# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
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data_PPNFeAu3_120K
_database_code_depnum_ccdc_archive 'CCDC 1977203'
loop_
_audit_author_name
_audit_author_address
'Zhao-Ping Ni'
;Key Laboratory of Bioinorganic and Synthetic Chemistry of Ministry of Education, School of Chemistry
China
;
_audit_update_record             
;
2020-01-11 deposited with the CCDC.	2020-03-13 downloaded from the CCDC.
;
_audit_creation_date             2019-08-03
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.17(Au18 C36 Fe6 N36), C36 H30 N1 P2'
_chemical_formula_sum            'C42 H30 Au3 Fe N7 P2'
_chemical_formula_weight         1341.42
_chemical_melting_point          ?
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'
Au Au -2.0133 8.8022 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c'
_space_group_name_Hall           '-R 3 2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'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'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'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'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-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'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-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'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   14.9822(5)
_cell_length_b                   14.9822(5)
_cell_length_c                   31.1973(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     6064.6(4)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    9884
_cell_measurement_temperature    120
_cell_measurement_theta_max      27.56
_cell_measurement_theta_min      2.72
_shelx_estimated_absorpt_T_max   0.545
_shelx_estimated_absorpt_T_min   0.446
_exptl_absorpt_coefficient_mu    11.323
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5816
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0787 before and 0.0538 after correction. The Ratio of minimum to maximum transmission is 0.7800. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.204
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             3744
_exptl_crystal_size_max          0.085
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.061
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_unetI/netI     0.0116
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            56341
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.556
_diffrn_reflns_theta_min         2.042
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1510
_reflns_number_total             1566
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         1.473
_refine_diff_density_min         -4.611
_refine_diff_density_rms         0.171
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     83
_refine_ls_number_reflns         1566
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.0205
_refine_ls_R_factor_gt           0.0193
_refine_ls_restrained_S_all      1.194
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0253P)²+47.6187P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0450
_refine_ls_wR_factor_ref         0.0457
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
P1 \\sim C2 \\sim N2: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C6) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C3) \\sim
Ueq, Uanis(C2) \\sim Ueq, Uanis(C7) \\sim Ueq: with sigma of 0.005 and sigma
for terminal atoms of 0.01
Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim
Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq: with sigma of 0.003 and sigma
for terminal atoms of 0.005
Uanis(N2) = Uanis(P1)
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7), C6(H6), C5(H5)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Au1 Au 0.18797(2) 0.333333 0.583333 0.01361(7) Uani 1 2 d S T P . .
Fe1 Fe 0.333333 0.666667 0.666667 0.00647(17) Uani 1 6 d S T P . .
P1 P 0.333333 0.666667 0.46645(4) 0.0192(3) Uani 1 3 d S TU P . .
N1 N 0.28524(17) 0.54437(18) 0.63150(7) 0.0110(4) Uani 1 1 d . . . . .
C1 C 0.2528(2) 0.4683(2) 0.61330(9) 0.0137(5) Uani 1 1 d . . . . .
C2 C 0.2184(3) 0.5588(3) 0.48724(10) 0.0223(6) Uani 1 1 d . U . . .
C3 C 0.1824(3) 0.4627(3) 0.46787(13) 0.0379(9) Uani 1 1 d . U . . .
H3 H 0.218392 0.455852 0.444174 0.045 Uiso 1 1 calc R . . . .
C4 C 0.0949(4) 0.3779(3) 0.48315(16) 0.0485(11) Uani 1 1 d . U . . .
H4 H 0.070859 0.312491 0.470151 0.058 Uiso 1 1 calc R . . . .
C7 C 0.1665(3) 0.5684(3) 0.52222(13) 0.0322(8) Uani 1 1 d . U . . .
H7 H 0.191567 0.633366 0.535847 0.039 Uiso 1 1 calc R . . . .
C6 C 0.0774(4) 0.4823(4) 0.53723(17) 0.0465(10) Uani 1 1 d . U . . .
H6 H 0.040768 0.487762 0.560992 0.056 Uiso 1 1 calc R . . . .
C5 C 0.0428(4) 0.3876(4) 0.51671(16) 0.0492(11) Uani 1 1 d . U . . .
H5 H -0.018400 0.328800 0.526487 0.059 Uiso 1 1 calc R . . . .
N2 N 0.333333 0.666667 0.416667 0.0192(3) Uani 1 6 d S TU P . .

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
Au1 0.01485(8) 0.00935(9) 0.01480(10) -0.00519(5) -0.00260(3) 0.00467(4)
Fe1 0.0062(2) 0.0062(2) 0.0070(4) 0.000 0.000 0.00309(12)
P1 0.0230(4) 0.0230(4) 0.0115(6) 0.000 0.000 0.0115(2)
N1 0.0091(10) 0.0118(11) 0.0118(10) 0.0006(9) 0.0002(8) 0.0050(9)
C1 0.0138(13) 0.0121(13) 0.0147(12) -0.0019(10) -0.0009(10) 0.0060(11)
C2 0.0211(14) 0.0212(14) 0.0230(13) 0.0021(11) -0.0067(11) 0.0095(11)
C3 0.0452(19) 0.0281(16) 0.0336(16) -0.0002(14) -0.0112(15) 0.0132(14)
C4 0.051(2) 0.0307(18) 0.051(2) 0.0037(16) -0.0214(18) 0.0110(16)
C7 0.0274(16) 0.0316(16) 0.0394(17) 0.0081(14) 0.0057(14) 0.0159(13)
C6 0.0347(18) 0.048(2) 0.059(2) 0.0176(17) 0.0102(16) 0.0221(16)
C5 0.0333(18) 0.0399(19) 0.064(2) 0.0205(17) -0.0114(17) 0.0103(15)
N2 0.0230(4) 0.0230(4) 0.0115(6) 0.000 0.000 0.0115(2)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Au1 C1 1.986(3) 17 ?
Au1 C1 1.986(3) . ?
Fe1 N1 1.939(2) 25_566 ?
Fe1 N1 1.939(2) 3_565 ?
Fe1 N1 1.939(2) 26_456 ?
Fe1 N1 1.939(2) 27_556 ?
Fe1 N1 1.939(2) . ?
Fe1 N1 1.939(2) 2_665 ?
P1 C2 1.793(3) . ?
P1 C2 1.794(3) 3_565 ?
P1 C2 1.794(3) 2_665 ?
P1 N2 1.5531(13) . ?
N1 C1 1.141(4) . ?
C2 C3 1.397(5) . ?
C2 C7 1.389(5) . ?
C3 C4 1.376(6) . ?
C4 C5 1.356(7) . ?
C7 C6 1.395(6) . ?
C6 C5 1.398(7) . ?

