#------------------------------------------------------------------------------
#$Date: 2023-03-01 11:02:49 +0200 (Wed, 01 Mar 2023) $
#$Revision: 281198 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/24/7712464.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_7712464
loop_
_publ_author_name
'Kitase, Kosuke'
'Akahoshi, Daisuke'
'Kitazawa, Takafumi'
_publ_section_title
;
Guest-triggered "Soma-Iwamoto-type" penetration complex
{Fe(4-methoxypyrimidine)2[M(CN)2]2}·Guest
(M = Ag, Au).
;
_journal_issue 9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first 2571
_journal_page_last 2579
_journal_paper_doi 10.1039/d2dt03716e
_journal_volume 52
_journal_year 2023
_chemical_formula_sum 'C31 H28 Ag4 Fe2 N17 O5'
_chemical_formula_weight 1261.88
_space_group_crystal_system monoclinic
_space_group_IT_number 15
_space_group_name_Hall '-C 2yc'
_space_group_name_H-M_alt 'C 1 2/c 1'
_atom_sites_solution_hydrogens geom
_audit_creation_method SHELXL-2017/1
_audit_update_record
;
2022-07-20 deposited with the CCDC. 2023-01-23 downloaded from the CCDC.
;
_cell_angle_alpha 90
_cell_angle_beta 90.039(4)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 29.288(6)
_cell_length_b 10.788(2)
_cell_length_c 14.325(3)
_cell_measurement_reflns_used 4103
_cell_measurement_temperature 296(2)
_cell_measurement_theta_max 24.12
_cell_measurement_theta_min 2.46
_cell_volume 4526.1(16)
_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-2017/1 (Sheldrick, 2017)'
_computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature 296(2)
_diffrn_detector_area_resol_mean 8.336
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0363
_diffrn_reflns_av_unetI/netI 0.0460
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max 39
_diffrn_reflns_limit_h_min -37
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_number 15585
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 28.422
_diffrn_reflns_theta_min 1.391
_exptl_absorpt_coefficient_mu 2.376
_exptl_absorpt_correction_T_max 0.82
_exptl_absorpt_correction_T_min 0.62
_exptl_absorpt_correction_type 'Numerical Mu From Formula'
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.852
_exptl_crystal_description plate
_exptl_crystal_F_000 2452
_exptl_crystal_preparation 'Magnetic properties'
_exptl_crystal_size_max 0.218
_exptl_crystal_size_mid 0.204
_exptl_crystal_size_min 0.088
_refine_diff_density_max 0.818
_refine_diff_density_min -0.921
_refine_diff_density_rms 0.133
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.836
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 347
_refine_ls_number_reflns 5665
_refine_ls_number_restraints 26
_refine_ls_restrained_S_all 0.837
_refine_ls_R_factor_all 0.0617
_refine_ls_R_factor_gt 0.0410
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.6143P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1140
_refine_ls_wR_factor_ref 0.1314
_reflns_Friedel_coverage 0.000
_reflns_number_gt 4262
_reflns_number_total 5665
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file d2dt03716e2.cif
_cod_data_source_block test_1_a_CCDC7
_cod_original_cell_volume 4526.1(17)
_cod_original_sg_symbol_H-M 'C 2/c'
_cod_database_code 7712464
_shelx_shelxl_version_number 2017/1
_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 0.625
_shelx_estimated_absorpt_t_max 0.818
_shelx_res_file
;
TITL test_1_a.res in C2/c
test_1_a.res
