# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_shen8
_database_code_depnum_ccdc_archive 'CCDC 2068053'
loop_
_audit_author_name
_audit_author_address
'Khalil Abboud'
;University of Florida
United States of America
;
# end Validation Reply Form
_audit_update_record             
;
2021-03-04 deposited with the CCDC.	2021-08-09 downloaded from the CCDC.
;


# start Validation Reply Form
_vrf_PLAT332_shen8               
;
PROBLEM: Large Phenyl C-C Range C9? -C14? . 0.28 Ang.
RESPONSE: The C9-C14 and C9'-C14' are idealized (AFIX 66) with equivalent
 displacement parameters
;
_vrf_PLAT971_shen8               
;
PROBLEM: Check Calcd Resid. Dens. 0.62A From Au1 2.56 eA-3
RESPONSE: Probably due to the gold anisotropy or data truncation.
;
# publcif _publ_body_element loop end

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H27 Au N3 P'
_chemical_formula_weight         609.44

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'
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.2089(6)
_cell_length_b                   14.1145(7)
_cell_length_c                   13.2833(7)
_cell_angle_alpha                90
_cell_angle_beta                 94.635(2)
_cell_angle_gamma                90
_cell_volume                     2281.5(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9965
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      32.83

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow

_exptl_crystal_density_meas      .

_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.774
_exptl_crystal_F_000             1192

_exptl_transmission_factor_min   0.3985
_exptl_transmission_factor_max   0.5659

_exptl_crystal_size_max          0.322
_exptl_crystal_size_mid          0.163
_exptl_crystal_size_min          0.152
_exptl_absorpt_coefficient_mu    6.537
_shelx_estimated_absorpt_T_min   0.227
_shelx_estimated_absorpt_T_max   0.437
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3341
_exptl_absorpt_correction_T_max  0.5316

_exptl_absorpt_process_details   
'Sheldrick, G. M., sadabs (2014). Acta Cryst. C71, 3--8.'

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'I\mS microsource 3.0'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?

_diffrn_reflns_number            70033
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_av_R_equivalents  0.0514
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.210
_diffrn_reflns_theta_max         33.273
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.926
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.926
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             8150
_reflns_number_gt                7065
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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. 
;

_computing_data_collection       'Bruker APEX3 (Bruker, 2014)'
_computing_cell_refinement       'Bruker APEX3 (Bruker, 2014)'
_computing_data_reduction        'Bruker Apex3 SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXL2014/7, Sheldrick G. M. 2014'
_computing_structure_refinement  'SHELXL2014/7, Sheldrick G. M. 2014'
_computing_molecular_graphics    'XP in SHELXTL-plus, Bruker 2014'
_computing_publication_material  'SHELXL2014/7, Sheldrick, G. M. 2014'

_refine_special_details          
;
All H atoms were positioned geometrically ( C---H = 0.93/1.00 Å) and   
allowed to ride with Uiso(H)= 1.2/1.5Ueq(C).
Methyl ones were allowed to rotate around the corresponding C---C.

The Au complex has one of the phenyl rings disordered and refined in two parts
 with their site occupation factors dependently refined to 0.54(1) and 0.45(1),
 respectively. A major disorder is observed in the C8 ring.  Only C1 and C2 are
 not disordered while the rest of the ring, C3-C8, is disordered and refined in
 three parts. The site occupation factors of the three parts of C3-C8 disordered
 parts are dependently refined using SUMP; refined to 0.49(1), 0.31(1 and
 0.20(1).  
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0191P)²+11.3588P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap

_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8150
_refine_ls_number_parameters     320
_refine_ls_number_restraints     104
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0420
_refine_ls_wR_factor_ref         0.0941
_refine_ls_wR_factor_gt          0.0909
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_restrained_S_all      1.130
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

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 0.20273(2) 0.56454(2) 0.61289(2) 0.02963(5) Uani 1 1 d . . . . .
P1 P 0.20932(8) 0.55279(8) 0.44577(8) 0.0272(2) Uani 1 1 d . . . . .
N1 N 0.2034(4) 0.5804(3) 0.7672(3) 0.0399(9) Uani 1 1 d . . . . .
N2 N 0.2110(4) 0.6645(4) 0.8067(4) 0.0500(11) Uani 1 1 d . . . . .
N3 N 0.1986(4) 0.6658(4) 0.8999(4) 0.0523(12) Uani 1 1 d . . . . .
C1 C 0.1766(5) 0.5205(4) 0.8386(4) 0.0491(13) Uani 1 1 d D . . . .
C2 C 0.1766(5) 0.5723(4) 0.9249(4) 0.0508(13) Uani 1 1 d D . . . .
C3 C 0.1624(12) 0.5372(13) 1.0299(8) 0.0493(19) Uani 0.490(13) 1 d D . P A 1
H3A H 0.105702 0.486919 1.025830 0.059 Uiso 0.490(13) 1 calc R U P A 1
H3AB H 0.134791 0.590010 1.069801 0.059 Uiso 0.490(13) 1 calc R U P A 1
C4 C 0.2661(13) 0.4981(9) 1.0858(10) 0.0493(19) Uani 0.490(13) 1 d D . P A 1
H4A H 0.244939 0.457835 1.142069 0.059 Uiso 0.490(13) 1 calc R U P A 1
H4AB H 0.309909 0.551690 1.115539 0.059 Uiso 0.490(13) 1 calc R U P A 1
C5 C 0.3384(9) 0.4398(8) 1.0197(8) 0.0493(19) Uani 0.490(13) 1 d D . P A 1
H5A H 0.405455 0.419508 1.061026 0.059 Uiso 0.490(13) 1 calc R U P A 1
H5AB H 0.361522 0.480257 0.964378 0.059 Uiso 0.490(13) 1 calc R U P A 1
C6 C 0.2792(11) 0.3516(7) 0.9740(7) 0.0493(19) Uani 0.490(13) 1 d D . P A 1
H6A H 0.326426 0.295705 0.989912 0.059 Uiso 0.490(13) 1 calc R U P A 1
H6AB H 0.210612 0.342543 1.007685 0.059 Uiso 0.490(13) 1 calc R U P A 1
C7 C 0.2500(11) 0.3539(8) 0.8593(8) 0.0493(19) Uani 0.490(13) 1 d D . P A 1
H7A H 0.315427 0.375038 0.826084 0.059 Uiso 0.490(13) 1 calc R U P A 1
H7AB H 0.232770 0.288511 0.836067 0.059 Uiso 0.490(13) 1 calc R U P A 1
C8 C 0.1540(12) 0.4174(7) 0.8244(10) 0.0493(19) Uani 0.490(13) 1 d D . P A 1
H8A H 0.133700 0.405326 0.751866 0.059 Uiso 0.490(13) 1 calc R U P A 1
H8AB H 0.090052 0.400232 0.861973 0.059 Uiso 0.490(13) 1 calc R U P A 1
C3' C 0.175(4) 0.523(4) 1.038(2) 0.155(10) Uani 0.309(14) 1 d D . P A 2
H3'A H 0.153338 0.568382 1.090072 0.186 Uiso 0.309(14) 1 calc R U P A 2
H3'B H 0.127299 0.466165 1.037722 0.186 Uiso 0.309(14) 1 calc R U P A 2
C4' C 0.307(3) 0.496(2) 1.052(3) 0.155(10) Uani 0.309(14) 1 d D . P A 2
H4'A H 0.343596 0.521430 1.115827 0.186 Uiso 0.309(14) 1 calc R U P A 2
H4'B H 0.346764 0.516447 0.994001 0.186 Uiso 0.309(14) 1 calc R U P A 2
C5' C 0.288(5) 0.380(3) 1.056(2) 0.155(10) Uani 0.309(14) 1 d D . P A 2
H5'A H 0.342533 0.348229 1.103486 0.186 Uiso 0.309(14) 1 calc R U P A 2
H5'B H 0.212627 0.362888 1.070821 0.186 Uiso 0.309(14) 1 calc R U P A 2
C6' C 0.311(3) 0.362(4) 0.937(3) 0.155(10) Uani 0.309(14) 1 d D . P A 2
H6'A H 0.340380 0.418856 0.904598 0.186 Uiso 0.309(14) 1 calc R U P A 2
H6'B H 0.360366 0.307349 0.928456 0.186 Uiso 0.309(14) 1 calc R U P A 2
C7' C 0.188(4) 0.340(2) 0.895(3) 0.155(10) Uani 0.309(14) 1 d D . P A 2
H7'A H 0.141474 0.336930 0.952763 0.186 Uiso 0.309(14) 1 calc R U P A 2
H7'B H 0.185393 0.276595 0.862474 0.186 Uiso 0.309(14) 1 calc R U P A 2
C8' C 0.137(4) 0.4156(16) 0.816(3) 0.155(10) Uani 0.309(14) 1 d D . P A 2
H8'A H 0.156654 0.397586 0.747702 0.186 Uiso 0.309(14) 1 calc R U P A 2
H8'B H 0.055811 0.413418 0.815429 0.186 Uiso 0.309(14) 1 calc R U P A 2
C3" C 0.147(3) 0.547(3) 1.0331(16) 0.057(5) Uani 0.201(14) 1 d D . P A 3
H3"A H 0.089266 0.497832 1.031116 0.068 Uiso 0.201(14) 1 calc R U P A 3
H3"B H 0.120907 0.603770 1.067879 0.068 Uiso 0.201(14) 1 calc R U P A 3
C4" C 0.256(3) 0.509(2) 1.088(2) 0.057(5) Uani 0.201(14) 1 d D . P A 3
H4"A H 0.253036 0.511039 1.162189 0.068 Uiso 0.201(14) 1 calc R U P A 3
H4"B H 0.319715 0.547625 1.069832 0.068 Uiso 0.201(14) 1 calc R U P A 3
C5" C 0.265(3) 0.4050(17) 1.049(2) 0.057(5) Uani 0.201(14) 1 d D . P A 3
H5"A H 0.193720 0.382421 1.017740 0.068 Uiso 0.201(14) 1 calc R U P A 3
H5"B H 0.289976 0.361770 1.105382 0.068 Uiso 0.201(14) 1 calc R U P A 3
C6" C 0.353(2) 0.412(2) 0.9694(17) 0.057(5) Uani 0.201(14) 1 d D . P A 3
H6"A H 0.370468 0.478839 0.954220 0.068 Uiso 0.201(14) 1 calc R U P A 3
H6"B H 0.422210 0.378906 0.993227 0.068 Uiso 0.201(14) 1 calc R U P A 3
C7" C 0.294(3) 0.3613(19) 0.8751(17) 0.057(5) Uani 0.201(14) 1 d D . P A 3
H7"A H 0.348905 0.352746 0.824472 0.068 Uiso 0.201(14) 1 calc R U P A 3
H7"B H 0.272246 0.297336 0.896251 0.068 Uiso 0.201(14) 1 calc R U P A 3
C8" C 0.191(2) 0.4111(15) 0.822(2) 0.057(5) Uani 0.201(14) 1 d D . P A 3
H8"A H 0.125097 0.378946 0.843947 0.068 Uiso 0.201(14) 1 calc R U P A 3
H8"B H 0.191785 0.400124 0.748199 0.068 Uiso 0.201(14) 1 calc R U P A 3
C9 C 0.131(2) 0.6444(15) 0.377(2) 0.0277(16) Uani 0.54(4) 1 d . . P B 1
C10 C 0.0328(14) 0.6804(11) 0.4144(13) 0.0277(16) Uani 0.54(4) 1 d . . P B 1
H10 H 0.011589 0.659148 0.477842 0.033 Uiso 0.54(4) 1 calc R U P B 1
C11 C -0.0323(10) 0.7462(9) 0.3592(9) 0.0277(16) Uani 0.54(4) 1 d . . P B 1
H11 H -0.098922 0.767525 0.383861 0.033 Uiso 0.54(4) 1 calc R U P B 1
C12 C -0.0028(12) 0.7778(10) 0.2759(11) 0.0277(16) Uani 0.54(4) 1 d . . P B 1
H12 H -0.048684 0.821590 0.238146 0.033 Uiso 0.54(4) 1 calc R U P B 1
C13 C 0.0992(14) 0.7481(12) 0.2377(14) 0.0277(16) Uani 0.54(4) 1 d . . P B 1
H13 H 0.121519 0.774166 0.176649 0.033 Uiso 0.54(4) 1 calc R U P B 1
C14 C 0.1651(14) 0.6808(11) 0.2909(12) 0.0277(16) Uani 0.54(4) 1 d . . P B 1
H14 H 0.232658 0.661069 0.266826 0.033 Uiso 0.54(4) 1 calc R U P B 1
C9' C 0.123(3) 0.638(2) 0.374(2) 0.039(4) Uani 0.46(4) 1 d . . P B 2
C10' C 0.025(2) 0.656(2) 0.408(2) 0.061(7) Uani 0.46(4) 1 d . . P B 2
H10' H 0.004924 0.628374 0.468258 0.073 Uiso 0.46(4) 1 calc R U P B 2
C11' C -0.044(2) 0.716(3) 0.354(2) 0.084(9) Uani 0.46(4) 1 d . . P B 2
H11' H -0.113997 0.729740 0.377489 0.101 Uiso 0.46(4) 1 calc R U P B 2
C12' C -0.011(2) 0.761(3) 0.2548(17) 0.076(8) Uani 0.46(4) 1 d . . P B 2
H12' H -0.059632 0.803306 0.217647 0.091 Uiso 0.46(4) 1 calc R U P B 2
C13' C 0.0813(17) 0.7399(19) 0.2238(16) 0.052(6) Uani 0.46(4) 1 d . . P B 2
H13' H 0.103492 0.767376 0.163386 0.063 Uiso 0.46(4) 1 calc R U P B 2
C14' C 0.1501(14) 0.6770(16) 0.2783(12) 0.039(4) Uani 0.46(4) 1 d . . P B 2
H14' H 0.217027 0.658915 0.251902 0.046 Uiso 0.46(4) 1 calc R U P B 2
C15 C 0.3490(3) 0.5693(3) 0.4117(3) 0.0300(8) Uani 1 1 d . . . . .
C16 C 0.4086(4) 0.6441(4) 0.4571(3) 0.0368(10) Uani 1 1 d . . . . .
H16 H 0.376876 0.682054 0.506150 0.044 Uiso 1 1 calc R U . . .
C21 C 0.1636(3) 0.4399(3) 0.3937(3) 0.0299(8) Uani 1 1 d . . . . .
C20 C 0.3968(4) 0.5133(3) 0.3415(3) 0.0343(9) Uani 1 1 d . . . . .
H20 H 0.357489 0.461384 0.310824 0.041 Uiso 1 1 calc R U . . .
C19 C 0.5031(4) 0.5338(4) 0.3162(4) 0.0407(11) Uani 1 1 d . . . . .
H19 H 0.536132 0.495784 0.267988 0.049 Uiso 1 1 calc R U . . .
C18 C 0.5602(4) 0.6088(4) 0.3609(4) 0.0407(11) Uani 1 1 d . . . . .
H18 H 0.632167 0.622746 0.342819 0.049 Uiso 1 1 calc R U . . .
C17 C 0.5138(4) 0.6635(4) 0.4311(4) 0.0398(11) Uani 1 1 d . . . . .
H17 H 0.553964 0.714802 0.462180 0.048 Uiso 1 1 calc R U . . .
C22 C 0.0941(4) 0.4338(4) 0.3045(4) 0.0401(10) Uani 1 1 d . . . . .
H22 H 0.070460 0.489858 0.269654 0.048 Uiso 1 1 calc R U . . .
C23 C 0.0603(4) 0.3468(4) 0.2676(4) 0.0442(12) Uani 1 1 d . . . . .
H23 H 0.013624 0.342975 0.206991 0.053 Uiso 1 1 calc R U . . .
C24 C 0.0935(4) 0.2652(4) 0.3179(4) 0.0390(10) Uani 1 1 d . . . . .
H24 H 0.069042 0.205384 0.292151 0.047 Uiso 1 1 calc R U . . .
C25 C 0.1626(4) 0.2700(4) 0.4059(4) 0.0370(9) Uani 1 1 d . . . . .
H25 H 0.186188 0.213504 0.439951 0.044 Uiso 1 1 calc R U . . .
C26 C 0.1972(3) 0.3576(3) 0.4440(3) 0.0306(8) Uani 1 1 d . . . . .
H26 H 0.243888 0.361044 0.504647 0.037 Uiso 1 1 calc R U . . .