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
C1 Au1 C1 177.69(16) 17 . ?
N1 Fe1 N1 91.13(9) 25_566 27_556 ?
N1 Fe1 N1 180.0 3_565 27_556 ?
N1 Fe1 N1 180.0 26_456 2_665 ?
N1 Fe1 N1 91.13(9) 26_456 27_556 ?
N1 Fe1 N1 91.13(10) 3_565 . ?
N1 Fe1 N1 88.87(9) 27_556 2_665 ?
N1 Fe1 N1 91.12(9) 25_566 26_456 ?
N1 Fe1 N1 88.87(10) 26_456 . ?
N1 Fe1 N1 180.00(15) 25_566 . ?
N1 Fe1 N1 88.87(9) 27_556 . ?
N1 Fe1 N1 88.87(9) 25_566 3_565 ?
N1 Fe1 N1 88.87(10) 25_566 2_665 ?
N1 Fe1 N1 91.13(9) 2_665 . ?
N1 Fe1 N1 88.87(9) 26_456 3_565 ?
N1 Fe1 N1 91.13(9) 3_565 2_665 ?
C2 P1 C2 107.69(11) . 2_665 ?
C2 P1 C2 107.69(11) 3_565 . ?
C2 P1 C2 107.69(11) 3_565 2_665 ?
N2 P1 C2 111.20(11) . . ?
N2 P1 C2 111.20(11) . 2_665 ?
N2 P1 C2 111.20(11) . 3_565 ?
C1 N1 Fe1 175.0(2) . . ?
N1 C1 Au1 176.5(3) . . ?
C3 C2 P1 118.3(3) . . ?
C7 C2 P1 121.7(3) . . ?
C7 C2 C3 120.0(4) . . ?
C4 C3 C2 119.9(4) . . ?
C5 C4 C3 120.2(5) . . ?
C2 C7 C6 119.6(4) . . ?
C7 C6 C5 118.9(5) . . ?
C4 C5 C6 121.4(4) . . ?
P1 N2 P1 180.0 . 10_455 ?

_iucr_refine_instructions_details 
;
TITL A_a.res in R-3c
    ppnfeau3_120k.res
    created by SHELXL-2018/1 at 11:49:35 on 03-Aug-2019
REM Old TITL A in R-3c
REM SHELXT solution in R-3c
REM R1 0.082, Rweak 0.003, Alpha 0.027, Orientation as input
REM Formula found by SHELXT: C37 N12 P2 Fe Au3
CELL 0.71073 14.9822 14.9822 31.1973 90 90 120
ZERR 6 0.0005 0.0005 0.001 0 0 0
LATT 3
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SYMM +Y,+X,0.5-Z
SYMM -Y+X,-Y,0.5-Z
SYMM -X,-X+Y,0.5-Z
SFAC C H Au Fe N P
UNIT 252 180 18 6 42 12
SIMU 0.01 0.02 1.7 P1 C2 N2
ISOR 0.005 0.01 C6 C5 C4 C3 C2 C7
ISOR 0.003 0.005 C6 C7 C2 C3 C4 C5
EADP N2 P1

L.S. 10
PLAN  20
SIZE 0.061 0.075 0.085
TEMP -153.15
LIST 6
fmap 2
acta
OMIT 0 2 4
REM <olex2.extras>
REM <HklSrc "%.\\PPNFeAu3_120K.hkl">
REM </olex2.extras>

WGHT    0.025300   47.618698
FVAR       0.02515
AU1   3    0.187975    0.333333    0.583333    10.50000    0.01485    0.00935 =
         0.01480   -0.00519   -0.00260    0.00467
FE1   4    0.333333    0.666667    0.666667    10.16667    0.00619    0.00619 =
         0.00704    0.00000    0.00000    0.00309
P1    6    0.333333    0.666667    0.466449    10.33333    0.02298    0.02298 =
         0.01152    0.00000    0.00000    0.01149
N1    5    0.285242    0.544374    0.631496    11.00000    0.00912    0.01176 =
         0.01182    0.00056    0.00020    0.00496
C1    1    0.252791    0.468326    0.613296    11.00000    0.01378    0.01205 =
         0.01470   -0.00189   -0.00085    0.00601
C2    1    0.218359    0.558763    0.487237    11.00000    0.02112    0.02122 =
         0.02299    0.00206   -0.00672    0.00951
C3    1    0.182428    0.462683    0.467871    11.00000    0.04517    0.02806 =
         0.03365   -0.00025   -0.01118    0.01321
AFIX  43
H3    2    0.218392    0.455852    0.444174    11.00000   -1.20000
AFIX   0
C4    1    0.094877    0.377931    0.483154    11.00000    0.05132    0.03071 =
         0.05062    0.00372   -0.02144    0.01096
AFIX  43
H4    2    0.070859    0.312491    0.470151    11.00000   -1.20000
AFIX   0
C7    1    0.166499    0.568445    0.522223    11.00000    0.02738    0.03155 =
         0.03938    0.00810    0.00569    0.01595
AFIX  43
H7    2    0.191567    0.633366    0.535847    11.00000   -1.20000
AFIX   0
C6    1    0.077379    0.482250    0.537230    11.00000    0.03466    0.04778 =
         0.05913    0.01756    0.01022    0.02214
AFIX  43
H6    2    0.040768    0.487762    0.560992    11.00000   -1.20000
AFIX   0
C5    1    0.042836    0.387589    0.516708    11.00000    0.03332    0.03990 =
         0.06358    0.02050   -0.01141    0.01027
AFIX  43
H5    2   -0.018400    0.328800    0.526487    11.00000   -1.20000
AFIX   0
N2    5    0.333333    0.666667    0.416667    10.16667    0.02298    0.02298 =
         0.01152    0.00000    0.00000    0.01149
HKLF 4




REM  A_a.res in R-3c
REM R1 =  0.0193 for    1510 Fo > 4sig(Fo)  and  0.0205 for all    1566 data
REM     83 parameters refined using     42 restraints

END  
     
WGHT      0.0253     47.6171 

REM Highest difference peak  1.473,  deepest hole -4.611,  1-sigma level  0.171
Q1    1   0.3797  0.6667  0.4167  10.50000  0.05    1.47
Q2    1   0.0580  0.3793  0.4975  11.00000  0.05    0.92
Q3    1   0.0645  0.4608  0.5197  11.00000  0.05    0.84
Q4    1   0.0321  0.4018  0.5325  11.00000  0.05    0.79
Q5    1   0.0890  0.5093  0.5514  11.00000  0.05    0.63
Q6    1   0.2957  0.5768  0.6453  11.00000  0.05    0.47
Q7    1   0.1365  0.5435  0.5070  11.00000  0.05    0.44
Q8    1   0.0452  0.5233  0.4985  11.00000  0.05    0.43
Q9    1   0.1273  0.4460  0.4732  11.00000  0.05    0.41
Q10   1   0.0043  0.4662  0.5451  11.00000  0.05    0.40
Q11   1   0.3333  0.6667  0.7004  10.33333  0.05    0.38
Q12   1   0.3333  0.4997  0.4167  10.50000  0.05    0.37
Q13   1  -0.0446  0.4851  0.5324  11.00000  0.05    0.36
Q14   1   0.0814  0.5387  0.5201  11.00000  0.05    0.34
Q15   1   0.0321  0.5368  0.5351  11.00000  0.05    0.34
Q16   1   0.1860  0.5599  0.4992  11.00000  0.05    0.34
Q17   1   0.0554  0.4616  0.4681  11.00000  0.05    0.33
Q18   1  -0.0001  0.4616  0.5229  11.00000  0.05    0.33
Q19   1   0.0962  0.5005  0.4873  11.00000  0.05    0.32
Q20   1   0.0843  0.5776  0.4881  11.00000  0.05    0.32