created by SHELXL-2017/1 at 14:43:13 on 11-Nov-2021
CELL 0.71073 29.2881 10.7883 14.3246 90.000 90.039 90.000
ZERR 4.000 0.0063 0.0024 0.0031 0.000 0.004 0.000
LATT 7
SYMM X, -Y, 1/2+Z
SFAC C H Ag Fe N O
UNIT 124 112 16 8 68 20
L.S. 32
ACTA
BOND $H
FMAP 2
PLAN 5
Dang 2.41 C51A C52A N51A C53A
SIZE 0.088 0.204 0.218
twin 1 0 0 0 -1 0 0 0 -1
DFIX 1.54 O2B C14B O51A C54A
DFIX 1.3 C13B O2B C13A O2A
DFIX 1.39 C51A N51A N51A C52A C52A C53A
DELU C51A N51A C52A C53A
SIMU C14B C54A
SIMU N7A N7B
TEMP 23.000
WGHT 0.100000 0.614273
BASF 0.47272
FVAR 0.11097 0.48190 0.41351
AG1 3 0.632600 0.380642 0.764091 11.00000 0.04883 0.07566 =
0.04775 -0.00551 0.02318 0.01555
AG2 3 0.886011 0.168784 0.741164 11.00000 0.04950 0.08143 =
0.05534 0.01697 -0.01875 0.01122
C1 1 0.682592 0.339061 0.669025 11.00000 0.05380 0.06293 =
0.03434 -0.00202 0.01496 0.01581
C2 1 0.582358 0.421894 0.858107 11.00000 0.03942 0.07024 =
0.04080 -0.00267 0.01597 0.00975
C3 1 0.834541 0.215724 0.649221 11.00000 0.03922 0.05885 =
0.04785 0.00918 -0.00665 0.00494
C4 1 0.936023 0.118615 0.836684 11.00000 0.04585 0.07919 =
0.03896 0.00980 -0.01187 0.01394
FE1 4 0.750000 0.250000 0.500000 10.50000 0.02437 0.04812 =
0.02764 -0.00074 0.00312 0.00855
FE2 4 0.500000 0.500000 1.000000 10.50000 0.02314 0.04631 =
0.02583 0.00177 0.00257 0.01010
N1 5 0.707601 0.314683 0.612056 11.00000 0.04416 0.05811 =
0.04107 -0.00351 0.01405 0.00855
N2 5 0.554097 0.450397 0.908897 11.00000 0.03778 0.06792 =
0.03844 0.00226 0.01153 0.00964
N3 5 0.805808 0.232922 0.596796 11.00000 0.03661 0.06152 =
0.04047 0.00235 -0.00495 0.00796
N4 5 0.961177 0.081060 0.888722 11.00000 0.04610 0.08004 =
0.04564 0.01357 -0.00483 0.01825
N5 5 0.770759 0.443520 0.463430 11.00000 0.03750 0.05345 =
0.04003 0.00671 0.00453 0.00042
N6 5 0.801802 0.636581 0.511882 11.00000 0.05673 0.05599 =
0.05165 0.00563 0.00000 0.00164
C5 1 0.787856 0.518866 0.526127 11.00000 0.05893 0.05682 =
0.03826 0.00028 -0.00845 0.00807
AFIX 43
H5 2 0.790660 0.488122 0.586514 11.00000 -1.20000
AFIX 0
C6 1 0.765944 0.490720 0.376298 11.00000 0.05709 0.06709 =
0.04238 0.00508 -0.00028 -0.01121
AFIX 43
H6 2 0.753532 0.441376 0.329484 11.00000 -1.20000
AFIX 0
C7 1 0.778731 0.607371 0.356100 11.00000 0.07292 0.06984 =
0.03873 0.01879 0.00125 -0.00538
AFIX 43
H7 2 0.775544 0.638920 0.296029 11.00000 -1.20000
AFIX 0
C8 1 0.796897 0.679705 0.427691 11.00000 0.04408 0.06167 =
0.06158 0.01007 0.00312 -0.00415
C9 1 0.830112 0.867099 0.479555 11.00000 0.08182 0.07057 =
0.07332 -0.00574 0.00340 -0.01399
AFIX 137
H9A 2 0.858059 0.828734 0.499382 11.00000 -1.50000
H9B 2 0.809533 0.872691 0.531519 11.00000 -1.50000
H9C 2 0.836450 0.948745 0.456275 11.00000 -1.50000
PART 1
AFIX 66
N7A 5 0.467809 0.316795 0.986032 21.00000 0.01656 0.03497 =
0.08399 0.00110 0.01880 0.00222
C11A 1 0.421154 0.303704 0.971165 21.00000 0.04579 0.03740 =
0.06145 0.00289 -0.00027 -0.00163
AFIX 43
H11A 2 0.403202 0.373252 0.959990 21.00000 -1.20000
AFIX 65
C12A 1 0.401330 0.186667 0.973000 21.00000 0.03782 0.05945 =
0.09668 -0.01867 0.00961 0.00471
AFIX 43
H12A 2 0.370114 0.177909 0.963053 21.00000 -1.20000
AFIX 65
C13A 1 0.428160 0.082719 0.989702 21.00000 0.05276 0.04857 =
0.08163 -0.02370 -0.00688 0.01347
N8A 5 0.474816 0.095808 1.004569 21.00000 0.04497 0.03764 =
0.12447 0.00207 -0.00494 -0.01330
C10A 1 0.494641 0.212845 1.002734 21.00000 0.07064 0.06156 =