_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 N1 2.061(4) . ?
Au1 P1 2.2340(10) . ?
P1 C21 1.807(5) . ?
P1 C9 1.81(2) . ?
P1 C15 1.815(4) . ?
P1 C9' 1.82(3) . ?
N1 N2 1.298(7) . ?
N1 C1 1.331(7) . ?
N2 N3 1.260(7) . ?
N3 C2 1.392(8) . ?
C1 C2 1.359(7) . ?
C1 C8 1.490(11) . ?
C1 C8" 1.57(2) . ?
C1 C8' 1.58(3) . ?
C2 C3 1.503(11) . ?
C2 C3" 1.55(2) . ?
C2 C3' 1.66(3) . ?
C3 C4 1.518(11) . ?
C3 H3A 0.9900 . ?
C3 H3AB 0.9900 . ?
C4 C5 1.535(13) . ?
C4 H4A 0.9900 . ?
C4 H4AB 0.9900 . ?
C5 C6 1.539(12) . ?
C5 H5A 0.9900 . ?
C5 H5AB 0.9900 . ?
C6 C7 1.536(11) . ?
C6 H6A 0.9900 . ?
C6 H6AB 0.9900 . ?
C7 C8 1.518(12) . ?
C7 H7A 0.9900 . ?
C7 H7AB 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8AB 0.9900 . ?
C3' C4' 1.65(3) . ?
C3' H3'A 0.9900 . ?
C3' H3'B 0.9900 . ?
C4' C5' 1.65(3) . ?
C4' H4'A 0.9900 . ?
C4' H4'B 0.9900 . ?
C5' C6' 1.65(3) . ?
C5' H5'A 0.9900 . ?
C5' H5'B 0.9900 . ?
C6' C7' 1.59(3) . ?
C6' H6'A 0.9900 . ?
C6' H6'B 0.9900 . ?
C7' C8' 1.59(3) . ?
C7' H7'A 0.9900 . ?
C7' H7'B 0.9900 . ?
C8' H8'A 0.9900 . ?
C8' H8'B 0.9900 . ?
C3" C4" 1.56(2) . ?
C3" H3"A 0.9900 . ?
C3" H3"B 0.9900 . ?
C4" C5" 1.57(2) . ?
C4" H4"A 0.9900 . ?
C4" H4"B 0.9900 . ?
C5" C6" 1.58(2) . ?
C5" H5"A 0.9900 . ?
C5" H5"B 0.9900 . ?
C6" C7" 1.57(2) . ?
C6" H6"A 0.9900 . ?
C6" H6"B 0.9900 . ?
C7" C8" 1.56(2) . ?
C7" H7"A 0.9900 . ?
C7" H7"B 0.9900 . ?
C8" H8"A 0.9900 . ?
C8" H8"B 0.9900 . ?
C9 C14 1.35(2) . ?
C9 C10 1.43(3) . ?
C10 C11 1.392(18) . ?
C10 H10 0.9500 . ?
C11 C12 1.27(2) . ?
C11 H11 0.9500 . ?
C12 C13 1.44(2) . ?
C12 H12 0.9500 . ?
C13 C14 1.399(19) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C9' C10' 1.34(4) . ?
C9' C14' 1.44(3) . ?
C10' C11' 1.35(2) . ?
C10' H10' 0.9500 . ?
C11' C12' 1.55(3) . ?
C11' H11' 0.9500 . ?
C12' C13' 1.27(3) . ?
C12' H12' 0.9500 . ?
C13' C14' 1.38(2) . ?
C13' H13' 0.9500 . ?
C14' H14' 0.9500 . ?
C15 C20 1.386(6) . ?
C15 C16 1.391(7) . ?
C16 C17 1.384(6) . ?
C16 H16 0.9500 . ?
C21 C26 1.386(6) . ?
C21 C22 1.403(6) . ?
C20 C19 1.397(6) . ?
C20 H20 0.9500 . ?
C19 C18 1.375(8) . ?
C19 H19 0.9500 . ?
C18 C17 1.368(8) . ?
C18 H18 0.9500 . ?
C17 H17 0.9500 . ?
C22 C23 1.373(7) . ?
C22 H22 0.9500 . ?
C23 C24 1.376(8) . ?
C23 H23 0.9500 . ?
C24 C25 1.387(7) . ?
C24 H24 0.9500 . ?
C25 C26 1.389(7) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?

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
N1 Au1 P1 176.98(13) . . ?
C21 P1 C9 107.7(8) . . ?
C21 P1 C15 106.6(2) . . ?
C9 P1 C15 104.4(8) . . ?
C21 P1 C9' 103.6(10) . . ?
C15 P1 C9' 107.2(9) . . ?
C21 P1 Au1 114.26(14) . . ?
C9 P1 Au1 112.9(8) . . ?
C15 P1 Au1 110.40(14) . . ?
C9' P1 Au1 114.2(10) . . ?
N2 N1 C1 107.8(4) . . ?
N2 N1 Au1 119.7(3) . . ?
C1 N1 Au1 131.2(4) . . ?
N3 N2 N1 113.6(5) . . ?
N2 N3 C2 105.2(5) . . ?
N1 C1 C2 106.0(5) . . ?
N1 C1 C8 125.7(7) . . ?
C2 C1 C8 128.2(7) . . ?
N1 C1 C8" 119.0(13) . . ?
C2 C1 C8" 131.0(11) . . ?
N1 C1 C8' 123.3(14) . . ?
C2 C1 C8' 130.1(14) . . ?
C1 C2 N3 107.2(5) . . ?
C1 C2 C3 127.8(9) . . ?
N3 C2 C3 124.9(8) . . ?
C1 C2 C3" 132.4(16) . . ?
N3 C2 C3" 120.1(15) . . ?
C1 C2 C3' 123(2) . . ?
N3 C2 C3' 129(2) . . ?
C2 C3 C4 114.8(9) . . ?
C2 C3 H3A 108.6 . . ?
C4 C3 H3A 108.6 . . ?
C2 C3 H3AB 108.6 . . ?
C4 C3 H3AB 108.6 . . ?
H3A C3 H3AB 107.5 . . ?
C3 C4 C5 114.3(8) . . ?
C3 C4 H4A 108.7 . . ?
C5 C4 H4A 108.7 . . ?
C3 C4 H4AB 108.7 . . ?
C5 C4 H4AB 108.7 . . ?
H4A C4 H4AB 107.6 . . ?
C4 C5 C6 112.7(10) . . ?
C4 C5 H5A 109.0 . . ?
C6 C5 H5A 109.0 . . ?
C4 C5 H5AB 109.0 . . ?
C6 C5 H5AB 109.0 . . ?
H5A C5 H5AB 107.8 . . ?
C7 C6 C5 116.1(9) . . ?
C7 C6 H6A 108.3 . . ?
C5 C6 H6A 108.3 . . ?
C7 C6 H6AB 108.3 . . ?
C5 C6 H6AB 108.3 . . ?
H6A C6 H6AB 107.4 . . ?
C8 C7 C6 115.3(9) . . ?
C8 C7 H7A 108.5 . . ?
C6 C7 H7A 108.5 . . ?
C8 C7 H7AB 108.5 . . ?
C6 C7 H7AB 108.5 . . ?
H7A C7 H7AB 107.5 . . ?
C1 C8 C7 114.1(9) . . ?
C1 C8 H8A 108.7 . . ?
C7 C8 H8A 108.7 . . ?
C1 C8 H8AB 108.7 . . ?
C7 C8 H8AB 108.7 . . ?
H8A C8 H8AB 107.6 . . ?
C4' C3' C2 97(3) . . ?
C4' C3' H3'A 112.5 . . ?
C2 C3' H3'A 112.4 . . ?
C4' C3' H3'B 112.5 . . ?
C2 C3' H3'B 112.4 . . ?
H3'A C3' H3'B 110.0 . . ?
C3' C4' C5' 95(3) . . ?
C3' C4' H4'A 112.7 . . ?
C5' C4' H4'A 112.7 . . ?
C3' C4' H4'B 112.7 . . ?
C5' C4' H4'B 112.7 . . ?
H4'A C4' H4'B 110.1 . . ?
C6' C5' C4' 95(3) . . ?
C6' C5' H5'A 112.7 . . ?
C4' C5' H5'A 112.7 . . ?
C6' C5' H5'B 112.7 . . ?
C4' C5' H5'B 112.7 . . ?
H5'A C5' H5'B 110.1 . . ?
C7' C6' C5' 98(3) . . ?
C7' C6' H6'A 112.2 . . ?
C5' C6' H6'A 112.2 . . ?
C7' C6' H6'B 112.2 . . ?
C5' C6' H6'B 112.2 . . ?
H6'A C6' H6'B 109.8 . . ?
C6' C7' C8' 113.9(18) . . ?
C6' C7' H7'A 108.8 . . ?
C8' C7' H7'A 108.8 . . ?
C6' C7' H7'B 108.8 . . ?
C8' C7' H7'B 108.8 . . ?
H7'A C7' H7'B 107.7 . . ?
C1 C8' C7' 114.1(16) . . ?
C1 C8' H8'A 108.7 . . ?
C7' C8' H8'A 108.7 . . ?
C1 C8' H8'B 108.7 . . ?
C7' C8' H8'B 108.7 . . ?
H8'A C8' H8'B 107.6 . . ?
C2 C3" C4" 105(2) . . ?
C2 C3" H3"A 110.8 . . ?
C4" C3" H3"A 110.8 . . ?
C2 C3" H3"B 110.8 . . ?
C4" C3" H3"B 110.8 . . ?
H3"A C3" H3"B 108.8 . . ?
C3" C4" C5" 104.3(19) . . ?
C3" C4" H4"A 110.9 . . ?
C5" C4" H4"A 110.9 . . ?
C3" C4" H4"B 110.9 . . ?
C5" C4" H4"B 110.9 . . ?
H4"A C4" H4"B 108.9 . . ?
C4" C5" C6" 103(2) . . ?
C4" C5" H5"A 111.1 . . ?
C6" C5" H5"A 111.1 . . ?
C4" C5" H5"B 111.1 . . ?
C6" C5" H5"B 111.1 . . ?
H5"A C5" H5"B 109.1 . . ?
C7" C6" C5" 102.4(18) . . ?
C7" C6" H6"A 111.3 . . ?
C5" C6" H6"A 111.3 . . ?
C7" C6" H6"B 111.3 . . ?
C5" C6" H6"B 111.3 . . ?
H6"A C6" H6"B 109.2 . . ?
C8" C7" C6" 117.3(12) . . ?
C8" C7" H7"A 108.0 . . ?
C6" C7" H7"A 108.0 . . ?
C8" C7" H7"B 108.0 . . ?
C6" C7" H7"B 108.0 . . ?
H7"A C7" H7"B 107.2 . . ?
C7" C8" C1 118.2(12) . . ?
C7" C8" H8"A 107.8 . . ?
C1 C8" H8"A 107.8 . . ?
C7" C8" H8"B 107.8 . . ?
C1 C8" H8"B 107.8 . . ?
H8"A C8" H8"B 107.1 . . ?
C14 C9 C10 118.8(18) . . ?
C14 C9 P1 121.0(15) . . ?
C10 C9 P1 120.2(18) . . ?
C11 C10 C9 121.0(17) . . ?
C11 C10 H10 119.5 . . ?
C9 C10 H10 119.5 . . ?
C12 C11 C10 120.1(14) . . ?
C12 C11 H11 119.9 . . ?
C10 C11 H11 119.9 . . ?
C11 C12 C13 121.1(14) . . ?
C11 C12 H12 119.4 . . ?
C13 C12 H12 119.4 . . ?
C14 C13 C12 119.7(16) . . ?
C14 C13 H13 120.1 . . ?
C12 C13 H13 120.1 . . ?
C9 C14 C13 119.0(14) . . ?
C9 C14 H14 120.5 . . ?
C13 C14 H14 120.5 . . ?
C10' C9' C14' 120(2) . . ?
C10' C9' P1 116(2) . . ?
C14' C9' P1 123.7(19) . . ?
C9' C10' C11' 119(2) . . ?
C9' C10' H10' 120.5 . . ?
C11' C10' H10' 120.5 . . ?
C10' C11' C12' 120.5(17) . . ?
C10' C11' H11' 119.8 . . ?
C12' C11' H11' 119.8 . . ?
C13' C12' C11' 118.7(18) . . ?
C13' C12' H12' 120.6 . . ?
C11' C12' H12' 120.6 . . ?
C12' C13' C14' 120(2) . . ?
C12' C13' H13' 120.1 . . ?
C14' C13' H13' 120.1 . . ?
C13' C14' C9' 122.2(17) . . ?
C13' C14' H14' 118.9 . . ?
C9' C14' H14' 118.9 . . ?
C20 C15 C16 119.4(4) . . ?
C20 C15 P1 123.3(4) . . ?
C16 C15 P1 117.3(3) . . ?
C17 C16 C15 120.3(5) . . ?
C17 C16 H16 119.8 . . ?
C15 C16 H16 119.8 . . ?
C26 C21 C22 119.3(4) . . ?
C26 C21 P1 119.0(3) . . ?
C22 C21 P1 121.6(4) . . ?
C15 C20 C19 119.6(5) . . ?
C15 C20 H20 120.2 . . ?
C19 C20 H20 120.2 . . ?
C18 C19 C20 120.2(5) . . ?
C18 C19 H19 119.9 . . ?
C20 C19 H19 119.9 . . ?
C17 C18 C19 120.4(4) . . ?
C17 C18 H18 119.8 . . ?
C19 C18 H18 119.8 . . ?
C18 C17 C16 120.1(5) . . ?
C18 C17 H17 119.9 . . ?
C16 C17 H17 119.9 . . ?
C23 C22 C21 120.0(5) . . ?
C23 C22 H22 120.0 . . ?
C21 C22 H22 120.0 . . ?
C22 C23 C24 120.5(4) . . ?
C22 C23 H23 119.8 . . ?
C24 C23 H23 119.8 . . ?
C23 C24 C25 120.2(5) . . ?
C23 C24 H24 119.9 . . ?
C25 C24 H24 119.9 . . ?
C24 C25 C26 119.8(5) . . ?
C24 C25 H25 120.1 . . ?
C26 C25 H25 120.1 . . ?
C21 C26 C25 120.1(4) . . ?
C21 C26 H26 119.9 . . ?
C25 C26 H26 119.9 . . ?