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0193 for 1510 Fo > 4sig(Fo) and 0.0205 for all 59980 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 1.47, deepest hole -4.61
  REM Mean Shift 0, Max Shift 0.003.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0205
  REM R1_gt = 0.0193
  REM wR_ref = 0.0457
  REM GOOF = 1.082
  REM Shift_max = 0.003
  REM Shift_mean = 0
  REM Reflections_all = 59980
  REM Reflections_gt = 1510
  REM Parameters = n/a
  REM Hole = -4.61
  REM Peak = 1.47
  REM Flack = n/a

  
;
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_PPNFeAu3_191K
_database_code_depnum_ccdc_archive 'CCDC 1977205'
loop_
_audit_author_name
_audit_author_address
'Zhao-Ping Ni'
;Key Laboratory of Bioinorganic and Synthetic Chemistry of Ministry of Education, School of Chemistry
China
;
_audit_update_record             
;
2020-01-11 deposited with the CCDC.	2020-03-13 downloaded from the CCDC.
;
_audit_creation_date             2019-08-03
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.17(Au18 C36 Fe6 N36), C36 H30 N1 P2'
_chemical_formula_sum            'C42 H30 Au3 Fe N7 P2'
_chemical_formula_weight         1341.42
_chemical_melting_point          ?
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'
Au Au -2.0133 8.8022 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c'
_space_group_name_Hall           '-R 3 2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'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'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'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'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-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'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-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'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   15.2390(9)
_cell_length_b                   15.2390(9)
_cell_length_c                   31.3855(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     6312.1(8)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    9881
_cell_measurement_temperature    191(2)
_cell_measurement_theta_max      27.36
_cell_measurement_theta_min      3.02
_shelx_estimated_absorpt_T_max   0.428
_shelx_estimated_absorpt_T_min   0.273
_exptl_absorpt_coefficient_mu    10.879
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4027
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1248 before and 0.0716 after correction. The Ratio of minimum to maximum transmission is 0.5400. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    2.117
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             3744
_exptl_crystal_size_max          0.161
_exptl_crystal_size_mid          0.144
_exptl_crystal_size_min          0.094
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0842
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            49891
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.840
_diffrn_reflns_theta_min         2.016
_diffrn_ambient_temperature      191(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1573
_reflns_number_total             1825
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         1.189
_refine_diff_density_min         -4.123
_refine_diff_density_rms         0.249
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.230
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     71
_refine_ls_number_reflns         1825
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0430
_refine_ls_restrained_S_all      1.230
_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)+(0.0292P)²+198.9260P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0992
_refine_ls_wR_factor_ref         0.1031
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(P1) = Uanis(N2)
3.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C6(H6), C5(H5), C4(H4), C3(H3)
3.b Fitted hexagon refined as free rotating group:
 C2(C7,C6,C5,C4,C3)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Au1 Au 0.333333 0.13933(3) 0.416667 0.03086(14) Uani 1 2 d S T P . .
Fe1 Fe 0.666667 0.333333 0.333333 0.0160(4) Uani 1 6 d S T P . .
P1 P 0.666667 0.333333 0.53388(10) 0.0308(7) Uani 1 3 d S T P . .
N1 N 0.5422(5) 0.2521(5) 0.3699(2) 0.0318(13) Uani 1 1 d . . . . .
N2 N 0.666667 0.333333 0.583333 0.0308(7) Uani 1 6 d S T P . .
C1 C 0.4677(6) 0.2091(6) 0.3874(2) 0.0321(16) Uani 1 1 d . . . . .
C2 C 0.5593(4) 0.3372(5) 0.51339(18) 0.0361(17) Uani 1 1 d . . . . .
C7 C 0.5672(4) 0.3990(5) 0.4793(2) 0.053(2) Uani 1 1 d G . . . .
H7 H 0.631000 0.440585 0.466121 0.063 Uiso 1 1 calc R . . . .
C6 C 0.4817(6) 0.4000(6) 0.4646(2) 0.085(4) Uani 1 1 d G . . . .
H6 H 0.487053 0.442223 0.441272 0.103 Uiso 1 1 calc R . . . .
C5 C 0.3883(5) 0.3392(7) 0.4839(3) 0.089(5) Uani 1 1 d G . . . .
H5 H 0.329877 0.339824 0.473783 0.107 Uiso 1 1 calc R . . . .
C4 C 0.3805(4) 0.2774(6) 0.5179(3) 0.085(5) Uani 1 1 d G . . . .
H4 H 0.316648 0.235788 0.531143 0.102 Uiso 1 1 calc R . . . .
C3 C 0.4660(5) 0.2764(5) 0.53271(19) 0.063(3) Uani 1 1 d G . . . .
H3 H 0.460595 0.234149 0.555993 0.076 Uiso 1 1 calc R . . . .

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
Au1 0.0300(2) 0.03174(19) 0.0303(2) 0.00229(8) 0.00458(15) 0.01498(11)
Fe1 0.0147(6) 0.0147(6) 0.0186(9) 0.000 0.000 0.0073(3)
P1 0.0370(11) 0.0370(11) 0.0184(14) 0.000 0.000 0.0185(5)
N1 0.027(3) 0.036(3) 0.032(3) -0.007(3) -0.001(2) 0.016(3)
N2 0.0370(11) 0.0370(11) 0.0184(14) 0.000 0.000 0.0185(5)
C1 0.033(4) 0.035(4) 0.032(4) 0.000(3) -0.001(3) 0.020(3)
C2 0.035(4) 0.040(4) 0.034(4) -0.014(3) 0.000(3) 0.019(4)
C7 0.044(5) 0.048(5) 0.070(6) 0.001(5) -0.013(5) 0.027(5)
C6 0.077(9) 0.059(7) 0.135(12) -0.013(8) -0.045(9) 0.045(7)
C5 0.056(7) 0.097(10) 0.138(13) -0.066(10) -0.050(8) 0.055(8)
C4 0.034(5) 0.114(12) 0.098(10) -0.046(9) -0.006(6) 0.031(7)
C3 0.044(5) 0.082(8) 0.054(6) -0.012(5) 0.004(4) 0.023(6)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Au1 C1 1.997(8) 12 ?
Au1 C1 1.997(8) . ?
Fe1 N1 2.025(6) . ?
Fe1 N1 2.025(6) 32 ?
Fe1 N1 2.025(6) 31_655 ?
Fe1 N1 2.025(6) 2_655 ?
Fe1 N1 2.025(6) 3_665 ?
Fe1 N1 2.025(6) 33_545 ?
P1 N2 1.552(3) . ?
P1 C2 1.786(4) 2_655 ?
P1 C2 1.786(5) 3_665 ?
P1 C2 1.786(5) . ?
N1 C1 1.130(10) . ?
C2 C7 1.3900 . ?
C2 C3 1.3900 . ?
C7 C6 1.3900 . ?
C6 C5 1.3900 . ?
C5 C4 1.3900 . ?
C4 C3 1.3900 . ?