0.06840 -0.00511 -0.02077 -0.01582
AFIX 43
H10A 2 0.525857 0.221602 1.012681 21.00000 -1.20000
AFIX 0
O2A 6 0.409454 -0.023892 0.994369 21.00000 0.05315 0.04460 =
0.16954 -0.00158 0.01238 -0.01366
C14A 1 0.437661 -0.131673 1.020005 21.00000 0.08983 0.03738 =
0.16655 -0.01175 -0.01794 -0.00314
AFIX 137
H14A 2 0.468924 -0.115708 1.003892 21.00000 -1.50000
H14B 2 0.427088 -0.203505 0.986865 21.00000 -1.50000
H14C 2 0.435358 -0.146064 1.085969 21.00000 -1.50000
AFIX 0
C51A 1 0.500000 0.200900 0.750000 30.50000 0.11003 0.11869 =
0.22939 0.00000 -0.11803 0.00000
AFIX 43
H51A 2 0.500000 0.287105 0.749998 30.50000 -1.20000
AFIX 0
C52A 1 0.459950 0.018587 0.741822 31.00000 0.06177 0.11202 =
0.05346 0.00116 0.00166 0.00261
C53A 1 0.500000 -0.052777 0.750000 30.50000 0.08499 0.08575 =
0.10798 0.00000 0.01519 0.00000
AFIX 43
H53A 2 0.500000 -0.138981 0.749999 30.50000 -1.20000
AFIX 0
N51A 5 0.457830 0.141793 0.746310 31.00000 0.09485 0.09902 =
0.08973 -0.00181 -0.01622 0.01770
O51A 6 0.421726 -0.040119 0.736600 31.00000 0.08111 0.07122 =
0.14426 0.01674 -0.00600 -0.01801
C54A 1 0.382034 0.052469 0.723355 31.00000 0.20653 0.09772 =
0.16307 0.04000 0.04087 0.10212
AFIX 133
H54A 2 0.383474 0.114857 0.771054 31.00000 -1.50000
H54B 2 0.353475 0.009181 0.727647 31.00000 -1.50000
H54C 2 0.384479 0.090927 0.663130 31.00000 -1.50000
PART 2
AFIX 66
N7B 5 0.465085 0.327605 0.956866 -21.00000 0.05873 0.05577 =
0.07799 -0.00308 0.01058 0.00216
C11B 1 0.444565 0.248300 1.020777 -21.00000 0.11526 0.10143 =
0.04688 -0.00048 0.03353 -0.00105
AFIX 43
H11B 2 0.445945 0.265895 1.084273 -21.00000 -1.20000
AFIX 65
C12B 1 0.421983 0.142696 0.989786 -21.00000 0.13726 0.11908 =
0.10896 -0.05503 0.07562 -0.09786
AFIX 43
H12B 2 0.408254 0.089636 1.032548 -21.00000 -1.20000
AFIX 65
C13B 1 0.419920 0.116398 0.894884 -21.00000 0.12221 0.07200 =
0.13064 -0.00349 0.01608 -0.04524
N8B 5 0.440440 0.195702 0.830972 -21.00000 0.10177 0.07769 =
0.07383 -0.02913 0.00517 -0.02789
C10B 1 0.463023 0.301306 0.861962 -21.00000 0.06276 0.09477 =
0.05242 -0.02126 -0.00376 -0.00856
AFIX 43
H10B 2 0.476752 0.354366 0.819200 -21.00000 -1.20000
AFIX 0
O2B 6 0.398074 0.023353 0.859225 -21.00000 0.26502 0.12789 =
0.17670 -0.04018 0.06374 -0.13093
C14B 1 0.384199 0.015490 0.754703 -21.00000 0.10903 0.06742 =
0.17644 -0.04262 0.01455 -0.02764
AFIX 137
H14D 2 0.354392 0.050890 0.746513 -21.00000 -1.50000
H14E 2 0.383745 -0.069718 0.735409 -21.00000 -1.50000
H14F 2 0.405886 0.060441 0.717596 -21.00000 -1.50000
PART 0
AFIX 0
O1 6 0.810073 0.795640 0.408627 11.00000 0.07482 0.06543 =
0.07691 0.02092 -0.00289 -0.01785
HKLF 4
REM test_1_a.res in C2/c
REM R1 = 0.0410 for 4262 Fo > 4sig(Fo) and 0.0617 for all 5665 data
REM 347 parameters refined using 26 restraints
END
WGHT 0.0589 0.0000
REM Highest difference peak 0.818, deepest hole -0.921, 1-sigma level 0.133
Q1 1 0.4588 -0.0735 0.7411 11.00000 0.05 0.82
Q2 1 0.4241 0.1019 0.7437 11.00000 0.05 0.76
Q3 1 0.4589 0.0462 0.7499 11.00000 0.05 0.76
Q4 1 0.5000 0.1106 0.7500 10.50000 0.05 0.60
Q5 1 0.4294 0.0779 0.7931 11.00000 0.05 0.56
;
_shelx_res_checksum 9328
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'
'-x, -y, -z'
'-x, y, -z-1/2'
'-x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z-1/2'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ag1 Ag 0.63260(2) 0.38064(6) 0.76409(4) 0.05740(17) Uani 1 1 d . . . . .