_refine_diff_density_max         2.544
_refine_diff_density_min         -1.604
_refine_diff_density_rms         0.160




_publcif_funding_html            
;
;
####################################################################### 
# 
# 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_shen16
_database_code_depnum_ccdc_archive 'CCDC 2068056'
loop_
_audit_author_name
_audit_author_address
'Khalil Abboud'
;University of Florida
United States of America
;
_audit_update_record             
;
2021-03-04 deposited with the CCDC.	2021-08-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C9 H27 N3 P2 Pt'
_chemical_formula_weight         434.36

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

_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. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   13.7352(9)
_cell_length_b                   11.7608(7)
_cell_length_c                   19.1917(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3100.2(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9372
_cell_measurement_theta_min      3.60
_cell_measurement_theta_max      30.50

_exptl_crystal_description       block
_exptl_crystal_colour            colourless

_exptl_crystal_density_meas      .

_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.861
_exptl_crystal_F_000             1680

_exptl_transmission_factor_min   0.3159
_exptl_transmission_factor_max   0.5644

_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.093
_exptl_absorpt_coefficient_mu    9.238
_shelx_estimated_absorpt_T_min   0.303
_shelx_estimated_absorpt_T_max   0.480

_exptl_absorpt_correction_type   multi-scan

_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?

_exptl_absorpt_process_details   
'Sheldrick, G. M., sadabs (2015). Acta Cryst. C71, 3-8.'

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro source 3.0'
_diffrn_measurement_device_type  'D8 Venture with PHOTON III'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?

_diffrn_reflns_number            51254
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_av_R_equivalents  0.0647
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.122
_diffrn_reflns_theta_max         30.529
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.988
_reflns_number_total             4710
_reflns_number_gt                4398
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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. 
;

_computing_data_collection       'Bruker APEX3 (Bruker, 2014)'
_computing_cell_refinement       'Bruker APEX3 (Bruker, 2014)'
_computing_data_reduction        'Bruker Apex3 SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXL2015, Sheldrick G. M. 2015'
_computing_structure_refinement  'SHELXL2015, Sheldrick G. M. 2015'
_computing_molecular_graphics    'XP in SHELXTL-plus, Bruker 2014'
_computing_publication_material  'SHELXL2015, Sheldrick, G. M. 2015'

_refine_special_details          
;
All H atoms were positioned geometrically ( C---H = 0.93/1.00 Å) and   
allowed to ride with Uiso(H)= 1.2/1.5Ueq(C).
Methyl ones were allowed to rotate around the corresponding C---C.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0047P)²+2.3196P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap

_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4710
_refine_ls_number_parameters     145
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0237
_refine_ls_R_factor_gt           0.0219
_refine_ls_wR_factor_ref         0.0485
_refine_ls_wR_factor_gt          0.0478
_refine_ls_goodness_of_fit_ref   1.200
_refine_ls_restrained_S_all      1.200
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000

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
Pt1 Pt 0.46346(2) 0.77073(2) 0.61054(2) 0.01192(4) Uani 1 1 d . . . . .
C1 C 0.48479(18) 0.7111(2) 0.43271(13) 0.0230(5) Uani 1 1 d . . . . .
H1A H 0.511231 0.786018 0.420782 0.034 Uiso 1 1 calc R U . . .
H1B H 0.454529 0.677256 0.391383 0.034 Uiso 1 1 calc R U . . .
H1C H 0.537522 0.661792 0.449137 0.034 Uiso 1 1 calc R U . . .
P1 P 0.39406(4) 0.72645(4) 0.50104(3) 0.01314(10) Uani 1 1 d . . . . .
N1 N 0.54245(14) 0.61263(19) 0.59492(11) 0.0215(4) Uani 1 1 d . . . . .
N2 N 0.59119(14) 0.57278(15) 0.64085(10) 0.0177(3) Uani 1 1 d . . . . .
C3 C 0.33260(16) 0.59019(17) 0.49372(11) 0.0175(4) Uani 1 1 d . . . . .
H3A H 0.276074 0.589026 0.524871 0.026 Uiso 1 1 calc R U . . .
H3B H 0.377604 0.529151 0.506785 0.026 Uiso 1 1 calc R U . . .
H3C H 0.310965 0.578903 0.445554 0.026 Uiso 1 1 calc R U . . .
P2 P 0.34156(4) 0.68345(5) 0.67828(3) 0.01432(10) Uani 1 1 d . . . . .
N3 N 0.63902(17) 0.5302(2) 0.68325(12) 0.0319(5) Uani 1 1 d . . . . .
C2 C 0.30797(16) 0.82824(19) 0.46509(12) 0.0198(4) Uani 1 1 d . . . . .
H2A H 0.339657 0.902491 0.460303 0.030 Uiso 1 1 calc R U . . .
H2B H 0.251856 0.835108 0.496355 0.030 Uiso 1 1 calc R U . . .
H2C H 0.285991 0.801989 0.419253 0.030 Uiso 1 1 calc R U . . .
C9 C 0.39491(18) 0.92643(19) 0.62314(13) 0.0214(4) Uani 1 1 d . . . . .
H9A H 0.333749 0.926816 0.596845 0.032 Uiso 1 1 calc R U . . .
H9B H 0.437428 0.987126 0.605880 0.032 Uiso 1 1 calc R U . . .
H9C H 0.381149 0.938942 0.672657 0.032 Uiso 1 1 calc R U . . .
C8 C 0.57384(17) 0.8600(2) 0.55751(14) 0.0256(5) Uani 1 1 d . . . . .
H8A H 0.622260 0.806105 0.539783 0.038 Uiso 1 1 calc R U . . .
H8B H 0.605329 0.913421 0.589598 0.038 Uiso 1 1 calc R U . . .
H8C H 0.545291 0.902156 0.518468 0.038 Uiso 1 1 calc R U . . .
C7 C 0.54011(16) 0.8044(2) 0.70277(14) 0.0249(5) Uani 1 1 d . . . . .
H7A H 0.547314 0.733927 0.729531 0.037 Uiso 1 1 calc R U . . .
H7B H 0.504204 0.860332 0.730559 0.037 Uiso 1 1 calc R U . . .
H7C H 0.604635 0.834659 0.691322 0.037 Uiso 1 1 calc R U . . .
C6 C 0.3369(2) 0.7256(2) 0.76926(13) 0.0322(6) Uani 1 1 d . . . . .
H6A H 0.328308 0.808145 0.772381 0.048 Uiso 1 1 calc R U . . .
H6B H 0.397796 0.703884 0.792329 0.048 Uiso 1 1 calc R U . . .
H6C H 0.282135 0.687453 0.792162 0.048 Uiso 1 1 calc R U . . .
C5 C 0.21578(16) 0.70876(19) 0.65244(12) 0.0195(4) Uani 1 1 d . . . . .
H5A H 0.207030 0.686690 0.603604 0.029 Uiso 1 1 calc R U . . .
H5B H 0.200438 0.789651 0.657919 0.029 Uiso 1 1 calc R U . . .
H5C H 0.172214 0.663568 0.681910 0.029 Uiso 1 1 calc R U . . .
C4 C 0.35155(17) 0.52986(19) 0.68456(13) 0.0235(5) Uani 1 1 d . . . . .
H4A H 0.344313 0.496251 0.638120 0.035 Uiso 1 1 calc R U . . .
H4B H 0.300311 0.500741 0.715283 0.035 Uiso 1 1 calc R U . . .
H4C H 0.415431 0.509693 0.703655 0.035 Uiso 1 1 calc R U . . .


_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
Pt1 C9 2.073(2) . ?
Pt1 C7 2.097(2) . ?
Pt1 C8 2.107(2) . ?
Pt1 N1 2.174(2) . ?
Pt1 P2 2.3552(5) . ?
Pt1 P1 2.3657(6) . ?
C1 P1 1.818(2) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
P1 C3 1.817(2) . ?
P1 C2 1.819(2) . ?
N1 N2 1.202(3) . ?
N2 N3 1.159(3) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
P2 C4 1.816(2) . ?
P2 C6 1.816(3) . ?
P2 C5 1.822(2) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?

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
C9 Pt1 C7 87.87(10) . . ?
C9 Pt1 C8 86.72(10) . . ?
C7 Pt1 C8 87.27(11) . . ?
C9 Pt1 N1 176.73(9) . . ?
C7 Pt1 N1 91.57(9) . . ?
C8 Pt1 N1 90.03(9) . . ?
C9 Pt1 P2 89.87(7) . . ?
C7 Pt1 P2 88.47(8) . . ?
C8 Pt1 P2 174.64(7) . . ?
N1 Pt1 P2 93.34(6) . . ?
C9 Pt1 P1 96.61(7) . . ?
C7 Pt1 P1 173.52(7) . . ?
C8 Pt1 P1 88.31(7) . . ?
N1 Pt1 P1 83.70(5) . . ?
P2 Pt1 P1 96.199(19) . . ?
P1 C1 H1A 109.5 . . ?
P1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
P1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 P1 C1 100.09(11) . . ?
C3 P1 C2 104.43(10) . . ?
C1 P1 C2 103.74(11) . . ?
C3 P1 Pt1 116.75(7) . . ?
C1 P1 Pt1 112.73(9) . . ?
C2 P1 Pt1 117.00(8) . . ?
N2 N1 Pt1 120.69(16) . . ?
N3 N2 N1 177.0(2) . . ?
P1 C3 H3A 109.5 . . ?
P1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
P1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C4 P2 C6 102.14(12) . . ?
C4 P2 C5 104.61(11) . . ?
C6 P2 C5 100.59(13) . . ?
C4 P2 Pt1 114.61(8) . . ?
C6 P2 Pt1 115.90(9) . . ?
C5 P2 Pt1 116.91(8) . . ?
P1 C2 H2A 109.5 . . ?
P1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
P1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Pt1 C9 H9A 109.5 . . ?
Pt1 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
Pt1 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
Pt1 C8 H8A 109.5 . . ?
Pt1 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
Pt1 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Pt1 C7 H7A 109.5 . . ?
Pt1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Pt1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
P2 C6 H6A 109.5 . . ?
P2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
P2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
P2 C5 H5A 109.5 . . ?
P2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
P2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
P2 C4 H4A 109.5 . . ?
P2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
P2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?