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
C1 Au1 C1 177.7(4) 12 . ?
N1 Fe1 N1 91.1(2) 33_545 32 ?
N1 Fe1 N1 180.0 2_655 32 ?
N1 Fe1 N1 91.1(2) 2_655 . ?
N1 Fe1 N1 91.1(2) 31_655 32 ?
N1 Fe1 N1 91.1(2) 2_655 3_665 ?
N1 Fe1 N1 180.0(3) 31_655 . ?
N1 Fe1 N1 91.1(2) 33_545 31_655 ?
N1 Fe1 N1 88.9(2) 31_655 3_665 ?
N1 Fe1 N1 180.0 33_545 3_665 ?
N1 Fe1 N1 88.9(2) 32 3_665 ?
N1 Fe1 N1 88.9(2) 33_545 2_655 ?
N1 Fe1 N1 88.9(2) 33_545 . ?
N1 Fe1 N1 91.1(2) . 3_665 ?
N1 Fe1 N1 88.9(2) 31_655 2_655 ?
N1 Fe1 N1 88.9(2) 32 . ?
N2 P1 C2 111.1(2) . . ?
N2 P1 C2 111.1(2) . 2_655 ?
N2 P1 C2 111.1(2) . 3_665 ?
C2 P1 C2 107.8(2) 2_655 . ?
C2 P1 C2 107.8(2) 2_655 3_665 ?
C2 P1 C2 107.8(2) 3_665 . ?
C1 N1 Fe1 173.2(6) . . ?
P1 N2 P1 180.0 . 16_545 ?
N1 C1 Au1 176.2(7) . . ?
C7 C2 P1 122.0(4) . . ?
C7 C2 C3 120.0 . . ?
C3 C2 P1 118.0(4) . . ?
C6 C7 C2 120.0 . . ?
C7 C6 C5 120.0 . . ?
C4 C5 C6 120.0 . . ?
C5 C4 C3 120.0 . . ?
C4 C3 C2 120.0 . . ?

_iucr_refine_instructions_details 
;
TITL B in R-3c
    b.res
    created by SHELXL-2018/1 at 14:47:26 on 03-Aug-2019
CELL 0.71073 15.23899 15.23899 31.38555 90 90 120
ZERR 6 0.00085 0.00085 0.00145 0 0 0
LATT 3
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SYMM +Y,+X,0.5-Z
SYMM -Y+X,-Y,0.5-Z
SYMM -X,-X+Y,0.5-Z
SFAC C H Au Fe N P
UNIT 252 180 18 6 42 12
EADP P1 N2

L.S. 4 0 0
PLAN  20
SIZE 0.094 0.144 0.161
TEMP -81.82
fmap 2 53
acta
REM <olex2.extras>
REM <HklSrc "%.\\B.hkl">
REM </olex2.extras>

WGHT    0.029200  198.925995
FVAR       0.02403
AU1   3    0.333333    0.139331    0.416667    10.50000    0.02996    0.03174 =
         0.03027    0.00229    0.00458    0.01498
FE1   4    0.666667    0.333333    0.333333    10.16667    0.01469    0.01469 =
         0.01859    0.00000    0.00000    0.00734
P1    6    0.666667    0.333333    0.533885    10.33333    0.03703    0.03703 =
         0.01842    0.00000    0.00000    0.01852
N1    5    0.542159    0.252132    0.369881    11.00000    0.02700    0.03649 =
         0.03199   -0.00659   -0.00115    0.01596
N2    5    0.666667    0.333333    0.583333    10.16667    0.03703    0.03703 =
         0.01842    0.00000    0.00000    0.01852
C1    1    0.467682    0.209138    0.387395    11.00000    0.03334    0.03509 =
         0.03153   -0.00038   -0.00126    0.01979
AFIX  66
C2    1    0.559333    0.337214    0.513393    11.00000    0.03458    0.04031 =
         0.03411   -0.01393   -0.00037    0.01933
C7    1    0.567190    0.399013    0.479320    11.00000    0.04421    0.04846 =
         0.07034    0.00081   -0.01325    0.02678
AFIX  43
H7    2    0.631000    0.440585    0.466121    11.00000   -1.20000
AFIX  65
C6    1    0.481682    0.399985    0.464560    11.00000    0.07661    0.05884 =
         0.13529   -0.01315   -0.04526    0.04467
AFIX  43
H6    2    0.487053    0.442223    0.441272    11.00000   -1.20000
AFIX  65
C5    1    0.388317    0.339159    0.483872    11.00000    0.05629    0.09692 =
         0.13762   -0.06625   -0.04981    0.05524
AFIX  43
H5    2    0.329877    0.339824    0.473783    11.00000   -1.20000
AFIX  65
C4    1    0.380459    0.277360    0.517945    11.00000    0.03448    0.11378 =
         0.09828   -0.04629   -0.00610    0.03103
AFIX  43
H4    2    0.316648    0.235788    0.531143    11.00000   -1.20000
AFIX  65
C3    1    0.465965    0.276386    0.532706    11.00000    0.04367    0.08167 =
         0.05362   -0.01198    0.00419    0.02279
AFIX  43
H3    2    0.460595    0.234149    0.555993    11.00000   -1.20000
AFIX   0
HKLF 4




REM  B in R-3c
REM R1 =  0.0430 for    1573 Fo > 4sig(Fo)  and  0.0548 for all    1825 data
REM     71 parameters refined using      0 restraints

END  
     
WGHT      0.0292    198.8716 

REM Highest difference peak  1.189,  deepest hole -4.123,  1-sigma level  0.249
Q1    1   0.6247  0.3790  0.5783  11.00000  0.05    1.19
Q2    1   0.5484  0.2150  0.5833  10.50000  0.05    0.73
Q3    1   0.3908  0.3939  0.5005  11.00000  0.05    0.65
Q4    1   0.4461  0.1922  0.4122  11.00000  0.05    0.64
Q5    1   0.3333  0.0515  0.4167  10.50000  0.05    0.64
Q6    1   0.5237  0.2389  0.5589  11.00000  0.05    0.60
Q7    1   0.4985  0.1652  0.5833  10.50000  0.05    0.58
Q8    1   0.2915  0.2489  0.4227  11.00000  0.05    0.58
Q9    1   0.4354  0.2975  0.5240  11.00000  0.05    0.57
Q10   1   0.5665  0.5182  0.4980  11.00000  0.05    0.56
Q11   1   0.5515  0.2911  0.5712  11.00000  0.05    0.56
Q12   1   0.7336  0.4696  0.4477  11.00000  0.05    0.55
Q13   1   0.4568  0.2273  0.6041  11.00000  0.05    0.55
Q14   1   0.3926  0.3230  0.5045  11.00000  0.05    0.54
Q15   1   0.5521  0.3241  0.4324  11.00000  0.05    0.53
Q16   1   0.4744  0.3045  0.5911  11.00000  0.05    0.53
Q17   1   0.4967  0.1994  0.5414  11.00000  0.05    0.52
Q18   1   0.6667  0.3333  0.4195  10.33333  0.05    0.52
Q19   1   0.5995  0.5245  0.4583  11.00000  0.05    0.51
Q20   1   0.4272  0.2508  0.4190  11.00000  0.05    0.50

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0430 for 1573 Fo > 4sig(Fo) and 0.0548 for all 53014 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 1.19, deepest hole -4.12
  REM Mean Shift 0, Max Shift 0.000.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0548
  REM R1_gt = 0.0430
  REM wR_ref = 0.1031
  REM GOOF = 1.230
  REM Shift_max = 0.000
  REM Shift_mean = 0
  REM Reflections_all = 53014
  REM Reflections_gt = 1573
  REM Parameters = n/a
  REM Hole = -4.12
  REM Peak = 1.19
  REM Flack = n/a