Ag2 Ag 0.88601(2) 0.16878(6) 0.74116(5) 0.06210(19) Uani 1 1 d . . . . .
C1 C 0.6826(3) 0.3391(7) 0.6690(5) 0.0503(16) Uani 1 1 d . . . . .
C2 C 0.5824(2) 0.4219(7) 0.8581(5) 0.0501(16) Uani 1 1 d . . . . .
C3 C 0.8345(2) 0.2157(7) 0.6492(5) 0.0486(15) Uani 1 1 d . . . . .
C4 C 0.9360(2) 0.1186(8) 0.8367(5) 0.0547(17) Uani 1 1 d . . . . .
Fe1 Fe 0.750000 0.250000 0.500000 0.0334(2) Uani 1 2 d S . P . .
Fe2 Fe 0.500000 0.500000 1.000000 0.0318(2) Uani 1 2 d S . P . .
N1 N 0.70760(19) 0.3147(6) 0.6121(4) 0.0478(13) Uani 1 1 d . . . . .
N2 N 0.55410(18) 0.4504(6) 0.9089(4) 0.0480(13) Uani 1 1 d . . . . .
N3 N 0.80581(19) 0.2329(6) 0.5968(4) 0.0462(13) Uani 1 1 d . . . . .
N4 N 0.9612(2) 0.0811(7) 0.8887(4) 0.0573(15) Uani 1 1 d . . . . .
N5 N 0.77076(17) 0.4435(5) 0.4634(4) 0.0437(12) Uani 1 1 d . . . . .
N6 N 0.8018(2) 0.6366(6) 0.5119(5) 0.0548(15) Uani 1 1 d . . . . .
C5 C 0.7879(2) 0.5189(7) 0.5261(5) 0.0513(16) Uani 1 1 d . . . . .
H5 H 0.790660 0.488122 0.586514 0.062 Uiso 1 1 calc R U . . .
C6 C 0.7659(2) 0.4907(8) 0.3763(5) 0.0555(17) Uani 1 1 d . . . . .
H6 H 0.753532 0.441376 0.329484 0.067 Uiso 1 1 calc R U . . .
C7 C 0.7787(3) 0.6074(8) 0.3561(5) 0.0605(19) Uani 1 1 d . . . . .
H7 H 0.775544 0.638920 0.296029 0.073 Uiso 1 1 calc R U . . .
C8 C 0.7969(2) 0.6797(7) 0.4277(6) 0.0558(18) Uani 1 1 d . . . . .
C9 C 0.8301(4) 0.8671(8) 0.4796(7) 0.075(2) Uani 1 1 d . . . . .
H9A H 0.858059 0.828734 0.499382 0.113 Uiso 1 1 calc R U . . .
H9B H 0.809533 0.872691 0.531519 0.113 Uiso 1 1 calc R U . . .
H9C H 0.836450 0.948745 0.456275 0.113 Uiso 1 1 calc R U . . .
N7A N 0.4678(3) 0.3168(5) 0.9860(9) 0.045(4) Uani 0.482(7) 1 d G U P A 1
C11A C 0.4212(3) 0.3037(6) 0.9712(9) 0.048(3) Uani 0.482(7) 1 d G . P A 1
H11A H 0.403202 0.373252 0.959990 0.058 Uiso 0.482(7) 1 calc R U P A 1
C12A C 0.4013(2) 0.1867(8) 0.9730(9) 0.065(6) Uani 0.482(7) 1 d G . P A 1
H12A H 0.370114 0.177909 0.963053 0.078 Uiso 0.482(7) 1 calc R U P A 1
C13A C 0.4282(3) 0.0827(6) 0.9897(10) 0.061(5) Uani 0.482(7) 1 d DG . P A 1
N8A N 0.4748(3) 0.0958(6) 1.0046(9) 0.069(5) Uani 0.482(7) 1 d G . P A 1
C10A C 0.4946(2) 0.2128(7) 1.0027(9) 0.067(5) Uani 0.482(7) 1 d G . P A 1
H10A H 0.525857 0.221602 1.012681 0.080 Uiso 0.482(7) 1 calc R U P A 1
O2A O 0.4095(4) -0.0239(9) 0.9944(15) 0.089(5) Uani 0.482(7) 1 d D . P A 1
C14A C 0.4377(9) -0.1317(16) 1.020(2) 0.098(9) Uani 0.482(7) 1 d . . P A 1
H14A H 0.468924 -0.115708 1.003892 0.147 Uiso 0.482(7) 1 calc R U P A 1
H14B H 0.427088 -0.203505 0.986865 0.147 Uiso 0.482(7) 1 calc R U P A 1
H14C H 0.435358 -0.146064 1.085969 0.147 Uiso 0.482(7) 1 calc R U P A 1