_refine_diff_density_max         1.175
_refine_diff_density_min         -1.577
_refine_diff_density_rms         0.194

####################################################################### 
# 
# 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_shen10
_database_code_depnum_ccdc_archive 'CCDC 2068054'
loop_
_audit_author_name
_audit_author_address
'Khalil Abboud'
;University of Florida
United States of America
;
# end Validation Reply Form

_audit_update_record             
;
2021-03-04 deposited with the CCDC.	2021-08-09 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT213_shen10              
;
PROBLEM: Atom C18? has ADP max/min Ratio ..... 6.8 oblate
RESPONSE: Atom C18' is the minor part of the disorder that did not refine
 better.
;
# publcif _publ_body_element loop end

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '(C23 H25 N5 O2 W), C3 H6 O1'
_chemical_formula_sum            'C26 H31 N5 O3 W'
_chemical_formula_weight         645.41

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   13.915(3)
_cell_length_b                   11.0476(18)
_cell_length_c                   16.410(4)
_cell_angle_alpha                90
_cell_angle_beta                 96.897(6)
_cell_angle_gamma                90
_cell_volume                     2504.4(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    458
_cell_measurement_theta_min      2.50
_cell_measurement_theta_max      19.48

_exptl_crystal_description       needle
_exptl_crystal_colour            red
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.712
_exptl_crystal_F_000             1280
_exptl_transmission_factor_min   0.3737
_exptl_transmission_factor_max   0.4951
_exptl_crystal_size_max          0.182
_exptl_crystal_size_mid          0.092
_exptl_crystal_size_min          0.043
_exptl_absorpt_coefficient_mu    4.650
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5049
_exptl_absorpt_correction_T_max  0.6263
_exptl_absorpt_process_details   
'Sheldrick, G. M., sadabs (2015). Acta Cryst. C71, 3-8.'

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro source 3.0'
_diffrn_measurement_device_type  'D8 Venture with PHOTON III'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?

_diffrn_reflns_number            115078
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_av_R_equivalents  0.0596
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.815
_diffrn_reflns_theta_max         32.763
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8864
_reflns_number_gt                7990
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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. 
;

_computing_data_collection       'Bruker APEX3 (Bruker, 2014)'
_computing_cell_refinement       'Bruker APEX3 (Bruker, 2014)'
_computing_data_reduction        'Bruker Apex3 SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXL2015, Sheldrick G. M. 2015'
_computing_structure_refinement  'SHELXL2015, Sheldrick G. M. 2015'
_computing_molecular_graphics    'XP in SHELXTL-plus, Bruker 2014'
_computing_publication_material  'SHELXL2015, Sheldrick, G. M. 2015'

_refine_special_details          
;
All H atoms were positioned geometrically ( C---H = 0.93/1.00 Å) and   
allowed to ride with Uiso(H)= 1.2/1.5Ueq(C).
Methyl ones were allowed to rotate around the corresponding C---C.

he asymmetric unit consists of the W complex and an acetone solvent molecule. 
 The complex has its oxygen atoms of the carbonyl groups disordered.  The bipy
 group is disordered and refined in two parts. The group of C3-C8 is also
 disordered and similarly refined in two parts.  Finally, the acetone solvent
 molecule is also disordered and refined in two parts.  The structure exhibits
 all atoms refined anisotropically.

;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0044P)²+5.7482P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8864
_refine_ls_number_parameters     443
_refine_ls_number_restraints     1160
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0292
_refine_ls_wR_factor_ref         0.0585
_refine_ls_wR_factor_gt          0.0570
_refine_ls_goodness_of_fit_ref   1.208
_refine_ls_restrained_S_all      1.138
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

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
W1 W 0.47054(2) 0.66423(2) 0.82044(2) 0.01681(3) Uani 1 1 d . U . . .
N1 N 0.42875(19) 0.7095(2) 0.63329(14) 0.0230(5) Uani 1 1 d . U . . .
N2 N 0.40888(17) 0.6357(2) 0.69507(13) 0.0202(4) Uani 1 1 d . U . . .
N3 N 0.34409(19) 0.5499(2) 0.66869(14) 0.0250(5) Uani 1 1 d . U . . .
C1 C 0.3742(2) 0.6700(2) 0.56564(16) 0.0224(5) Uani 1 1 d . U . . .
C2 C 0.3212(2) 0.5690(3) 0.58789(17) 0.0251(5) Uani 1 1 d . U . . .
C3 C 0.2484(2) 0.4873(3) 0.53889(18) 0.0335(7) Uani 1 1 d D U . . .
H3A H 0.192475 0.475902 0.570153 0.040 Uiso 0.930(9) 1 calc R U P A 1
H3B H 0.278565 0.406967 0.533466 0.040 Uiso 0.930(9) 1 calc R U P A 1
H3C H 0.184697 0.514878 0.552881 0.040 Uiso 0.070(9) 1 calc R U P A 2
H3D H 0.259058 0.406570 0.564634 0.040 Uiso 0.070(9) 1 calc R U P A 2
C4 C 0.2111(3) 0.5334(4) 0.45333(18) 0.0348(10) Uani 0.930(9) 1 d D U P A 1
H4A H 0.200975 0.621947 0.456340 0.042 Uiso 0.930(9) 1 calc R U P A 1
H4B H 0.147419 0.495741 0.435881 0.042 Uiso 0.930(9) 1 calc R U P A 1
C5 C 0.2780(2) 0.5080(6) 0.3879(3) 0.0362(12) Uani 0.930(9) 1 d D U P A 1
H5A H 0.267443 0.423076 0.369778 0.043 Uiso 0.930(9) 1 calc R U P A 1
H5B H 0.257115 0.560205 0.340042 0.043 Uiso 0.930(9) 1 calc R U P A 1
C4' C 0.232(3) 0.462(4) 0.4470(6) 0.033(6) Uani 0.070(9) 1 d D U P A 2
H4'A H 0.161147 0.467305 0.431037 0.040 Uiso 0.070(9) 1 calc R U P A 2
H4'B H 0.249588 0.375981 0.440242 0.040 Uiso 0.070(9) 1 calc R U P A 2
C5' C 0.2784(8) 0.532(8) 0.382(4) 0.033(7) Uani 0.070(9) 1 d D U P A 2
H5'A H 0.255508 0.616892 0.378554 0.040 Uiso 0.070(9) 1 calc R U P A 2
H5'B H 0.263391 0.493773 0.327146 0.040 Uiso 0.070(9) 1 calc R U P A 2
C6 C 0.3868(2) 0.5262(3) 0.41062(18) 0.0316(6) Uani 1 1 d D U . . .
H6A H 0.406517 0.482647 0.462685 0.038 Uiso 0.930(9) 1 calc R U P A 1
H6B H 0.420528 0.487275 0.367710 0.038 Uiso 0.930(9) 1 calc R U P A 1
H6C H 0.398665 0.482334 0.463492 0.038 Uiso 0.070(9) 1 calc R U P A 2
H6D H 0.421029 0.483333 0.369635 0.038 Uiso 0.070(9) 1 calc R U P A 2
C7 C 0.4226(2) 0.6560(3) 0.42078(18) 0.0321(6) Uani 1 1 d . U . . .
H7A H 0.410488 0.697090 0.366892 0.038 Uiso 1 1 calc R U . . .
H7B H 0.493508 0.654531 0.436649 0.038 Uiso 1 1 calc R U . . .
C8 C 0.3761(2) 0.7324(3) 0.48470(17) 0.0271(6) Uani 1 1 d . U . . .
H8A H 0.412479 0.809178 0.493879 0.033 Uiso 1 1 calc R U . . .
H8B H 0.308925 0.752924 0.461983 0.033 Uiso 1 1 calc R U . . .
N4 N 0.4435(2) 0.46483(17) 0.8279(2) 0.0188(7) Uani 0.783(8) 1 d G U P B 1
C9 C 0.5157(2) 0.3802(2) 0.8198(2) 0.0223(8) Uani 0.783(8) 1 d G U P B 1
H9A H 0.577679 0.406074 0.808232 0.027 Uiso 0.783(8) 1 calc R U P B 1
C10 C 0.4970(3) 0.2575(2) 0.82869(19) 0.0303(10) Uani 0.783(8) 1 d G U P B 1
H10A H 0.546323 0.199672 0.823158 0.036 Uiso 0.783(8) 1 calc R U P B 1
C11 C 0.4063(3) 0.21962(18) 0.84566(19) 0.0323(10) Uani 0.783(8) 1 d G U P B 1
H11A H 0.393551 0.135824 0.851719 0.039 Uiso 0.783(8) 1 calc R U P B 1
C12 C 0.3342(3) 0.3043(2) 0.85376(19) 0.0294(9) Uani 0.783(8) 1 d G U P B 1
H12A H 0.272133 0.278378 0.865354 0.035 Uiso 0.783(8) 1 calc R U P B 1
C13 C 0.3528(2) 0.4269(2) 0.8449(2) 0.0209(8) Uani 0.783(8) 1 d G U P B 1
N5 N 0.31471(17) 0.6370(3) 0.8383(3) 0.0190(8) Uani 0.783(8) 1 d G U P B 1
C14 C 0.2824(2) 0.5197(2) 0.8492(2) 0.0197(7) Uani 0.783(8) 1 d G U P B 1
C15 C 0.1861(2) 0.4991(3) 0.85944(18) 0.0263(9) Uani 0.783(8) 1 d G U P B 1
H15A H 0.163978 0.418931 0.866866 0.032 Uiso 0.783(8) 1 calc R U P B 1
C16 C 0.12202(18) 0.5957(4) 0.85887(19) 0.0308(10) Uani 0.783(8) 1 d G U P B 1
H16A H 0.056176 0.581633 0.865897 0.037 Uiso 0.783(8) 1 calc R U P B 1
C17 C 0.1543(2) 0.7130(3) 0.8480(2) 0.0277(9) Uani 0.783(8) 1 d G U P B 1
H17A H 0.110565 0.779082 0.847614 0.033 Uiso 0.783(8) 1 calc R U P B 1
C18 C 0.2507(2) 0.7337(2) 0.8377(3) 0.0241(9) Uani 0.783(8) 1 d G U P B 1
H18 H 0.272756 0.813831 0.830299 0.029 Uiso 0.783(8) 1 calc R U P B 1
N4' N 0.4735(9) 0.4627(7) 0.8217(9) 0.023(3) Uani 0.217(8) 1 d G U P B 2
C9' C 0.5537(9) 0.3922(10) 0.8111(9) 0.033(3) Uani 0.217(8) 1 d G U P B 2
H9'A H 0.611069 0.429196 0.796951 0.039 Uiso 0.217(8) 1 calc R U P B 2
C10' C 0.5501(11) 0.2674(9) 0.8212(8) 0.039(4) Uani 0.217(8) 1 d G U P B 2
H10B H 0.604963 0.219158 0.814002 0.047 Uiso 0.217(8) 1 calc R U P B 2
C11' C 0.4662(13) 0.2132(7) 0.8419(7) 0.040(4) Uani 0.217(8) 1 d G U P B 2
H11B H 0.463731 0.127920 0.848869 0.048 Uiso 0.217(8) 1 calc R U P B 2
C12' C 0.3859(11) 0.2838(10) 0.8525(7) 0.036(3) Uani 0.217(8) 1 d G U P B 2
H12B H 0.328602 0.246719 0.866685 0.043 Uiso 0.217(8) 1 calc R U P B 2
C13' C 0.3896(9) 0.4085(9) 0.8424(7) 0.017(2) Uani 0.217(8) 1 d G U P B 2
N5' N 0.3306(6) 0.6098(11) 0.8432(9) 0.022(2) Uani 0.217(8) 1 d G U P B 2
C14' C 0.3129(8) 0.4869(10) 0.8519(8) 0.025(3) Uani 0.217(8) 1 d G U P B 2
C15' C 0.2205(9) 0.4470(12) 0.8626(7) 0.037(3) Uani 0.217(8) 1 d G U P B 2
H15B H 0.208408 0.363054 0.868585 0.044 Uiso 0.217(8) 1 calc R U P B 2
C16' C 0.1458(7) 0.5301(16) 0.8647(7) 0.036(4) Uani 0.217(8) 1 d G U P B 2
H16B H 0.082615 0.502835 0.872033 0.044 Uiso 0.217(8) 1 calc R U P B 2
C17' C 0.1634(6) 0.6530(14) 0.8560(7) 0.034(3) Uani 0.217(8) 1 d G U P B 2
H17B H 0.112362 0.709699 0.857414 0.041 Uiso 0.217(8) 1 calc R U P B 2
C18' C 0.2558(7) 0.6928(11) 0.8453(8) 0.013(2) Uani 0.217(8) 1 d G U P B 2
H18' H 0.267902 0.776783 0.839347 0.016 Uiso 0.217(8) 1 calc R U P B 2
C19 C 0.5902(2) 0.6216(3) 0.92798(17) 0.0226(5) Uani 1 1 d . U . . .
H19A H 0.624307 0.682972 0.902770 0.027 Uiso 1 1 calc R U . . .
H19B H 0.616440 0.542302 0.934246 0.027 Uiso 1 1 calc R U . . .
C20 C 0.5002(2) 0.6484(2) 0.95624(15) 0.0209(5) Uani 1 1 d . U . . .
H20A H 0.464294 0.589257 0.981704 0.025 Uiso 1 1 calc R U . . .
C21 C 0.4675(2) 0.7690(3) 0.94406(16) 0.0225(5) Uani 1 1 d . U . . .
H21A H 0.505239 0.825911 0.918374 0.027 Uiso 1 1 calc R U . . .
H21B H 0.407697 0.793052 0.961569 0.027 Uiso 1 1 calc R U . . .
O1 O 0.48074(18) 0.94346(19) 0.79174(15) 0.0345(5) Uani 1 1 d . U . . .
O2 O 0.6697(16) 0.703(3) 0.752(2) 0.021(3) Uani 0.42(14) 1 d D U P C 1
O2' O 0.6765(9) 0.715(3) 0.769(3) 0.028(3) Uani 0.58(14) 1 d D U P C 2
C22 C 0.4743(2) 0.8391(2) 0.80121(17) 0.0229(5) Uani 1 1 d . U . . .
C23 C 0.5982(2) 0.6885(2) 0.78260(17) 0.0238(5) Uani 1 1 d D U . . .
O81 O 0.2813(4) 0.6465(6) 0.0819(5) 0.061(2) Uani 0.491(5) 1 d . U P D 1
C82 C 0.1144(5) 0.6812(6) 0.0562(4) 0.0280(13) Uani 0.491(5) 1 d . U P D 1
H82A H 0.056509 0.645967 0.075417 0.042 Uiso 0.491(5) 1 calc R U P D 1
H82B H 0.118162 0.767421 0.070239 0.042 Uiso 0.491(5) 1 calc R U P D 1
H82C H 0.110818 0.671687 -0.003437 0.042 Uiso 0.491(5) 1 calc R U P D 1
C83 C 0.2014(5) 0.6186(6) 0.0961(5) 0.0318(14) Uani 0.491(5) 1 d . U P D 1
C84 C 0.1853(10) 0.5142(12) 0.1523(8) 0.051(3) Uani 0.491(5) 1 d . U P D 1
H84A H 0.115896 0.505593 0.156191 0.076 Uiso 0.491(5) 1 calc R U P D 1
H84B H 0.209937 0.439491 0.130227 0.076 Uiso 0.491(5) 1 calc R U P D 1
H84C H 0.219616 0.529831 0.207011 0.076 Uiso 0.491(5) 1 calc R U P D 1
O91 O 0.0531(3) 0.5284(4) 0.0373(3) 0.0325(11) Uani 0.509(5) 1 d . U P D 2
C92 C 0.1688(7) 0.6798(7) 0.0729(5) 0.0403(18) Uani 0.509(5) 1 d . U P D 2
H92A H 0.220105 0.693386 0.118264 0.060 Uiso 0.509(5) 1 calc R U P D 2
H92B H 0.197070 0.676385 0.021030 0.060 Uiso 0.509(5) 1 calc R U P D 2
H92C H 0.121890 0.746268 0.070749 0.060 Uiso 0.509(5) 1 calc R U P D 2
C93 C 0.1190(4) 0.5634(5) 0.0858(3) 0.0241(11) Uani 0.509(5) 1 d . U P D 2
C94 C 0.1533(6) 0.4959(12) 0.1628(7) 0.0330(19) Uani 0.509(5) 1 d . U P D 2
H94A H 0.207286 0.539763 0.193428 0.049 Uiso 0.509(5) 1 calc R U P D 2
H94B H 0.100200 0.488668 0.196693 0.049 Uiso 0.509(5) 1 calc R U P D 2
H94C H 0.175009 0.414910 0.148823 0.049 Uiso 0.509(5) 1 calc R U P D 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
W1 C22 1.959(3) . ?
W1 C23 1.969(3) . ?
W1 N5' 2.115(7) . ?
W1 N2 2.155(2) . ?
W1 C20 2.224(3) . ?
W1 N4' 2.227(7) . ?
W1 N4 2.2405(19) . ?
W1 N5 2.243(2) . ?
W1 C19 2.325(3) . ?
W1 C21 2.340(3) . ?
N1 C1 1.340(4) . ?
N1 N2 1.355(3) . ?
N2 N3 1.343(3) . ?
N3 C2 1.342(4) . ?
C1 C2 1.409(4) . ?
C1 C8 1.499(4) . ?
C2 C3 1.514(4) . ?
C3 C4' 1.524(5) . ?
C3 C4 1.525(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 H3C 0.9900 . ?
C3 H3D 0.9900 . ?
C4 C5 1.529(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.528(4) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C4' C5' 1.526(5) . ?
C4' H4'A 0.9900 . ?
C4' H4'B 0.9900 . ?
C5' C6 1.526(5) . ?
C5' H5'A 0.9900 . ?
C5' H5'B 0.9900 . ?
C6 C7 1.522(5) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 H6C 0.9900 . ?
C6 H6D 0.9900 . ?
C7 C8 1.547(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
N4 C9 1.3900 . ?
N4 C13 1.3900 . ?
C9 C10 1.3900 . ?
C9 H9A 0.9500 . ?
C10 C11 1.3900 . ?
C10 H10A 0.9500 . ?
C11 C12 1.3900 . ?
C11 H11A 0.9500 . ?
C12 C13 1.3900 . ?
C12 H12A 0.9500 . ?
C13 C14 1.425(3) . ?
N5 C14 1.3900 . ?
N5 C18 1.3900 . ?
C14 C15 1.3900 . ?
C15 C16 1.3900 . ?
C15 H15A 0.9500 . ?
C16 C17 1.3900 . ?
C16 H16A 0.9500 . ?
C17 C18 1.3900 . ?
C17 H17A 0.9500 . ?
C18 H18 0.9500 . ?
N4' C9' 1.3900 . ?
N4' C13' 1.3900 . ?
C9' C10' 1.3900 . ?
C9' H9'A 0.9500 . ?
C10' C11' 1.3900 . ?
C10' H10B 0.9500 . ?
C11' C12' 1.3900 . ?
C11' H11B 0.9500 . ?
C12' C13' 1.3900 . ?
C12' H12B 0.9500 . ?
C13' C14' 1.397(12) . ?
N5' C14' 1.3900 . ?
N5' C18' 1.3900 . ?
C14' C15' 1.3900 . ?
C15' C16' 1.3900 . ?
C15' H15B 0.9500 . ?
C16' C17' 1.3900 . ?
C16' H16B 0.9500 . ?
C17' C18' 1.3900 . ?
C17' H17B 0.9500 . ?
C18' H18' 0.9500 . ?
C19 C20 1.418(4) . ?
C19 H19A 0.9500 . ?
C19 H19B 0.9500 . ?
C20 C21 1.414(4) . ?
C20 H20A 0.9500 . ?
C21 H21A 0.9500 . ?
C21 H21B 0.9500 . ?
O1 C22 1.168(3) . ?
O2 C23 1.176(5) . ?
O2' C23 1.176(5) . ?
O81 C83 1.203(9) . ?
C82 C83 1.477(9) . ?
C82 H82A 0.9800 . ?
C82 H82B 0.9800 . ?
C82 H82C 0.9800 . ?
C83 C84 1.510(14) . ?
C84 H84A 0.9800 . ?
C84 H84B 0.9800 . ?
C84 H84C 0.9800 . ?
O91 C93 1.204(7) . ?
C92 C93 1.487(9) . ?
C92 H92A 0.9800 . ?
C92 H92B 0.9800 . ?
C92 H92C 0.9800 . ?
C93 C94 1.496(11) . ?
C94 H94A 0.9800 . ?
C94 H94B 0.9800 . ?
C94 H94C 0.9800 . ?