  
;
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_PPNFeAu3_162K
_database_code_depnum_ccdc_archive 'CCDC 1977204'
loop_
_audit_author_name
_audit_author_address
'Zhao-Ping Ni'
;Key Laboratory of Bioinorganic and Synthetic Chemistry of Ministry of Education, School of Chemistry
China
;
_audit_update_record             
;
2020-01-11 deposited with the CCDC.	2020-03-13 downloaded from the CCDC.
;
_audit_creation_date             2019-07-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.17(Au18 C36 Fe6 N36), C36 H30 N1 P2'
_chemical_formula_sum            'C42 H30 Au3 Fe N7 P2'
_chemical_formula_weight         1341.42
_chemical_melting_point          ?
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'
Au Au -2.0133 8.8022 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c'
_space_group_name_Hall           '-R 3 2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'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'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'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'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-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'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-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'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   15.0857(8)
_cell_length_b                   15.0857(8)
_cell_length_c                   31.2708(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     6163.2(7)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    9958
_cell_measurement_temperature    162(2)
_cell_measurement_theta_max      27.69
_cell_measurement_theta_min      3.04
_shelx_estimated_absorpt_T_max   0.421
_shelx_estimated_absorpt_T_min   0.267
_exptl_absorpt_coefficient_mu    11.142
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.3808
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1328 before and 0.0713 after correction. The Ratio of minimum to maximum transmission is 0.5107. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.169
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             3744
_exptl_crystal_size_max          0.161
_exptl_crystal_size_mid          0.144
_exptl_crystal_size_min          0.094
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0871
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            48041
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.317
_diffrn_reflns_theta_min         2.031
_diffrn_ambient_temperature      162(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1471
_reflns_number_total             1703
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         1.145
_refine_diff_density_min         -1.792
_refine_diff_density_rms         0.200
_refine_ls_extinction_coef       .
_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     85
_refine_ls_number_reflns         1703
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0250
_refine_ls_restrained_S_all      1.072
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0322P)²+23.1218P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0546
_refine_ls_wR_factor_ref         0.0591
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid bond restraints
 P1, N2
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(N2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C6(H6), C5(H5), C4(H4), C3(H3)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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
Au1 Au 0.333333 0.14267(2) 0.416667 0.02448(9) Uani 1 2 d S T P . .
Fe1 Fe 0.666667 0.333333 0.333333 0.0140(2) Uani 1 6 d S T P . .
N1 N 0.5431(2) 0.2559(2) 0.36899(10) 0.0232(6) Uani 1 1 d . . . . .
C1 C 0.4679(3) 0.2131(3) 0.38695(12) 0.0257(8) Uani 1 1 d . . . . .
P1 P 0.666667 0.333333 0.53375(5) 0.0251(3) Uani 1 3 d S TU P . .
N2 N 0.666667 0.333333 0.583333 0.051(2) Uani 1 6 d S TU P . .
C2 C 0.5591(3) 0.3392(3) 0.51316(12) 0.0310(9) Uani 1 1 d . . . . .
C7 C 0.5677(4) 0.4001(4) 0.47865(16) 0.0432(11) Uani 1 1 d . . . . .
H7 H 0.631889 0.440459 0.464963 0.052 Uiso 1 1 calc R . . . .
C6 C 0.4813(5) 0.4018(5) 0.4641(2) 0.0694(18) Uani 1 1 d . . . . .
H6 H 0.486362 0.443936 0.440590 0.083 Uiso 1 1 calc R . . . .
C5 C 0.3875(5) 0.3413(5) 0.4842(3) 0.075(2) Uani 1 1 d . . . . .
H5 H 0.328651 0.343055 0.474547 0.089 Uiso 1 1 calc R . . . .
C4 C 0.3794(4) 0.2798(6) 0.5175(2) 0.072(2) Uani 1 1 d . . . . .
H4 H 0.314740 0.237467 0.530548 0.086 Uiso 1 1 calc R . . . .
C3 C 0.4637(3) 0.2786(4) 0.53223(16) 0.0515(13) Uani 1 1 d . . . . .
H3 H 0.457510 0.236013 0.555754 0.062 Uiso 1 1 calc R . . . .

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
Au1 0.02415(12) 0.02579(11) 0.02295(12) 0.00183(4) 0.00367(7) 0.01207(6)
Fe1 0.0140(3) 0.0140(3) 0.0140(5) 0.000 0.000 0.00700(16)
N1 0.0233(16) 0.0261(16) 0.0229(15) -0.0035(12) -0.0012(12) 0.0143(13)
C1 0.031(2) 0.0274(19) 0.0246(18) -0.0027(14) -0.0031(15) 0.0191(17)
P1 0.0305(5) 0.0305(5) 0.0142(7) 0.000 0.000 0.0152(3)
N2 0.066(4) 0.066(4) 0.021(3) 0.000 0.000 0.0332(18)
C2 0.028(2) 0.034(2) 0.032(2) -0.0120(17) -0.0018(16) 0.0160(17)
C7 0.040(3) 0.037(2) 0.058(3) -0.002(2) -0.013(2) 0.024(2)
C6 0.071(4) 0.056(4) 0.098(5) -0.013(3) -0.040(4) 0.044(3)
C5 0.047(3) 0.078(4) 0.120(6) -0.057(4) -0.040(4) 0.048(3)
C4 0.033(3) 0.101(5) 0.079(4) -0.045(4) -0.005(3) 0.032(3)
C3 0.032(2) 0.067(3) 0.044(3) -0.013(2) 0.004(2) 0.016(2)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Au1 C1 1.990(4) 12 ?
Au1 C1 1.990(4) . ?
Fe1 N1 1.976(3) 33_545 ?
Fe1 N1 1.976(3) 3_665 ?
Fe1 N1 1.976(3) . ?
Fe1 N1 1.976(3) 2_655 ?
Fe1 N1 1.976(3) 32 ?
Fe1 N1 1.976(3) 31_655 ?
N1 C1 1.134(5) . ?
P1 N2 1.5504(15) . ?
P1 C2 1.789(4) 2_655 ?
P1 C2 1.789(4) . ?
P1 C2 1.789(4) 3_665 ?
C2 C7 1.380(6) . ?
C2 C3 1.395(6) . ?
C7 C6 1.392(7) . ?
C6 C5 1.393(10) . ?
C5 C4 1.360(10) . ?
C4 C3 1.360(8) . ?