C51A C 0.500000 0.201(3) 0.750000 0.15(2) Uani 0.414(6) 2 d DS TU P B 1
H51A H 0.500000 0.287105 0.749998 0.183 Uiso 0.414(6) 2 calc R U P B 1
C52A C 0.4599(6) 0.0186(17) 0.7418(18) 0.076(5) Uani 0.414(6) 1 d D U P B 1
C53A C 0.500000 -0.053(2) 0.750000 0.093(9) Uani 0.414(6) 2 d DS TU P B 1
H53A H 0.500000 -0.138981 0.749999 0.111 Uiso 0.414(6) 2 calc R U P B 1
N51A N 0.4578(6) 0.1418(15) 0.7463(18) 0.095(6) Uani 0.414(6) 1 d D U P B 1
O51A O 0.4217(6) -0.0401(14) 0.7366(19) 0.099(6) Uani 0.414(6) 1 d D . P B 1
C54A C 0.3820(15) 0.052(4) 0.723(4) 0.16(2) Uani 0.414(6) 1 d D U P B 1
H54A H 0.383474 0.114857 0.771054 0.234 Uiso 0.414(6) 1 calc R U P B 1
H54B H 0.353475 0.009181 0.727647 0.234 Uiso 0.414(6) 1 calc R U P B 1
H54C H 0.384479 0.090927 0.663130 0.234 Uiso 0.414(6) 1 calc R U P B 1
N7B N 0.4651(5) 0.3276(10) 0.9569(8) 0.064(5) Uani 0.518(7) 1 d G U P A 2
C11B C 0.4446(5) 0.2483(13) 1.0208(6) 0.088(6) Uani 0.518(7) 1 d G . P A 2
H11B H 0.445945 0.265895 1.084273 0.105 Uiso 0.518(7) 1 calc R U P A 2
C12B C 0.4220(6) 0.1427(13) 0.9898(9) 0.122(15) Uani 0.518(7) 1 d G . P A 2
H12B H 0.408254 0.089636 1.032548 0.146 Uiso 0.518(7) 1 calc R U P A 2
C13B C 0.4199(6) 0.1164(11) 0.8949(10) 0.108(8) Uani 0.518(7) 1 d DG . P A 2
N8B N 0.4404(5) 0.1957(11) 0.8310(7) 0.084(5) Uani 0.518(7) 1 d G . P A 2
C10B C 0.4630(4) 0.3013(9) 0.8620(7) 0.070(4) Uani 0.518(7) 1 d G . P A 2
H10B H 0.476752 0.354366 0.819200 0.084 Uiso 0.518(7) 1 calc R U P A 2
O2B O 0.3981(9) 0.0234(19) 0.8592(17) 0.190(13) Uani 0.518(7) 1 d D . P A 2
C14B C 0.3842(10) 0.015(2) 0.755(2) 0.118(12) Uani 0.518(7) 1 d D U P A 2
H14D H 0.354392 0.050890 0.746513 0.176 Uiso 0.518(7) 1 calc R U P A 2
H14E H 0.383745 -0.069718 0.735409 0.176 Uiso 0.518(7) 1 calc R U P A 2
H14F H 0.405886 0.060441 0.717596 0.176 Uiso 0.518(7) 1 calc R U P A 2
O1 O 0.8101(2) 0.7956(6) 0.4086(5) 0.0724(17) Uani 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ag1 0.0488(3) 0.0757(3) 0.0478(3) -0.0055(3) 0.0232(2) 0.0155(2)
Ag2 0.0495(3) 0.0814(4) 0.0553(3) 0.0170(3) -0.0187(3) 0.0112(3)
C1 0.054(4) 0.063(4) 0.034(3) -0.002(3) 0.015(3) 0.016(3)
C2 0.039(3) 0.070(4) 0.041(4) -0.003(3) 0.016(3) 0.010(3)
C3 0.039(3) 0.059(4) 0.048(4) 0.009(3) -0.007(3) 0.005(3)
C4 0.046(3) 0.079(5) 0.039(3) 0.010(3) -0.012(3) 0.014(3)
Fe1 0.0244(5) 0.0481(6) 0.0276(5) -0.0007(5) 0.0031(4) 0.0086(5)
Fe2 0.0231(4) 0.0463(5) 0.0258(6) 0.0018(4) 0.0026(4) 0.0101(5)
N1 0.044(3) 0.058(3) 0.041(3) -0.004(2) 0.014(2) 0.009(3)
N2 0.038(2) 0.068(4) 0.038(3) 0.002(3) 0.012(2) 0.010(2)
N3 0.037(3) 0.062(4) 0.040(3) 0.002(2) -0.005(2) 0.008(3)
N4 0.046(3) 0.080(4) 0.046(3) 0.014(3) -0.005(3) 0.018(3)