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
C22 W1 C23 76.86(11) . . ?
C22 W1 N5' 110.6(3) . . ?
C23 W1 N5' 168.4(4) . . ?
C22 W1 N2 90.33(10) . . ?
C23 W1 N2 89.40(11) . . ?
N5' W1 N2 81.8(4) . . ?
C22 W1 C20 103.49(11) . . ?
C23 W1 C20 105.10(11) . . ?
N5' W1 C20 82.2(4) . . ?
N2 W1 C20 161.79(9) . . ?
C22 W1 N4' 170.6(3) . . ?
C23 W1 N4' 97.0(3) . . ?
N5' W1 N4' 74.3(4) . . ?
N2 W1 N4' 82.4(4) . . ?
C20 W1 N4' 84.9(4) . . ?
C22 W1 N4 170.47(12) . . ?
C23 W1 N4 108.33(11) . . ?
N2 W1 N4 81.86(11) . . ?
C20 W1 N4 83.12(12) . . ?
C22 W1 N5 101.43(11) . . ?
C23 W1 N5 169.20(14) . . ?
N2 W1 N5 79.91(13) . . ?
C20 W1 N5 85.69(13) . . ?
N4 W1 N5 71.94(9) . . ?
C22 W1 C19 106.94(11) . . ?
C23 W1 C19 71.08(11) . . ?
N5' W1 C19 113.5(4) . . ?
N2 W1 C19 149.53(9) . . ?
C20 W1 C19 36.24(10) . . ?
N4' W1 C19 77.3(4) . . ?
N4 W1 C19 82.47(11) . . ?
N5 W1 C19 119.30(12) . . ?
C22 W1 C21 69.85(11) . . ?
C23 W1 C21 108.49(11) . . ?
N5' W1 C21 82.8(4) . . ?
N2 W1 C21 148.56(9) . . ?
C20 W1 C21 35.98(10) . . ?
N4' W1 C21 119.3(4) . . ?
N4 W1 C21 114.71(12) . . ?
N5 W1 C21 80.47(13) . . ?
C19 W1 C21 61.84(10) . . ?
C1 N1 N2 106.1(2) . . ?
N3 N2 N1 111.9(2) . . ?
N3 N2 W1 125.85(17) . . ?
N1 N2 W1 122.20(18) . . ?
C2 N3 N2 106.2(2) . . ?
N1 C1 C2 107.7(2) . . ?
N1 C1 C8 121.0(3) . . ?
C2 C1 C8 131.2(3) . . ?
N3 C2 C1 108.1(3) . . ?
N3 C2 C3 119.7(3) . . ?
C1 C2 C3 132.2(3) . . ?
C2 C3 C4' 130.3(18) . . ?
C2 C3 C4 114.9(3) . . ?
C2 C3 H3A 108.5 . . ?
C4 C3 H3A 108.5 . . ?
C2 C3 H3B 108.5 . . ?
C4 C3 H3B 108.5 . . ?
H3A C3 H3B 107.5 . . ?
C2 C3 H3C 104.7 . . ?
C4' C3 H3C 104.7 . . ?
C2 C3 H3D 104.7 . . ?
C4' C3 H3D 104.7 . . ?
H3C C3 H3D 105.7 . . ?
C3 C4 C5 114.6(3) . . ?
C3 C4 H4A 108.6 . . ?
C5 C4 H4A 108.6 . . ?
C3 C4 H4B 108.6 . . ?
C5 C4 H4B 108.6 . . ?
H4A C4 H4B 107.6 . . ?
C6 C5 C4 118.3(4) . . ?
C6 C5 H5A 107.7 . . ?
C4 C5 H5A 107.7 . . ?
C6 C5 H5B 107.7 . . ?
C4 C5 H5B 107.7 . . ?
H5A C5 H5B 107.1 . . ?
C3 C4' C5' 125(4) . . ?
C3 C4' H4'A 106.1 . . ?
C5' C4' H4'A 106.1 . . ?
C3 C4' H4'B 106.1 . . ?
C5' C4' H4'B 106.1 . . ?
H4'A C4' H4'B 106.3 . . ?
C4' C5' C6 104(3) . . ?
C4' C5' H5'A 110.9 . . ?
C6 C5' H5'A 110.9 . . ?
C4' C5' H5'B 110.9 . . ?
C6 C5' H5'B 110.9 . . ?
H5'A C5' H5'B 108.9 . . ?
C7 C6 C5' 107(3) . . ?
C7 C6 C5 116.9(3) . . ?
C7 C6 H6A 108.1 . . ?
C5 C6 H6A 108.1 . . ?
C7 C6 H6B 108.1 . . ?
C5 C6 H6B 108.1 . . ?
H6A C6 H6B 107.3 . . ?
C7 C6 H6C 110.3 . . ?
C5' C6 H6C 110.3 . . ?
C7 C6 H6D 110.3 . . ?
C5' C6 H6D 110.3 . . ?
H6C C6 H6D 108.6 . . ?
C6 C7 C8 115.5(3) . . ?
C6 C7 H7A 108.4 . . ?
C8 C7 H7A 108.4 . . ?
C6 C7 H7B 108.4 . . ?
C8 C7 H7B 108.4 . . ?
H7A C7 H7B 107.5 . . ?
C1 C8 C7 113.8(2) . . ?
C1 C8 H8A 108.8 . . ?
C7 C8 H8A 108.8 . . ?
C1 C8 H8B 108.8 . . ?
C7 C8 H8B 108.8 . . ?
H8A C8 H8B 107.7 . . ?
C9 N4 C13 120.0 . . ?
C9 N4 W1 121.92(13) . . ?
C13 N4 W1 118.02(13) . . ?
N4 C9 C10 120.0 . . ?
N4 C9 H9A 120.0 . . ?
C10 C9 H9A 120.0 . . ?
C11 C10 C9 120.0 . . ?
C11 C10 H10A 120.0 . . ?
C9 C10 H10A 120.0 . . ?
C10 C11 C12 120.0 . . ?
C10 C11 H11A 120.0 . . ?
C12 C11 H11A 120.0 . . ?
C13 C12 C11 120.0 . . ?
C13 C12 H12A 120.0 . . ?
C11 C12 H12A 120.0 . . ?
C12 C13 N4 120.0 . . ?
C12 C13 C14 123.92(19) . . ?
N4 C13 C14 116.04(18) . . ?
C14 N5 C18 120.0 . . ?
C14 N5 W1 118.32(14) . . ?
C18 N5 W1 121.68(14) . . ?
C15 C14 N5 120.0 . . ?
C15 C14 C13 124.49(19) . . ?
N5 C14 C13 115.44(19) . . ?
C14 C15 C16 120.0 . . ?
C14 C15 H15A 120.0 . . ?
C16 C15 H15A 120.0 . . ?
C17 C16 C15 120.0 . . ?
C17 C16 H16A 120.0 . . ?
C15 C16 H16A 120.0 . . ?
C16 C17 C18 120.0 . . ?
C16 C17 H17A 120.0 . . ?
C18 C17 H17A 120.0 . . ?
C17 C18 N5 120.0 . . ?
C17 C18 H18 120.0 . . ?
N5 C18 H18 120.0 . . ?
C9' N4' C13' 120.0 . . ?
C9' N4' W1 125.0(5) . . ?
C13' N4' W1 114.7(5) . . ?
C10' C9' N4' 120.0 . . ?
C10' C9' H9'A 120.0 . . ?
N4' C9' H9'A 120.0 . . ?
C11' C10' C9' 120.0 . . ?
C11' C10' H10B 120.0 . . ?
C9' C10' H10B 120.0 . . ?
C12' C11' C10' 120.0 . . ?
C12' C11' H11B 120.0 . . ?
C10' C11' H11B 120.0 . . ?
C13' C12' C11' 120.0 . . ?
C13' C12' H12B 120.0 . . ?
C11' C12' H12B 120.0 . . ?
C12' C13' N4' 120.0 . . ?
C12' C13' C14' 124.2(8) . . ?
N4' C13' C14' 115.8(8) . . ?
C14' N5' C18' 120.0 . . ?
C14' N5' W1 118.3(5) . . ?
C18' N5' W1 121.6(5) . . ?
N5' C14' C15' 120.0 . . ?
N5' C14' C13' 116.5(8) . . ?
C15' C14' C13' 123.3(8) . . ?
C16' C15' C14' 120.0 . . ?
C16' C15' H15B 120.0 . . ?
C14' C15' H15B 120.0 . . ?
C15' C16' C17' 120.0 . . ?
C15' C16' H16B 120.0 . . ?
C17' C16' H16B 120.0 . . ?
C18' C17' C16' 120.0 . . ?
C18' C17' H17B 120.0 . . ?
C16' C17' H17B 120.0 . . ?
C17' C18' N5' 120.0 . . ?
C17' C18' H18' 120.0 . . ?
N5' C18' H18' 120.0 . . ?
C20 C19 W1 68.01(15) . . ?
C20 C19 H19A 120.0 . . ?
W1 C19 H19A 82.8 . . ?
C20 C19 H19B 120.0 . . ?
W1 C19 H19B 120.0 . . ?
H19A C19 H19B 120.0 . . ?
C21 C20 C19 115.7(2) . . ?
C21 C20 W1 76.50(15) . . ?
C19 C20 W1 75.75(15) . . ?
C21 C20 H20A 122.2 . . ?
C19 C20 H20A 122.2 . . ?
W1 C20 H20A 116.8 . . ?
C20 C21 W1 67.52(14) . . ?
C20 C21 H21A 120.0 . . ?
W1 C21 H21A 82.8 . . ?
C20 C21 H21B 120.0 . . ?
W1 C21 H21B 120.5 . . ?
H21A C21 H21B 120.0 . . ?
O1 C22 W1 176.9(3) . . ?
O2 C23 W1 174(2) . . ?
O2' C23 W1 171(2) . . ?
C83 C82 H82A 109.5 . . ?
C83 C82 H82B 109.5 . . ?
H82A C82 H82B 109.5 . . ?
C83 C82 H82C 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
O81 C83 C82 121.4(8) . . ?
O81 C83 C84 121.5(8) . . ?
C82 C83 C84 117.0(7) . . ?
C83 C84 H84A 109.5 . . ?
C83 C84 H84B 109.5 . . ?
H84A C84 H84B 109.5 . . ?
C83 C84 H84C 109.5 . . ?
H84A C84 H84C 109.5 . . ?
H84B C84 H84C 109.5 . . ?
C93 C92 H92A 109.5 . . ?
C93 C92 H92B 109.5 . . ?
H92A C92 H92B 109.5 . . ?
C93 C92 H92C 109.5 . . ?
H92A C92 H92C 109.5 . . ?
H92B C92 H92C 109.5 . . ?
O91 C93 C92 121.0(6) . . ?
O91 C93 C94 122.6(7) . . ?
C92 C93 C94 116.4(7) . . ?
C93 C94 H94A 109.5 . . ?
C93 C94 H94B 109.5 . . ?
H94A C94 H94B 109.5 . . ?
C93 C94 H94C 109.5 . . ?
H94A C94 H94C 109.5 . . ?
H94B C94 H94C 109.5 . . ?