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
C1 Au1 C1 177.3(2) 12 . ?
N1 Fe1 N1 88.71(12) 32 . ?
N1 Fe1 N1 88.71(12) 32 3_665 ?
N1 Fe1 N1 180.0 2_655 32 ?
N1 Fe1 N1 88.71(12) 33_545 . ?
N1 Fe1 N1 88.71(12) 2_655 31_655 ?
N1 Fe1 N1 180.00(13) 33_545 3_665 ?
N1 Fe1 N1 91.29(12) 32 31_655 ?
N1 Fe1 N1 180.0 31_655 . ?
N1 Fe1 N1 88.71(12) 2_655 33_545 ?
N1 Fe1 N1 91.29(12) 2_655 3_665 ?
N1 Fe1 N1 91.29(12) 32 33_545 ?
N1 Fe1 N1 88.72(12) 31_655 3_665 ?
N1 Fe1 N1 91.28(12) 31_655 33_545 ?
N1 Fe1 N1 91.29(12) . 3_665 ?
N1 Fe1 N1 91.29(12) 2_655 . ?
C1 N1 Fe1 174.4(3) . . ?
N1 C1 Au1 176.8(3) . . ?
N2 P1 C2 111.09(13) . . ?
N2 P1 C2 111.09(13) . 2_655 ?
N2 P1 C2 111.09(13) . 3_665 ?
C2 P1 C2 107.81(14) 2_655 . ?
C2 P1 C2 107.80(14) 3_665 . ?
C2 P1 C2 107.81(14) 2_655 3_665 ?
P1 N2 P1 180.0 . 16_545 ?
C7 C2 P1 121.9(3) . . ?
C7 C2 C3 119.6(4) . . ?
C3 C2 P1 118.5(4) . . ?
C2 C7 C6 119.3(5) . . ?
C7 C6 C5 119.7(6) . . ?
C4 C5 C6 120.5(5) . . ?
C5 C4 C3 120.2(6) . . ?
C4 C3 C2 120.7(6) . . ?

_iucr_refine_instructions_details 
;
TITL C in R-3c
    c.res
    created by SHELXL-2018/1 at 15:14:28 on 17-Jul-2019
CELL 0.71073 15.08575 15.08575 31.27077 90 90 120
ZERR 6 0.0008 0.0008 0.00139 0 0 0
LATT 3
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SYMM +Y,+X,0.5-Z
SYMM -Y+X,-Y,0.5-Z
SYMM -X,-X+Y,0.5-Z
SFAC C H Au Fe N P
UNIT 252 180 18 6 42 12
DELU 0.005 0.01 P1 N2
ISOR 0.01 0.02 N2

L.S. 20 0 0
PLAN  20
SIZE 0.094 0.144 0.161
TEMP -111(2)
fmap 2 53
acta
REM <olex2.extras>
REM <HklSrc "%.\\C.hkl">
REM </olex2.extras>

WGHT    0.032200   23.121799
FVAR       0.02177
AU1   3    0.333333    0.142669    0.416667    10.50000    0.02415    0.02579 =
         0.02295    0.00183    0.00367    0.01207
FE1   4    0.666667    0.333333    0.333333    10.16667    0.01401    0.01401 =
         0.01401    0.00000    0.00000    0.00700
N1    5    0.543098    0.255910    0.368990    11.00000    0.02329    0.02606 =
         0.02293   -0.00354   -0.00123    0.01429
C1    1    0.467943    0.213131    0.386945    11.00000    0.03099    0.02741 =
         0.02461   -0.00273   -0.00307    0.01907
P1    6    0.666667    0.333333    0.533754    10.33333    0.03048    0.03048 =
         0.01425    0.00000    0.00000    0.01524
N2    5    0.666667    0.333333    0.583333    10.16667    0.06649    0.06649 =
         0.02070    0.00000    0.00000    0.03325
C2    1    0.559071    0.339246    0.513163    11.00000    0.02787    0.03363 =
         0.03227   -0.01197   -0.00185    0.01603
C7    1    0.567672    0.400110    0.478649    11.00000    0.03981    0.03750 =
         0.05818   -0.00231   -0.01278    0.02382
AFIX  43
H7    2    0.631889    0.440459    0.464963    11.00000   -1.20000
AFIX   0
C6    1    0.481314    0.401772    0.464101    11.00000    0.07069    0.05574 =
         0.09786   -0.01330   -0.04003    0.04368
AFIX  43
H6    2    0.486362    0.443936    0.440590    11.00000   -1.20000
AFIX   0
C5    1    0.387471    0.341302    0.484191    11.00000    0.04694    0.07836 =
         0.12027   -0.05746   -0.04000    0.04776
AFIX  43
H5    2    0.328651    0.343055    0.474547    11.00000   -1.20000
AFIX   0
C4    1    0.379406    0.279761    0.517513    11.00000    0.03300    0.10086 =
         0.07916   -0.04470   -0.00547    0.03191
AFIX  43
H4    2    0.314740    0.237467    0.530548    11.00000   -1.20000
AFIX   0
C3    1    0.463678    0.278593    0.532233    11.00000    0.03173    0.06711 =
         0.04387   -0.01307    0.00386    0.01575
AFIX  43
H3    2    0.457510    0.236013    0.555754    11.00000   -1.20000
AFIX   0
HKLF 4




REM  C in R-3c
REM R1 =  0.0250 for    1471 Fo > 4sig(Fo)  and  0.0363 for all    1703 data
REM     85 parameters refined using      7 restraints

END  
     
WGHT      0.0322     23.1273 

REM Highest difference peak  1.145,  deepest hole -1.792,  1-sigma level  0.200
Q1    1   0.7162  0.3828  0.5833  10.50000  0.05    1.15
Q2    1   0.5202  0.3005  0.5231  11.00000  0.05    0.53
Q3    1   0.5346  0.1900  0.5656  11.00000  0.05    0.53
Q4    1   0.4516  0.1570  0.5956  11.00000  0.05    0.51
Q5    1   0.5902  0.3578  0.5232  11.00000  0.05    0.44
Q6    1   0.4556  0.1996  0.6164  11.00000  0.05    0.44
Q7    1   0.4786  0.2978  0.5808  11.00000  0.05    0.43
Q8    1   0.5032  0.4642  0.4181  11.00000  0.05    0.42
Q9    1   0.3880  0.3333  0.5833  10.50000  0.05    0.42
Q10   1   0.2149  0.3323  0.4832  11.00000  0.05    0.42
Q11   1   0.4890  0.2711  0.4888  11.00000  0.05    0.41
Q12   1   0.4533  0.3887  0.5618  11.00000  0.05    0.41
Q13   1   0.6390  0.4495  0.4976  11.00000  0.05    0.41
Q14   1   0.5352  0.2590  0.4991  11.00000  0.05    0.41
Q15   1   0.3290  0.4108  0.4316  11.00000  0.05    0.41
Q16   1   0.5259  0.1925  0.5833  10.50000  0.05    0.40
Q17   1   0.4978  0.2945  0.5449  11.00000  0.05    0.40
Q18   1   0.4289  0.2951  0.5246  11.00000  0.05    0.40
Q19   1   0.4488  0.1394  0.5391  11.00000  0.05    0.40
Q20   1   0.4657  0.2308  0.5903  11.00000  0.05    0.40

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0250 for 1471 Fo > 4sig(Fo) and 0.0363 for all 51108 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 1.15, deepest hole -1.79
  REM Mean Shift 0, Max Shift -0.001.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0363
  REM R1_gt = 0.0250
  REM wR_ref = 0.0591
  REM GOOF = 1.070
  REM Shift_max = -0.001
  REM Shift_mean = 0
  REM Reflections_all = 51108
  REM Reflections_gt = 1471
  REM Parameters = n/a
  REM Hole = -1.79
  REM Peak = 1.15
  REM Flack = n/a