N5 0.037(3) 0.053(3) 0.040(3) 0.007(2) 0.005(2) 0.000(2)
N6 0.057(4) 0.056(3) 0.052(4) 0.006(3) 0.000(3) 0.002(3)
C5 0.059(4) 0.057(4) 0.038(4) 0.000(3) -0.008(3) 0.008(3)
C6 0.057(4) 0.067(4) 0.042(4) 0.005(3) 0.000(3) -0.011(3)
C7 0.073(5) 0.070(5) 0.039(4) 0.019(3) 0.001(4) -0.005(4)
C8 0.044(4) 0.062(5) 0.062(5) 0.010(4) 0.003(3) -0.004(3)
C9 0.082(6) 0.071(5) 0.073(6) -0.006(5) 0.003(5) -0.014(5)
N7A 0.017(5) 0.035(7) 0.084(11) 0.001(6) 0.019(6) 0.002(5)
C11A 0.046(7) 0.037(7) 0.061(9) 0.003(6) 0.000(6) -0.002(5)
C12A 0.038(8) 0.059(10) 0.097(15) -0.019(10) 0.010(8) 0.005(7)
C13A 0.053(10) 0.049(10) 0.082(14) -0.024(9) -0.007(9) 0.013(8)
N8A 0.045(7) 0.038(6) 0.124(14) 0.002(7) -0.005(8) -0.013(5)
C10A 0.071(11) 0.062(8) 0.068(11) -0.005(8) -0.021(9) -0.016(9)
O2A 0.053(6) 0.045(7) 0.170(16) -0.002(8) 0.012(8) -0.014(5)
C14A 0.090(15) 0.037(8) 0.17(3) -0.012(12) -0.018(17) -0.003(9)
C51A 0.11(2) 0.119(19) 0.23(6) 0.000 -0.12(4) 0.000
C52A 0.062(9) 0.112(10) 0.053(11) 0.001(12) 0.002(10) 0.003(9)
C53A 0.085(15) 0.086(15) 0.11(3) 0.000 0.02(2) 0.000
N51A 0.095(12) 0.099(10) 0.090(16) -0.002(14) -0.016(14) 0.018(9)
O51A 0.081(10) 0.071(9) 0.144(19) 0.017(12) -0.006(12) -0.018(8)
C54A 0.21(4) 0.10(3) 0.16(4) 0.04(2) 0.04(3) 0.10(3)
N7B 0.059(10) 0.056(9) 0.078(12) -0.003(7) 0.011(8) 0.002(7)
C11B 0.115(16) 0.101(15) 0.047(10) 0.000(10) 0.034(10) -0.001(14)
C12B 0.14(3) 0.12(2) 0.11(2) -0.055(17) 0.08(2) -0.10(2)
C13B 0.122(19) 0.072(13) 0.13(2) -0.003(13) 0.016(17) -0.045(13)
N8B 0.102(12) 0.078(10) 0.074(10) -0.029(8) 0.005(9) -0.028(9)
C10B 0.063(9) 0.095(12) 0.052(9) -0.021(9) -0.004(7) -0.009(9)
O2B 0.27(3) 0.128(16) 0.18(2) -0.040(15) 0.06(2) -0.131(19)
C14B 0.109(18) 0.067(15) 0.18(4) -0.043(19) 0.01(2) -0.028(15)
O1 0.075(4) 0.065(4) 0.077(4) 0.021(3) -0.003(3) -0.018(3)
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'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 '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'
O O 0.0106 0.0060 '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
_geom_angle_publ_flag
C2 Ag1 C1 179.5(3) . . ?
C2 Ag1 Ag2 71.2(2) . 8_657 ?
C1 Ag1 Ag2 108.8(2) . 8_657 ?
C3 Ag2 C4 177.9(3) . . ?
C3 Ag2 Ag1 95.8(2) . 8_647 ?
C4 Ag2 Ag1 83.1(2) . 8_647 ?
N1 C1 Ag1 174.9(7) . . ?
N2 C2 Ag1 176.8(7) . . ?
N3 C3 Ag2 175.1(7) . . ?
N4 C4 Ag2 173.6(8) . . ?
N1 Fe1 N1 180.0 7_656 . ?
N1 Fe1 N3 90.8(2) 7_656 . ?
N1 Fe1 N3 89.2(2) . . ?
N1 Fe1 N3 89.2(2) 7_656 7_656 ?
N1 Fe1 N3 90.8(2) . 7_656 ?
N3 Fe1 N3 180.0 . 7_656 ?
N1 Fe1 N5 91.7(2) 7_656 7_656 ?
N1 Fe1 N5 88.3(2) . 7_656 ?
N3 Fe1 N5 88.6(2) . 7_656 ?
N3 Fe1 N5 91.4(2) 7_656 7_656 ?