_refine_diff_density_max         1.149
_refine_diff_density_min         -0.891
_refine_diff_density_rms         0.124




_publcif_funding_html            
;
;
####################################################################### 
# 
# 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_shen18
_database_code_depnum_ccdc_archive 'CCDC 2069850'
loop_
_audit_author_name
_audit_author_address
'Dr. Khalil A. Abboud'
;Unviersity of Florida
United States of America
;
# end Validation Reply Form
_audit_update_record             
;
2021-06-26 deposited with the CCDC.	2021-08-09 downloaded from the CCDC.
;
_audit_creation_date             2021-05-12
# publcif _publ_body_element loop end
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_publcif_funding_html            
;
;

_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C17 N3 P2 Pt'
_chemical_formula_sum            'C17 H39 N3 P2 Pt'
_chemical_formula_weight         542.54
_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'
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'
Pt Pt -1.7033 8.3905 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   7.5376(9)
_cell_length_b                   13.5921(17)
_cell_length_c                   21.634(3)
_cell_angle_alpha                90
_cell_angle_beta                 98.856(4)
_cell_angle_gamma                90
_cell_volume                     2190.0(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9895
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.39
_cell_measurement_theta_min      3.15
_shelx_estimated_absorpt_T_max   0.803
_shelx_estimated_absorpt_T_min   0.499
_exptl_absorpt_coefficient_mu    6.557
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'Sheldrick, G. M., sadabs (2015). Acta Cryst. C71, 3-8.'
_exptl_crystal_colour            gold
_exptl_crystal_density_diffrn    1.646
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.123
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.035
_exptl_transmission_factor_max   0.4952
_exptl_transmission_factor_min   0.2959
_diffrn_reflns_av_R_equivalents  0.0584
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.927
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            58423
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.927
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.844
_diffrn_reflns_theta_min         1.905
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_device_type  'D8 Venture with PHOTON III'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro source 3.0'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6772
_reflns_number_total             7562
_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       'Bruker APEX3 (Bruker, 2014)'
_computing_data_collection       'Bruker APEX3 (Bruker, 2014)'
_computing_data_reduction        'Bruker Apex3 SAINT (Bruker, 2014)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL2015, Sheldrick G. M. 2015'
_computing_structure_solution    'SHELXL2015, Sheldrick G. M. 2015'
_refine_diff_density_max         2.869
_refine_diff_density_min         -3.098
_refine_diff_density_rms         0.722
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.170
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         7562
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0294
_refine_ls_restrained_S_all      1.170
_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/[σ²(Fo²)+(0.0338P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0657
_refine_ls_wR_factor_ref         0.0679
_refine_special_details          
;
All H atoms were positioned geometrically ( C---H = 0.93/1.00 Å) and   
allowed to ride with Uiso(H)= 1.2/1.5Ueq(C).
Methyl ones were allowed to rotate around the corresponding C---C.
;
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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
Pt1 Pt 0.38975(2) 0.26884(2) 0.42527(2) 0.01342(4) Uani 1 1 d . . . . .
P1 P 0.58045(8) 0.37268(5) 0.37523(3) 0.01647(12) Uani 1 1 d . . . . .
P2 P 0.49780(8) 0.11817(5) 0.38927(3) 0.01737(12) Uani 1 1 d . . . . .
N1 N 0.0922(3) 0.19127(16) 0.32461(10) 0.0168(4) Uani 1 1 d . . . . .
N2 N 0.1892(3) 0.27144(14) 0.34447(11) 0.0154(4) Uani 1 1 d . . . . .
N3 N 0.1705(3) 0.34428(16) 0.30242(10) 0.0176(4) Uani 1 1 d . . . . .
C1 C 0.0068(3) 0.21472(18) 0.26688(12) 0.0163(4) Uani 1 1 d . . . . .
C2 C 0.0547(3) 0.31002(19) 0.25331(12) 0.0178(4) Uani 1 1 d . . . . .
C3 C 0.0057(4) 0.3637(2) 0.19302(13) 0.0257(6) Uani 1 1 d . . . . .
H3A H 0.003959 0.435283 0.201403 0.031 Uiso 1 1 calc R U . . .
H3B H -0.116633 0.343930 0.173523 0.031 Uiso 1 1 calc R U . . .
C4 C 0.1384(4) 0.3426(2) 0.14710(13) 0.0295(6) Uani 1 1 d . . . . .
H4A H 0.085218 0.366603 0.105121 0.035 Uiso 1 1 calc R U . . .
H4B H 0.249621 0.380705 0.160502 0.035 Uiso 1 1 calc R U . . .
C5 C 0.1888(4) 0.2340(2) 0.14170(15) 0.0258(6) Uani 1 1 d . . . . .
H5A H 0.256284 0.212581 0.182386 0.031 Uiso 1 1 calc R U . . .
H5B H 0.270713 0.228368 0.110225 0.031 Uiso 1 1 calc R U . . .
C6 C 0.0304(4) 0.1626(2) 0.12339(12) 0.0246(5) Uani 1 1 d . . . . .
H6A H -0.078057 0.201736 0.107861 0.029 Uiso 1 1 calc R U . . .
H6B H 0.056965 0.121173 0.088280 0.029 Uiso 1 1 calc R U . . .
C7 C -0.0133(3) 0.0945(2) 0.17565(12) 0.0200(5) Uani 1 1 d . . . . .
H7A H 0.100263 0.064684 0.196413 0.024 Uiso 1 1 calc R U . . .
H7B H -0.090386 0.040445 0.156211 0.024 Uiso 1 1 calc R U . . .
C8 C -0.1075(3) 0.14272(19) 0.22627(11) 0.0191(5) Uani 1 1 d . . . . .
H8A H -0.216667 0.176956 0.205607 0.023 Uiso 1 1 calc R U . . .
H8B H -0.146243 0.090377 0.253093 0.023 Uiso 1 1 calc R U . . .
C9 C 0.2861(3) 0.3970(2) 0.46124(12) 0.0198(5) Uani 1 1 d . . . . .
H9A H 0.209908 0.431941 0.427451 0.030 Uiso 1 1 calc R U . . .
H9B H 0.385445 0.439771 0.479246 0.030 Uiso 1 1 calc R U . . .
H9C H 0.214794 0.378926 0.493743 0.030 Uiso 1 1 calc R U . . .
C10 C 0.2123(3) 0.1888(2) 0.47211(12) 0.0224(5) Uani 1 1 d . . . . .
H10A H 0.132684 0.148970 0.441847 0.034 Uiso 1 1 calc R U . . .
H10B H 0.140407 0.234434 0.493074 0.034 Uiso 1 1 calc R U . . .
H10C H 0.281095 0.145539 0.503259 0.034 Uiso 1 1 calc R U . . .
C11 C 0.5728(4) 0.2647(2) 0.50790(14) 0.0240(6) Uani 1 1 d . . . . .
H11A H 0.695120 0.260840 0.497911 0.036 Uiso 1 1 calc R U . . .
H11B H 0.548963 0.206959 0.532431 0.036 Uiso 1 1 calc R U . . .
H11C H 0.560523 0.324521 0.532216 0.036 Uiso 1 1 calc R U . . .
C12 C 0.8098(3) 0.3855(2) 0.41542(16) 0.0321(7) Uani 1 1 d . . . . .
H12A H 0.808241 0.402716 0.459325 0.048 Uiso 1 1 calc R U . . .
H12B H 0.873989 0.323212 0.413205 0.048 Uiso 1 1 calc R U . . .
H12C H 0.870794 0.437535 0.395376 0.048 Uiso 1 1 calc R U . . .
C13 C 0.5079(3) 0.49999(19) 0.36370(13) 0.0224(5) Uani 1 1 d . . . . .
H13A H 0.483526 0.527348 0.403459 0.034 Uiso 1 1 calc R U . . .
H13B H 0.602619 0.538440 0.348670 0.034 Uiso 1 1 calc R U . . .
H13C H 0.398376 0.502724 0.332759 0.034 Uiso 1 1 calc R U . . .
C14 C 0.6152(4) 0.3414(2) 0.29629(14) 0.0291(6) Uani 1 1 d . . . . .
H14A H 0.498714 0.332438 0.269754 0.044 Uiso 1 1 calc R U . . .
H14B H 0.681283 0.394527 0.279361 0.044 Uiso 1 1 calc R U . . .
H14C H 0.684479 0.280204 0.297190 0.044 Uiso 1 1 calc R U . . .
C15 C 0.7351(4) 0.0945(2) 0.41437(16) 0.0326(7) Uani 1 1 d . . . . .
H15A H 0.805248 0.150961 0.403580 0.049 Uiso 1 1 calc R U . . .
H15B H 0.757334 0.084380 0.459748 0.049 Uiso 1 1 calc R U . . .
H15C H 0.770662 0.035530 0.393313 0.049 Uiso 1 1 calc R U . . .
C16 C 0.3874(4) 0.0081(2) 0.41237(15) 0.0305(6) Uani 1 1 d . . . . .
H16A H 0.257155 0.014736 0.400406 0.046 Uiso 1 1 calc R U . . .
H16B H 0.429405 -0.049349 0.391354 0.046 Uiso 1 1 calc R U . . .
H16C H 0.416077 -0.000498 0.457790 0.046 Uiso 1 1 calc R U . . .
C17 C 0.4743(4) 0.0968(2) 0.30508(12) 0.0260(5) Uani 1 1 d . . . . .
H17A H 0.349202 0.107556 0.286098 0.039 Uiso 1 1 calc R U . . .
H17B H 0.552264 0.142349 0.286633 0.039 Uiso 1 1 calc R U . . .
H17C H 0.508915 0.028905 0.297319 0.039 Uiso 1 1 calc R U . . .