  
;
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_PPNFeAu3_298K
_database_code_depnum_ccdc_archive 'CCDC 1977206'
loop_
_audit_author_name
_audit_author_address
'Zhao-Ping Ni'
;Key Laboratory of Bioinorganic and Synthetic Chemistry of Ministry of Education, School of Chemistry
China
;
_audit_update_record             
;
2020-01-11 deposited with the CCDC.	2020-03-13 downloaded from the CCDC.
;
_audit_creation_date             2019-08-03
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.17(Au18 C36 Fe6 N36), 1(C36 H30 N1 P2)'
_chemical_formula_sum            'C42 H30 Au3 Fe N7 P2'
_chemical_formula_weight         1341.39
_chemical_melting_point          ?
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'
Au Au -2.0133 8.8022 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c'
_space_group_name_Hall           '-R 3 2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'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'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'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'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-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'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-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'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   15.5023(7)
_cell_length_b                   15.5023(7)
_cell_length_c                   31.5971(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     6576.1(6)
_cell_formula_units_Z            6.00012
_cell_measurement_reflns_used    9932
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.83
_cell_measurement_theta_min      2.63
_shelx_estimated_absorpt_T_max   0.440
_shelx_estimated_absorpt_T_min   0.284
_exptl_absorpt_coefficient_mu    10.442
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4803
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1056 before and 0.0723 after correction. The Ratio of minimum to maximum transmission is 0.6441. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.032
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             3744
_exptl_crystal_size_max          0.161
_exptl_crystal_size_mid          0.144
_exptl_crystal_size_min          0.094
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0850
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            51693
_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         28.312
_diffrn_reflns_theta_min         1.991
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean ?
_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       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1464
_reflns_number_total             1832
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2014)'
_computing_structure_solution    'XT (Sheldrick, 2014)'
_refine_diff_density_max         1.984
_refine_diff_density_min         -3.540
_refine_diff_density_rms         0.267
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     53
_refine_ls_number_reflns         1832
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0446
_refine_ls_restrained_S_all      1.094
_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)+(0.0609P)²+111.3072P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1108
_refine_ls_wR_factor_ref         0.1235
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(P1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C2) = Uanis(C3) = Uanis(C4) = Uanis(C5) = Uanis(C6) = Uanis(C7)
Uanis(P1) = Uanis(N2)
3.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C6(H6), C5(H5), C4(H4), C3(H3)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Au1 Au 0.333333 0.13257(3) 0.416667 0.04832(18) Uani 1 2 d S T P . .
Fe1 Fe 0.666667 0.333333 0.333333 0.0238(4) Uani 1 6 d S T P . .
N1 N 0.5384(4) 0.2425(5) 0.3716(2) 0.0465(14) Uani 1 1 d . . . . .
C1 C 0.4645(6) 0.2011(6) 0.3882(2) 0.0475(17) Uani 1 1 d . . . . .
P1 P 0.666667 0.333333 0.53451(12) 0.0534(7) Uani 1 3 d S TU P . .
N2 N 0.666667 0.333333 0.583333 0.0534(7) Uani 1 6 d S T P . .
C2 C 0.5596(9) 0.3350(11) 0.5144(5) 0.0947(16) Uani 1 1 d . . . . .
C7 C 0.5667(10) 0.3944(11) 0.4806(5) 0.0947(16) Uani 1 1 d . . . . .
H7 H 0.627615 0.434361 0.467344 0.114 Uiso 1 1 calc R . . . .
C6 C 0.4805(9) 0.3936(11) 0.4664(5) 0.0947(16) Uani 1 1 d . . . . .
H6 H 0.483158 0.432765 0.443573 0.114 Uiso 1 1 calc R . . . .
C5 C 0.3909(9) 0.3328(11) 0.4871(4) 0.0947(16) Uani 1 1 d . . . . .
H5 H 0.334321 0.334815 0.478937 0.114 Uiso 1 1 calc R . . . .
C4 C 0.3838(10) 0.2724(12) 0.5180(5) 0.0947(16) Uani 1 1 d . . . . .
H4 H 0.322296 0.229356 0.530104 0.114 Uiso 1 1 calc R . . . .
C3 C 0.4696(9) 0.2739(10) 0.5323(4) 0.0947(16) Uani 1 1 d . . . . .
H3 H 0.465077 0.232416 0.554526 0.114 Uiso 1 1 calc R . . . .

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
Au1 0.0334(2) 0.0516(2) 0.0539(3) 0.00875(8) 0.01751(16) 0.01672(12)
Fe1 0.0210(5) 0.0210(5) 0.0294(9) 0.000 0.000 0.0105(3)
N1 0.034(3) 0.045(3) 0.054(3) 0.009(3) 0.017(3) 0.014(3)
C1 0.040(4) 0.045(4) 0.051(4) 0.003(3) 0.010(3) 0.017(3)
P1 0.0553(7) 0.0553(7) 0.0497(10) 0.000 0.000 0.0276(4)
N2 0.0553(7) 0.0553(7) 0.0497(10) 0.000 0.000 0.0276(4)
C2 0.073(3) 0.105(4) 0.114(4) -0.016(3) -0.010(3) 0.050(3)
C7 0.073(3) 0.105(4) 0.114(4) -0.016(3) -0.010(3) 0.050(3)
C6 0.073(3) 0.105(4) 0.114(4) -0.016(3) -0.010(3) 0.050(3)
C5 0.073(3) 0.105(4) 0.114(4) -0.016(3) -0.010(3) 0.050(3)
C4 0.073(3) 0.105(4) 0.114(4) -0.016(3) -0.010(3) 0.050(3)
C3 0.073(3) 0.105(4) 0.114(4) -0.016(3) -0.010(3) 0.050(3)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Au1 C1 1.978(7) 12 ?
Au1 C1 1.978(7) . ?
Fe1 N1 2.144(6) 33_545 ?
Fe1 N1 2.144(6) 2_655 ?
Fe1 N1 2.144(6) 31_655 ?
Fe1 N1 2.144(6) 32 ?
Fe1 N1 2.144(6) . ?
Fe1 N1 2.144(6) 3_665 ?
N1 C1 1.125(9) . ?
P1 N2 1.543(4) . ?
P1 C2 1.789(13) 2_655 ?
P1 C2 1.789(13) 3_665 ?
P1 C2 1.789(13) . ?
C2 C7 1.380(19) . ?
C2 C3 1.358(18) . ?
C7 C6 1.403(17) . ?
C6 C5 1.392(19) . ?
C5 C4 1.318(19) . ?
C4 C3 1.394(16) . ?

