5) . .
N2 C1 Ag1 126.7(4) . .
N1 C1 Ag1 127.0(4) . .
C3 C2 C7 122.0(5) . .
C3 C2 N2 106.3(5) . .
C7 C2 N2 131.7(5) . .
C2 C3 C4 122.1(5) . .
C2 C3 N1 105.8(5) . .
C4 C3 N1 132.1(5) . .
C5 C4 C3 115.4(5) . .
C5 C4 H4 122.3 . .
C3 C4 H4 122.3 . .
C4 C5 C6 122.8(5) . .
C4 C5 H5 118.6 . .
C6 C5 H5 118.6 . .
C7 C6 C5 121.6(6) . .
C7 C6 H6 119.2 . .
C5 C6 H6 119.2 . .
C6 C7 C2 116.1(5) . .
C6 C7 H7 121.9 . .
C2 C7 H7 121.9 . .
N1 C8 C9 115.4(5) . .
N1 C8 H8A 108.4 . .
C9 C8 H8A 108.4 . .
N1 C8 H8B 108.4 . .
C9 C8 H8B 108.4 . .
H8A C8 H8B 107.5 . .
C8 C9 C8 116.2(6) . 12
C8 C9 H9A 108.2 . .
C8 C9 H9A 108.2 12 .
C8 C9 H9B 108.2 . .
C8 C9 H9B 108.2 12 .
H9A C9 H9B 107.4 . .
N2 C10 C11 111.7(5) . .
N2 C10 H10A 109.3 . .
C11 C10 H10A 109.3 . .
N2 C10 H10B 109.3 . .
C11 C10 H10B 109.3 . .
H10A C10 H10B 107.9 . .
N3 C11 C10 109.9(5) . .
N3 C11 H11A 109.7 . .
C10 C11 H11A 109.7 . .
N3 C11 H11B 109.7 . .
C10 C11 H11B 109.7 . .
H11A C11 H11B 108.2 . .
C1 N1 C3 110.6(5) . .
C1 N1 C8 125.0(5) . .
C3 N1 C8 124.3(5) . .
C1 N2 C2 111.0(4) . .
C1 N2 C10 125.6(5) . .
C2 N2 C10 123.2(4) . .
C11 N3 C11 112.3(6) 12 .
C11 N3 Ag2 112.3(4) 12 .
C11 N3 Ag2 112.3(4) . .
C11 N3 H3 106.4 12 .
C11 N3 H3 106.4 . .
Ag2 N3 H3 106.4 . .
F4 P3 F6 89.84(16) . 4_556
F4 P3 F6 89.84(16) . .
F6 P3 F6 179.7(3) 4_556 .
F4 P3 F5 180.0 . .
F6 P3 F5 90.16(16) 4_556 .
F6 P3 F5 90.16(16) . .
F4 P3 F7 89.90(15) . 4_556
F6 P3 F7 89.3(2) 4_556 4_556
F6 P3 F7 90.7(2) . 4_556
F5 P3 F7 90.10(15) . 4_556
F4 P3 F7 89.90(15) . .
F6 P3 F7 90.7(2) 4_556 .
F6 P3 F7 89.3(2) . .
F5 P3 F7 90.10(15) . .
F7 P3 F7 179.8(3) 4_556 .
F2 P4 F3 90.7(2) . 12_755
F2 P4 F3 90.7(2) . 10_556
F3 P4 F3 178.6(4) 12_755 10_556
F2 P4 F3 90.7(2) . 3_755
F3 P4 F3 90.9(3) 12_755 3_755
F3 P4 F3 89.1(3) 10_556 3_755
F2 P4 F3 90.7(2) . .
F3 P4 F3 89.1(3) 12_755 .
F3 P4 F3 90.9(3) 10_556 .
F3 P4 F3 178.6(4) 3_755 .
F2 P4 F1 180.0 . .
F3 P4 F1 89.3(2) 12_755 .
F3 P4 F1 89.3(2) 10_556 .
F3 P4 F1 89.3(2) 3_755 .
F3 P4 F1 89.3(2) . .
C12 N4 Ag2 165.1(13) . .
N4 C12 C13 162.4(19) . .
C12 C13 H13A 107.5 . .
C12 C13 H13B 106.1 . .
H13A C13 H13B 109.5 . .
C12 C13 H13C 114.7 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ag1 C1 2.097(6) .
Ag1 C1 2.097(6) 10_556
Ag1 Ag1 3.3126(12) 3
Ag1 Ag2 3.3396(11) .
Ag2 N3 2.183(7) 10_556
Ag2 N3 2.183(7) .
Ag2 N4 2.659(9) .
Ag2 Ag1 3.3396(11) 3
C1 N2 1.353(7) .
C1 N1 1.354(7) .
C2 C3 1.387(8) .
C2 C7 1.391(7) .
C2 N2 1.400(7) .
C3 C4 1.404(8) .
C3 N1 1.415(7) .
C4 C5 1.364(8) .
C4 H4 0.9500 .
C5 C6 1.412(9) .
C5 H5 0.9500 .
C6 C7 1.372(8) .
C6 H6 0.9500 .
C7 H7 0.9500 .
C8 N1 1.481(7) .
C8 C9 1.512(6) .
C8 H8A 0.9900 .
C8 H8B 0.9900 .
C9 C8 1.512(6) 12
C9 H9A 0.9900 .
C9 H9B 0.9900 .
C10 N2 1.463(7) .
C10 C11 1.507(8) .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
C11 N3 1.485(6) .
C11 H11A 0.9900 .
C11 H11B 0.9900 .
F1 P4 1.609(8) .
F2 P4 1.583(9) .
F3 P4 1.602(4) .
F4 P3 1.591(6) .
F5 P3 1.599(5) .
F6 P3 1.593(4) .
F7 P3 1.601(3) .
N3 C11 1.485(6) 12
N3 H3 1.0000 .
P3 F6 1.593(4) 4_556
P3 F7 1.601(3) 4_556
P4 F3 1.602(4) 12_755
P4 F3 1.602(4) 10_556
P4 F3 1.602(4) 3_755
N4 C12 1.221(15) .
C12 C13 1.439(17) .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