_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
Pt1 P1 2.3893(6) . ?
Pt1 P2 2.3789(7) . ?
Pt1 N2 2.128(2) . ?
Pt1 C9 2.107(3) . ?
Pt1 C10 2.102(2) . ?
Pt1 C11 2.084(3) . ?
P1 C12 1.820(3) . ?
P1 C13 1.820(3) . ?
P1 C14 1.818(3) . ?
P2 C15 1.816(3) . ?
P2 C16 1.819(3) . ?
P2 C17 1.826(3) . ?
N1 N2 1.345(3) . ?
N1 C1 1.352(3) . ?
N2 N3 1.337(3) . ?
N3 C2 1.350(3) . ?
C1 C2 1.388(4) . ?
C1 C8 1.496(3) . ?
C2 C3 1.491(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.542(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C5 1.533(4) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.543(4) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 C7 1.535(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.540(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?

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
P2 Pt1 P1 95.74(2) . . ?
N2 Pt1 P1 91.08(6) . . ?
N2 Pt1 P2 88.92(6) . . ?
C9 Pt1 P1 87.82(8) . . ?
C9 Pt1 P2 176.33(8) . . ?
C9 Pt1 N2 91.88(9) . . ?
C10 Pt1 P1 174.98(8) . . ?
C10 Pt1 P2 89.27(8) . . ?
C10 Pt1 N2 88.87(9) . . ?
C10 Pt1 C9 87.16(11) . . ?
C11 Pt1 P1 92.25(9) . . ?
C11 Pt1 P2 92.46(8) . . ?
C11 Pt1 N2 176.25(10) . . ?
C11 Pt1 C9 86.53(11) . . ?
C11 Pt1 C10 87.65(11) . . ?
C12 P1 Pt1 115.70(10) . . ?
C12 P1 C13 102.57(13) . . ?
C13 P1 Pt1 115.75(9) . . ?
C14 P1 Pt1 118.11(10) . . ?
C14 P1 C12 101.97(15) . . ?
C14 P1 C13 100.24(13) . . ?
C15 P2 Pt1 115.18(10) . . ?
C15 P2 C16 104.10(15) . . ?
C15 P2 C17 102.11(14) . . ?
C16 P2 Pt1 115.09(11) . . ?
C16 P2 C17 99.48(14) . . ?
C17 P2 Pt1 118.57(9) . . ?
N2 N1 C1 105.2(2) . . ?
N1 N2 Pt1 122.09(16) . . ?
N3 N2 Pt1 123.92(16) . . ?
N3 N2 N1 112.8(2) . . ?
N2 N3 C2 105.5(2) . . ?
N1 C1 C2 108.2(2) . . ?
N1 C1 C8 122.5(2) . . ?
C2 C1 C8 129.1(2) . . ?
N3 C2 C1 108.3(2) . . ?
N3 C2 C3 124.3(2) . . ?
C1 C2 C3 127.2(2) . . ?
C2 C3 H3A 109.2 . . ?
C2 C3 H3B 109.2 . . ?
C2 C3 C4 112.0(2) . . ?
H3A C3 H3B 107.9 . . ?
C4 C3 H3A 109.2 . . ?
C4 C3 H3B 109.2 . . ?
C3 C4 H4A 108.5 . . ?
C3 C4 H4B 108.5 . . ?
H4A C4 H4B 107.5 . . ?
C5 C4 C3 114.9(2) . . ?
C5 C4 H4A 108.5 . . ?
C5 C4 H4B 108.5 . . ?
C4 C5 H5A 108.3 . . ?
C4 C5 H5B 108.3 . . ?
C4 C5 C6 115.8(3) . . ?
H5A C5 H5B 107.4 . . ?
C6 C5 H5A 108.3 . . ?
C6 C5 H5B 108.3 . . ?
C5 C6 H6A 108.3 . . ?
C5 C6 H6B 108.3 . . ?
H6A C6 H6B 107.4 . . ?
C7 C6 C5 115.8(2) . . ?
C7 C6 H6A 108.3 . . ?
C7 C6 H6B 108.3 . . ?
C6 C7 H7A 108.2 . . ?
C6 C7 H7B 108.2 . . ?
C6 C7 C8 116.2(2) . . ?
H7A C7 H7B 107.4 . . ?
C8 C7 H7A 108.2 . . ?
C8 C7 H7B 108.2 . . ?
C1 C8 C7 114.1(2) . . ?
C1 C8 H8A 108.7 . . ?
C1 C8 H8B 108.7 . . ?
C7 C8 H8A 108.7 . . ?
C7 C8 H8B 108.7 . . ?
H8A C8 H8B 107.6 . . ?
Pt1 C9 H9A 109.5 . . ?
Pt1 C9 H9B 109.5 . . ?
Pt1 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
Pt1 C10 H10A 109.5 . . ?
Pt1 C10 H10B 109.5 . . ?
Pt1 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Pt1 C11 H11A 109.5 . . ?
Pt1 C11 H11B 109.5 . . ?
Pt1 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
P1 C12 H12A 109.5 . . ?
P1 C12 H12B 109.5 . . ?
P1 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
P1 C13 H13A 109.5 . . ?
P1 C13 H13B 109.5 . . ?
P1 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
P1 C14 H14A 109.5 . . ?
P1 C14 H14B 109.5 . . ?
P1 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
P2 C15 H15A 109.5 . . ?
P2 C15 H15B 109.5 . . ?
P2 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
P2 C16 H16A 109.5 . . ?
P2 C16 H16B 109.5 . . ?
P2 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
P2 C17 H17A 109.5 . . ?
P2 C17 H17B 109.5 . . ?
P2 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_vrf_PLAT934_shen18              
;
PROBLEM: Number of (Iobs-Icalc)/Sigma(W) > 10 Outliers .. 10 Check
RESPONSE: Put forward the best model after absorption corrections.
;
# start Validation Reply Form
_vrf_PLAT971_shen18              
;
PROBLEM: Check Calcd Resid. Dens. 0.81A From Pt1 3.54 eA-3
RESPONSE: This can beattributed to the Pt anisotropy.
;
_vrf_PLAT972_shen18              
;
PROBLEM: Check Calcd Resid. Dens. 2.00A From C12 -3.38 eA-3
RESPONSE: It is negative and does not make chemical sense.
;
_vrf_PLAT977_shen18              
;
PROBLEM: Check Negative Difference Density on H8B -1.58 eA-3
RESPONSE:  It is negative and does not make chemical sense.
;
####################################################################### 
# 
# 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_shen11
_database_code_depnum_ccdc_archive 'CCDC 2068055'
loop_
_audit_author_name
_audit_author_address
'Khalil Abboud'
;University of Florida
United States of America
;

_audit_update_record             
;
2021-03-04 deposited with the CCDC.	2021-08-09 downloaded from the CCDC.
;
# publcif _publ_body_element loop end

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H20 N5 O3 Re'
_chemical_formula_weight         576.62

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 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. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.099(7)
_cell_length_b                   10.839(6)
_cell_length_c                   11.962(9)
_cell_angle_alpha                77.240(15)
_cell_angle_beta                 72.021(16)
_cell_angle_gamma                85.85(2)
_cell_volume                     1214.7(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9594
_cell_measurement_theta_min      2.0
_cell_measurement_theta_max      28.0

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.576
_exptl_crystal_F_000             560
_exptl_transmission_factor_min   0.4553
_exptl_transmission_factor_max   0.5659
_exptl_crystal_size_max          0.343
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.034
_exptl_absorpt_coefficient_mu    5.030
_shelx_estimated_absorpt_T_min   0.277
_shelx_estimated_absorpt_T_max   0.848
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   
'Sheldrick, G. M., sadabs (2015). Acta Cryst. C71, 3-8.'

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'micro source 3.0'
_diffrn_measurement_device_type  'D8 Venture with PHOTON III'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            77811
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.926
_diffrn_reflns_theta_max         33.181
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.924
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8592
_reflns_number_gt                7613
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 Structure factors included contributions from the .fab file. 
  
 _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. 
;

_computing_data_collection       'Bruker APEX3 (Bruker, 2014)'
_computing_cell_refinement       'Bruker APEX3 (Bruker, 2014)'
_computing_data_reduction        'Bruker Apex3 SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXL2015, Sheldrick G. M. 2015'
_computing_structure_refinement  'SHELXL2015, Sheldrick G. M. 2015'
_computing_molecular_graphics    'XP in SHELXTL-plus, Bruker 2014'
_computing_publication_material  'SHELXL2015, Sheldrick, G. M. 2015'
_refine_special_details          
; 
All H atoms were positioned geometrically ( C---H = 0.93/1.00 Å) and 
allowed to ride with Uiso(H)= 1.2/1.5Ueq(C). 
Methyl ones were allowed to rotate around the corresponding C---C. 

One oxygen atom of a carbonyl ligand is disordered and refined in two parts with
 their site occupations factors dependently refined.  The C3-C8 part of the C8
 ring is also disordered and also refined in two parts with their site
 occupation factors dependently refined.  The equivalent bonds in the --C3-C8-
 part of the ring were constrained to stay geometrically equivalent using the
 SADI command lines. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0187P)²+1.8934P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8592
_refine_ls_number_parameters     331
_refine_ls_number_restraints     660
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0262
_refine_ls_wR_factor_ref         0.0607
_refine_ls_wR_factor_gt          0.0578
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