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
C1 Au1 C1 177.4(5) 12 . ?
N1 Fe1 N1 91.4(3) 2_655 3_665 ?
N1 Fe1 N1 91.4(3) 2_655 . ?
N1 Fe1 N1 88.6(3) 31_655 3_665 ?
N1 Fe1 N1 88.6(3) 33_545 . ?
N1 Fe1 N1 180.0 31_655 . ?
N1 Fe1 N1 91.4(3) 3_665 . ?
N1 Fe1 N1 91.4(3) 33_545 31_655 ?
N1 Fe1 N1 91.4(3) 33_545 32 ?
N1 Fe1 N1 88.6(3) 32 3_665 ?
N1 Fe1 N1 91.4(3) 31_655 32 ?
N1 Fe1 N1 88.6(3) 33_545 2_655 ?
N1 Fe1 N1 180.0 2_655 32 ?
N1 Fe1 N1 88.6(3) 32 . ?
N1 Fe1 N1 180.0 33_545 3_665 ?
N1 Fe1 N1 88.6(3) 31_655 2_655 ?
C1 N1 Fe1 169.7(7) . . ?
N1 C1 Au1 177.6(8) . . ?
N2 P1 C2 110.8(5) . 2_655 ?
N2 P1 C2 110.8(5) . . ?
N2 P1 C2 110.8(5) . 3_665 ?
C2 P1 C2 108.1(5) 2_655 . ?
C2 P1 C2 108.1(5) 2_655 3_665 ?
C2 P1 C2 108.1(5) 3_665 . ?
P1 N2 P1 180.0 . 16_545 ?
C7 C2 P1 121.3(11) . . ?
C3 C2 P1 118.7(12) . . ?
C3 C2 C7 120.0(13) . . ?
C2 C7 C6 118.9(14) . . ?
C5 C6 C7 118.6(15) . . ?
C4 C5 C6 122.0(13) . . ?
C5 C4 C3 119.3(14) . . ?
C2 C3 C4 121.0(15) . . ?

_iucr_refine_instructions_details 
;
TITL a_a.res in R-3c
    a.res
    created by SHELXL-2018/1 at 16:02:23 on 17-Jul-2019
REM Old TITL A in R-3c
REM SHELXT solution in R-3c
REM R1 0.194, Rweak 0.012, Alpha 0.013, Orientation as input
REM Formula found by SHELXT: C24 N12 P2 Fe Au3
CELL 0.71073 15.5023 15.5023 31.5971 90 90 120
ZERR 6.00012 0.0007 0.0007 0.0012 0 0 0
LATT 3
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SYMM +Y,+X,0.5-Z
SYMM -Y+X,-Y,0.5-Z
SYMM -X,-X+Y,0.5-Z
SFAC C H Au Fe N P
UNIT 252 180 18 6 42 12
ISOR 0.001 0.002 P1
EADP C2 C3 C4 C5 C6 C7
EADP P1 N2

L.S. 20
PLAN  20
SIZE 0.094 0.144 0.161
TEMP 24.93
list 4
fmap 2 53
ACTA
REM <olex2.extras>
REM <HklSrc "%.\\A.hkl">
REM </olex2.extras>

WGHT    0.060900  111.307205
FVAR       0.08319
AU1   3    0.333333    0.132569    0.416667    10.50000    0.03343    0.05159 =
         0.05389    0.00875    0.01751    0.01672
FE1   4    0.666667    0.333333    0.333333    10.16667    0.02101    0.02101 =
         0.02944    0.00000    0.00000    0.01050
N1    5    0.538356    0.242502    0.371565    11.00000    0.03384    0.04466 =
         0.05414    0.00938    0.01684    0.01447
C1    1    0.464514    0.201105    0.388223    11.00000    0.04045    0.04520 =
         0.05062    0.00308    0.01046    0.01669
P1    6    0.666667    0.333333    0.534512    10.33333    0.05528    0.05528 =
         0.04967    0.00000    0.00000    0.02764
N2    5    0.666667    0.333333    0.583333    10.16667    0.05528    0.05528 =
         0.04967    0.00000    0.00000    0.02764
C2    1    0.559632    0.335030    0.514439    11.00000    0.07279    0.10531 =
         0.11373   -0.01586   -0.01030    0.05025
C7    1    0.566696    0.394411    0.480559    11.00000    0.07279    0.10531 =
         0.11373   -0.01586   -0.01030    0.05025
AFIX  43
H7    2    0.627615    0.434361    0.467344    11.00000   -1.20000
AFIX   0
C6    1    0.480492    0.393550    0.466368    11.00000    0.07279    0.10531 =
         0.11373   -0.01586   -0.01030    0.05025
AFIX  43
H6    2    0.483158    0.432765    0.443573    11.00000   -1.20000
AFIX   0
C5    1    0.390900    0.332776    0.487120    11.00000    0.07279    0.10531 =
         0.11373   -0.01586   -0.01030    0.05025
AFIX  43
H5    2    0.334321    0.334815    0.478937    11.00000   -1.20000
AFIX   0
C4    1    0.383825    0.272442    0.518008    11.00000    0.07279    0.10531 =
         0.11373   -0.01586   -0.01030    0.05025
AFIX  43
H4    2    0.322296    0.229356    0.530104    11.00000   -1.20000
AFIX   0
C3    1    0.469595    0.273923    0.532349    11.00000    0.07279    0.10531 =
         0.11373   -0.01586   -0.01030    0.05025
AFIX  43
H3    2    0.465077    0.232416    0.554526    11.00000   -1.20000
AFIX   0
HKLF 4




REM  a_a.res in R-3c
REM R1 =  0.0446 for    1464 Fo > 4sig(Fo)  and  0.0618 for all    1832 data
REM     53 parameters refined using      6 restraints

END  
     
WGHT      0.0608    111.7124 

REM Highest difference peak  1.984,  deepest hole -3.540,  1-sigma level  0.267
Q1    1   0.3806  0.3165  0.5080  11.00000  0.05    0.89
Q2    1   0.4122  0.3671  0.4646  11.00000  0.05    0.88
Q3    1   0.4589  0.3100  0.5272  11.00000  0.05    0.78
Q4    1   0.5158  0.4038  0.4453  11.00000  0.05    0.77
Q5    1   0.3772  0.2227  0.5273  11.00000  0.05    0.67
Q6    1   0.6567  0.3010  0.5303  11.00000  0.05    0.63
Q7    1   0.4553  0.3904  0.4893  11.00000  0.05    0.62
Q8    1   0.5705  0.3781  0.4685  11.00000  0.05    0.59
Q9    1   0.4355  0.3255  0.5660  11.00000  0.05    0.58
Q10   1   0.3722  0.2258  0.5324  11.00000  0.05    0.57
Q11   1   0.5650  0.4123  0.4965  11.00000  0.05    0.57
Q12   1   0.4502  0.2858  0.5866  11.00000  0.05    0.57
Q13   1   0.3884  0.2930  0.5915  11.00000  0.05    0.55
Q14   1   0.3277  0.1925  0.5546  11.00000  0.05    0.55
Q15   1   0.4650  0.1822  0.5869  11.00000  0.05    0.51
Q16   1   0.4478  0.3333  0.5833  10.50000  0.05    0.50
Q17   1   0.4732  0.1680  0.5526  11.00000  0.05    0.48
Q18   1   0.4038  0.3342  0.5229  11.00000  0.05    0.47
Q19   1   0.4489  0.2159  0.5327  11.00000  0.05    0.47
Q20   1   0.4434  0.3848  0.5660  11.00000  0.05    0.46

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0446 for 1464 Fo > 4sig(Fo) and 0.0618 for all 54869 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 1.98, deepest hole -3.54
  REM Mean Shift 0, Max Shift 0.000.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0618
  REM R1_gt = 0.0446
  REM wR_ref = 0.1235
  REM GOOF = 1.090
  REM Shift_max = 0.000
  REM Shift_mean = 0
  REM Reflections_all = 54869
  REM Reflections_gt = 1464
  REM Parameters = n/a
  REM Hole = -3.54
  REM Peak = 1.98
  REM Flack = n/a

  
;
_olex2_submission_special_instructions 'No special instructions were received'