N1 Fe1 N5 88.3(2) 7_656 . ?
N1 Fe1 N5 91.7(2) . . ?
N3 Fe1 N5 91.4(2) . . ?
N3 Fe1 N5 88.6(2) 7_656 . ?
N5 Fe1 N5 180.0 7_656 . ?
N2 Fe2 N2 180.0 . 5_667 ?
N2 Fe2 N4 87.6(2) . 7_657 ?
N2 Fe2 N4 92.4(2) 5_667 7_657 ?
N2 Fe2 N4 92.4(2) . 3_455 ?
N2 Fe2 N4 87.6(2) 5_667 3_455 ?
N4 Fe2 N4 180.0 7_657 3_455 ?
N2 Fe2 N7A 87.8(3) . 5_667 ?
N2 Fe2 N7A 92.2(3) 5_667 5_667 ?
N4 Fe2 N7A 94.1(3) 7_657 5_667 ?
N4 Fe2 N7A 85.9(3) 3_455 5_667 ?
N2 Fe2 N7A 92.2(3) . . ?
N2 Fe2 N7A 87.8(3) 5_667 . ?
N4 Fe2 N7A 85.9(3) 7_657 . ?
N4 Fe2 N7A 94.1(3) 3_455 . ?
N7A Fe2 N7A 180.0 5_667 . ?
N2 Fe2 N7B 92.2(4) . 5_667 ?
N2 Fe2 N7B 87.8(4) 5_667 5_667 ?
N4 Fe2 N7B 83.7(4) 7_657 5_667 ?
N4 Fe2 N7B 96.3(4) 3_455 5_667 ?
N7A Fe2 N7B 11.5(5) 5_667 5_667 ?
N7A Fe2 N7B 168.5(5) . 5_667 ?
N2 Fe2 N7B 87.8(4) . . ?
N2 Fe2 N7B 92.2(4) 5_667 . ?
N4 Fe2 N7B 96.3(4) 7_657 . ?
N4 Fe2 N7B 83.7(4) 3_455 . ?
N7B Fe2 N7B 180.0 5_667 . ?
C1 N1 Fe1 173.2(6) . . ?
C2 N2 Fe2 178.0(6) . . ?
C3 N3 Fe1 175.3(6) . . ?
C4 N4 Fe2 171.0(6) . 3_545 ?
C5 N5 C6 115.9(7) . . ?
C5 N5 Fe1 121.5(5) . . ?
C6 N5 Fe1 122.6(5) . . ?
C8 N6 C5 116.3(7) . . ?
N5 C5 N6 126.6(7) . . ?
N5 C5 H5 116.7 . . ?
N6 C5 H5 116.7 . . ?
C7 C6 N5 121.4(7) . . ?
C7 C6 H6 119.3 . . ?
N5 C6 H6 119.3 . . ?
C6 C7 C8 118.2(7) . . ?
C6 C7 H7 120.9 . . ?
C8 C7 H7 120.9 . . ?
N6 C8 O1 119.5(8) . . ?
N6 C8 C7 121.6(7) . . ?
O1 C8 C7 118.9(7) . . ?
O1 C9 H9A 109.5 . . ?
O1 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
O1 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C11A N7A C10A 120.0 . . ?
C11A N7A Fe2 121.8(4) . . ?
C10A N7A Fe2 117.9(4) . . ?
N7A C11A C12A 120.0 . . ?
N7A C11A H11A 120.0 . . ?
C12A C11A H11A 120.0 . . ?
C13A C12A C11A 120.0 . . ?
C13A C12A H12A 120.0 . . ?
C11A C12A H12A 120.0 . . ?
O2A C13A C12A 119.6(8) . . ?
O2A C13A N8A 120.4(8) . . ?
C12A C13A N8A 120.0 . . ?
C10A N8A C13A 120.0 . . ?
N8A C10A N7A 120.0 . . ?
N8A C10A H10A 120.0 . . ?
N7A C10A H10A 120.0 . . ?
C13A O2A C14A 118.9(13) . . ?
O2A C14A H14A 109.5 . . ?
O2A C14A H14B 109.5 . . ?
H14A C14A H14B 109.5 . . ?
O2A C14A H14C 109.5 . . ?
H14A C14A H14C 109.5 . . ?
H14B C14A H14C 109.5 . . ?
N51A C51A N51A 125(3) 6_657 . ?
N51A C51A H51A 117.3 6_657 . ?
N51A C51A H51A 117.3 . . ?
O51A C52A N51A 116.9(15) . . ?
O51A C52A C53A 117.4(16) . . ?
N51A C52A C53A 125.5(18) . . ?
C52A C53A C52A 114(2) 6_657 . ?
C52A C53A H53A 123.2 6_657 . ?
C52A C53A H53A 123.2 . . ?
C52A N51A C51A 114.7(19) . . ?
C52A O51A C54A 110(2) . . ?
O51A C54A H54A 109.5 . . ?
O51A C54A H54B 109.5 . . ?
H54A C54A H54B 109.5 . . ?
O51A C54A H54C 109.5 . . ?
H54A C54A H54C 109.5 . . ?
H54B C54A H54C 109.5 . . ?
C11B N7B C10B 120.0 . . ?
C11B N7B Fe2 122.3(6) . . ?
C10B N7B Fe2 117.7(6) . . ?
N7B C11B C12B 120.0 . . ?
N7B C11B H11B 120.0 . . ?
C12B C11B H11B 120.0 . . ?
C11B C12B C13B 120.0 . . ?
C11B C12B H12B 120.0 . . ?
C13B C12B H12B 120.0 . . ?
O2B C13B N8B 115.5(14) . . ?
O2B C13B C12B 124.4(14) . . ?
N8B C13B C12B 120.0 . . ?
C13B N8B C10B 120.0 . . ?
N8B C10B N7B 120.0 . . ?
N8B C10B H10B 120.0 . . ?
N7B C10B H10B 120.0 . . ?
C13B O2B C14B 123.5(18) . . ?
O2B C14B H14D 109.5 . . ?
O2B C14B H14E 109.5 . . ?
H14D C14B H14E 109.5 . . ?
O2B C14B H14F 109.5 . . ?
H14D C14B H14F 109.5 . . ?
H14E C14B H14F 109.5 . . ?
C8 O1 C9 119.1(7) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ag1 C2 2.044(6) . ?
Ag1 C1 2.050(6) . ?
Ag1 Ag2 3.1569(11) 8_657 ?
Ag2 C3 2.064(6) . ?
Ag2 C4 2.076(7) . ?
C1 N1 1.128(8) . ?
C2 N2 1.144(8) . ?
C3 N3 1.143(8) . ?
C4 N4 1.123(9) . ?
Fe1 N1 2.147(5) 7_656 ?
Fe1 N1 2.147(5) . ?
Fe1 N3 2.151(5) . ?
Fe1 N3 2.151(5) 7_656 ?
Fe1 N5 2.237(6) 7_656 ?
Fe1 N5 2.237(6) . ?
Fe2 N2 2.122(5) . ?
Fe2 N2 2.122(5) 5_667 ?
Fe2 N4 2.144(6) 7_657 ?
Fe2 N4 2.144(6) 3_455 ?
Fe2 N7A 2.199(6) 5_667 ?
Fe2 N7A 2.199(6) . ?
Fe2 N7B 2.210(8) 5_667 ?
Fe2 N7B 2.210(8) . ?
N5 C5 1.311(9) . ?
N5 C6 1.355(9) . ?
N6 C8 1.301(10) . ?
N6 C5 1.350(10) . ?
C5 H5 0.9300 . ?
C6 C7 1.345(11) . ?
C6 H6 0.9300 . ?
C7 C8 1.394(11) . ?
C7 H7 0.9300 . ?
C8 O1 1.337(10) . ?
C9 O1 1.404(11) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
N7A C11A 1.3900 . ?
N7A C10A 1.3900 . ?
C11A C12A 1.3900 . ?
C11A H11A 0.9300 . ?
C12A C13A 1.3900 . ?
C12A H12A 0.9300 . ?
C13A O2A 1.276(10) . ?
C13A N8A 1.3900 . ?
N8A C10A 1.3900 . ?
C10A H10A 0.9300 . ?
O2A C14A 1.47(2) . ?
C14A H14A 0.9600 . ?
C14A H14B 0.9600 . ?
C14A H14C 0.9600 . ?
C51A N51A 1.391(16) 6_657 ?
C51A N51A 1.391(16) . ?
C51A H51A 0.9300 . ?
C52A O51A 1.29(2) . ?
C52A N51A 1.332(16) . ?
C52A C53A 1.408(15) . ?
C53A H53A 0.9300 . ?
O51A C54A 1.544(19) . ?
C54A H54A 0.9600 . ?
C54A H54B 0.9600 . ?
C54A H54C 0.9600 . ?
N7B C11B 1.3900 . ?
N7B C10B 1.3900 . ?
C11B C12B 1.3900 . ?
C11B H11B 0.9300 . ?
C12B C13B 1.3900 . ?
C12B H12B 0.9300 . ?
C13B O2B 1.295(14) . ?
C13B N8B 1.3900 . ?
N8B C10B 1.3900 . ?
C10B H10B 0.9300 . ?
O2B C14B 1.553(19) . ?
C14B H14D 0.9600 . ?
C14B H14E 0.9600 . ?
C14B H14F 0.9600 . ?