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
Re1 Re 0.78350(2) 0.19658(2) 0.51839(2) 0.02893(3) Uani 1 1 d . U . . .
O1 O 1.050(3) 0.220(4) 0.303(3) 0.052(4) Uani 0.56(18) 1 d D U P A 1
O1' O 1.032(5) 0.215(6) 0.290(3) 0.056(6) Uani 0.44(18) 1 d D U P A 2
O2 O 0.9692(2) 0.1576(2) 0.6849(2) 0.0471(5) Uani 1 1 d . U . . .
O3 O 0.7857(2) -0.09021(19) 0.5350(2) 0.0469(5) Uani 1 1 d . U . . .
N1 N 0.5745(3) 0.2502(2) 0.7552(2) 0.0349(5) Uani 1 1 d . U . . .
N2 N 0.5949(2) 0.18913(19) 0.66552(19) 0.0285(4) Uani 1 1 d . U . . .
N3 N 0.4854(2) 0.1176(2) 0.6792(2) 0.0320(4) Uani 1 1 d . U . . .
N4 N 0.7606(2) 0.4007(2) 0.4956(2) 0.0301(4) Uani 1 1 d . U . . .
N5 N 0.6461(2) 0.2491(2) 0.40646(19) 0.0289(4) Uani 1 1 d . U . . .
C1 C 0.4458(3) 0.2169(3) 0.8299(2) 0.0382(6) Uani 1 1 d D U . . .
C2 C 0.3909(3) 0.1340(3) 0.7821(2) 0.0347(5) Uani 1 1 d D U . . .
C3 C 0.2506(3) 0.0712(3) 0.8246(3) 0.0463(7) Uani 1 1 d D U . . .
H3X H 0.261611 -0.020023 0.856466 0.06(2) Uiso 0.565(5) 1 calc R . P B 1
H3Y H 0.214287 0.079310 0.755263 0.05(2) Uiso 0.565(5) 1 calc R . P B 1
H3Z H 0.236643 0.041162 0.756655 0.027(18) Uiso 0.435(5) 1 calc R . P B 2
H3V H 0.178209 0.135918 0.845723 0.031(19) Uiso 0.435(5) 1 calc R . P B 2
C4 C 0.1453(6) 0.1284(7) 0.9217(4) 0.070(2) Uani 0.565(5) 1 d D U P B 1
H4A H 0.050138 0.115661 0.919514 0.084 Uiso 0.565(5) 1 calc R U P B 1
H4B H 0.161404 0.220539 0.905144 0.084 Uiso 0.565(5) 1 calc R U P B 1
C5 C 0.1562(6) 0.0686(9) 1.0468(5) 0.076(2) Uani 0.565(5) 1 d D U P B 1
H5A H 0.096122 0.118458 1.103454 0.091 Uiso 0.565(5) 1 calc R U P B 1
H5B H 0.115731 -0.017168 1.069777 0.091 Uiso 0.565(5) 1 calc R U P B 1
C6 C 0.2989(7) 0.0560(6) 1.0675(6) 0.0557(18) Uani 0.565(5) 1 d D U P B 1
H6A H 0.289844 0.003743 1.148567 0.067 Uiso 0.565(5) 1 calc R U P B 1
H6B H 0.362822 0.011311 1.008024 0.067 Uiso 0.565(5) 1 calc R U P B 1
C7 C 0.3620(6) 0.1833(5) 1.0568(4) 0.0362(11) Uani 0.565(5) 1 d D U P B 1
H7A H 0.456730 0.169393 1.065271 0.043 Uiso 0.565(5) 1 calc R U P B 1
H7B H 0.304897 0.222900 1.123252 0.043 Uiso 0.565(5) 1 calc R U P B 1
C8 C 0.3704(10) 0.2734(6) 0.9371(3) 0.0444(19) Uani 0.565(5) 1 d D U P B 1
H8A H 0.274897 0.297262 0.934120 0.053 Uiso 0.565(5) 1 calc R U P B 1
H8B H 0.418887 0.351426 0.932322 0.053 Uiso 0.565(5) 1 calc R U P B 1
C4' C 0.2274(8) -0.0400(5) 0.9320(4) 0.0451(18) Uani 0.435(5) 1 d D U P B 2
H4'A H 0.267775 -0.116850 0.902130 0.054 Uiso 0.435(5) 1 calc R U P B 2
H4'B H 0.125941 -0.053679 0.968430 0.054 Uiso 0.435(5) 1 calc R U P B 2
C5' C 0.2887(8) -0.0263(7) 1.0305(5) 0.0476(18) Uani 0.435(5) 1 d D U P B 2
H5'A H 0.274054 -0.106630 1.091143 0.057 Uiso 0.435(5) 1 calc R U P B 2
H5'B H 0.390384 -0.013943 0.994386 0.057 Uiso 0.435(5) 1 calc R U P B 2
C6' C 0.2293(13) 0.0815(6) 1.0949(7) 0.059(3) Uani 0.435(5) 1 d D U P B 2
H6'A H 0.259070 0.066523 1.168298 0.070 Uiso 0.435(5) 1 calc R U P B 2
H6'B H 0.126711 0.073624 1.121763 0.070 Uiso 0.435(5) 1 calc R U P B 2
C7' C 0.2636(14) 0.2188(8) 1.0306(10) 0.106(5) Uani 0.435(5) 1 d D U P B 2
H7'A H 0.197426 0.245294 0.983468 0.127 Uiso 0.435(5) 1 calc R U P B 2
H7'B H 0.240287 0.269154 1.093840 0.127 Uiso 0.435(5) 1 calc R U P B 2
C8' C 0.4074(12) 0.2620(15) 0.9465(8) 0.062(4) Uani 0.435(5) 1 d D U P B 2
H8'A H 0.410144 0.355638 0.928352 0.074 Uiso 0.435(5) 1 calc R U P B 2
H8'B H 0.477743 0.230550 0.988240 0.074 Uiso 0.435(5) 1 calc R U P B 2
C9 C 0.8184(3) 0.4721(3) 0.5467(3) 0.0342(5) Uani 1 1 d . U . . .
H9A H 0.869212 0.431379 0.599547 0.041 Uiso 1 1 calc R U . . .
C10 C 0.8068(3) 0.6027(3) 0.5251(3) 0.0368(6) Uani 1 1 d . U . . .
H10A H 0.849474 0.650488 0.562161 0.044 Uiso 1 1 calc R U . . .
C11 C 0.7320(3) 0.6625(3) 0.4490(3) 0.0374(6) Uani 1 1 d . U . . .
H11A H 0.724101 0.752096 0.431887 0.045 Uiso 1 1 calc R U . . .
C12 C 0.6688(3) 0.5900(2) 0.3978(3) 0.0349(5) Uani 1 1 d . U . . .
H12A H 0.615109 0.629315 0.346893 0.042 Uiso 1 1 calc R U . . .
C13 C 0.6849(3) 0.4590(2) 0.4221(2) 0.0306(5) Uani 1 1 d . U . . .
C14 C 0.6218(3) 0.3749(2) 0.3719(2) 0.0302(5) Uani 1 1 d . U . . .
C15 C 0.5408(3) 0.4186(3) 0.2952(3) 0.0381(6) Uani 1 1 d . U . . .
H15A H 0.525615 0.506689 0.271505 0.046 Uiso 1 1 calc R U . . .
C16 C 0.4827(4) 0.3323(3) 0.2537(3) 0.0424(7) Uani 1 1 d . U . . .
H16A H 0.428137 0.360307 0.200708 0.051 Uiso 1 1 calc R U . . .
C17 C 0.5060(3) 0.2043(3) 0.2913(3) 0.0394(6) Uani 1 1 d . U . . .
H17A H 0.467036 0.143299 0.264592 0.047 Uiso 1 1 calc R U . . .
C18 C 0.5860(3) 0.1662(3) 0.3676(2) 0.0346(5) Uani 1 1 d . U . . .
H18A H 0.599442 0.078234 0.393951 0.042 Uiso 1 1 calc R U . . .
C19 C 0.9457(3) 0.2103(3) 0.3804(3) 0.0393(6) Uani 1 1 d D U . . .
C20 C 0.9001(3) 0.1706(3) 0.6230(3) 0.0341(5) Uani 1 1 d . U . . .
C21 C 0.7846(3) 0.0172(3) 0.5307(3) 0.0345(5) Uani 1 1 d . U . . .


_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
Re1 C21 1.917(3) . ?
Re1 C19 1.920(3) . ?
Re1 C20 1.933(3) . ?
Re1 N2 2.150(2) . ?
Re1 N4 2.173(2) . ?
Re1 N5 2.176(3) . ?
O1 C19 1.160(5) . ?
O1' C19 1.160(5) . ?
O2 C20 1.146(4) . ?
O3 C21 1.153(3) . ?
N1 N2 1.337(3) . ?
N1 C1 1.351(4) . ?
N2 N3 1.345(3) . ?
N3 C2 1.343(3) . ?
N4 C9 1.344(3) . ?
N4 C13 1.363(4) . ?
N5 C18 1.353(3) . ?
N5 C14 1.363(3) . ?
C1 C2 1.393(4) . ?
C1 C8' 1.508(4) . ?
C1 C8 1.508(3) . ?
C2 C3 1.507(3) . ?
C3 C4 1.525(3) . ?
C3 C4' 1.527(3) . ?
C3 H3X 0.9900 . ?
C3 H3Y 0.9900 . ?
C3 H3Z 0.9900 . ?
C3 H3V 0.9900 . ?
C4 C5 1.527(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.527(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.526(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.526(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C4' C5' 1.527(3) . ?
C4' H4'A 0.9900 . ?
C4' H4'B 0.9900 . ?
C5' C6' 1.526(3) . ?
C5' H5'A 0.9900 . ?
C5' H5'B 0.9900 . ?
C6' C7' 1.526(3) . ?
C6' H6'A 0.9900 . ?
C6' H6'B 0.9900 . ?
C7' C8' 1.526(3) . ?
C7' H7'A 0.9900 . ?
C7' H7'B 0.9900 . ?
C8' H8'A 0.9900 . ?
C8' H8'B 0.9900 . ?
C9 C10 1.385(4) . ?
C9 H9A 0.9500 . ?
C10 C11 1.383(4) . ?
C10 H10A 0.9500 . ?
C11 C12 1.387(4) . ?
C11 H11A 0.9500 . ?
C12 C13 1.393(4) . ?
C12 H12A 0.9500 . ?
C13 C14 1.470(4) . ?
C14 C15 1.396(4) . ?
C15 C16 1.390(4) . ?
C15 H15A 0.9500 . ?
C16 C17 1.388(4) . ?
C16 H16A 0.9500 . ?
C17 C18 1.377(4) . ?
C17 H17A 0.9500 . ?
C18 H18A 0.9500 . ?

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
C21 Re1 C19 89.42(13) . . ?
C21 Re1 C20 88.62(12) . . ?
C19 Re1 C20 90.35(14) . . ?
C21 Re1 N2 92.45(10) . . ?
C19 Re1 N2 176.25(11) . . ?
C20 Re1 N2 92.94(12) . . ?
C21 Re1 N4 172.88(11) . . ?
C19 Re1 N4 92.41(11) . . ?
C20 Re1 N4 98.24(10) . . ?
N2 Re1 N4 85.35(8) . . ?
C21 Re1 N5 98.22(11) . . ?
C19 Re1 N5 92.01(13) . . ?
C20 Re1 N5 172.78(10) . . ?
N2 Re1 N5 84.50(10) . . ?
N4 Re1 N5 74.85(8) . . ?
N2 N1 C1 105.7(2) . . ?
N1 N2 N3 112.5(2) . . ?
N1 N2 Re1 124.61(17) . . ?
N3 N2 Re1 122.88(16) . . ?
C2 N3 N2 105.6(2) . . ?
C9 N4 C13 118.7(2) . . ?
C9 N4 Re1 124.4(2) . . ?
C13 N4 Re1 116.90(16) . . ?
C18 N5 C14 118.2(2) . . ?
C18 N5 Re1 124.75(19) . . ?
C14 N5 Re1 117.02(17) . . ?
N1 C1 C2 107.9(2) . . ?
N1 C1 C8' 114.9(5) . . ?
C2 C1 C8' 136.6(5) . . ?
N1 C1 C8 125.1(5) . . ?
C2 C1 C8 126.6(5) . . ?
N3 C2 C1 108.3(2) . . ?
N3 C2 C3 120.7(2) . . ?
C1 C2 C3 130.9(3) . . ?
C2 C3 C4 112.7(4) . . ?
C2 C3 C4' 116.1(3) . . ?
C2 C3 H3X 109.1 . . ?
C4 C3 H3X 109.1 . . ?
C2 C3 H3Y 109.1 . . ?
C4 C3 H3Y 109.1 . . ?
H3X C3 H3Y 107.8 . . ?
C2 C3 H3Z 108.3 . . ?
C4' C3 H3Z 108.3 . . ?
C2 C3 H3V 108.3 . . ?
C4' C3 H3V 108.3 . . ?
H3Z C3 H3V 107.4 . . ?
C3 C4 C5 111.7(5) . . ?
C3 C4 H4A 109.3 . . ?
C5 C4 H4A 109.3 . . ?
C3 C4 H4B 109.3 . . ?
C5 C4 H4B 109.3 . . ?
H4A C4 H4B 107.9 . . ?
C6 C5 C4 119.3(5) . . ?
C6 C5 H5A 107.5 . . ?
C4 C5 H5A 107.5 . . ?
C6 C5 H5B 107.5 . . ?
C4 C5 H5B 107.5 . . ?
H5A C5 H5B 107.0 . . ?
C7 C6 C5 112.9(6) . . ?
C7 C6 H6A 109.0 . . ?
C5 C6 H6A 109.0 . . ?
C7 C6 H6B 109.0 . . ?
C5 C6 H6B 109.0 . . ?
H6A C6 H6B 107.8 . . ?
C6 C7 C8 112.4(5) . . ?
C6 C7 H7A 109.1 . . ?
C8 C7 H7A 109.1 . . ?
C6 C7 H7B 109.1 . . ?
C8 C7 H7B 109.1 . . ?
H7A C7 H7B 107.9 . . ?
C1 C8 C7 113.0(4) . . ?
C1 C8 H8A 109.0 . . ?
C7 C8 H8A 109.0 . . ?
C1 C8 H8B 109.0 . . ?
C7 C8 H8B 109.0 . . ?
H8A C8 H8B 107.8 . . ?
C3 C4' C5' 116.0(4) . . ?
C3 C4' H4'A 108.3 . . ?
C5' C4' H4'A 108.3 . . ?
C3 C4' H4'B 108.3 . . ?
C5' C4' H4'B 108.3 . . ?
H4'A C4' H4'B 107.4 . . ?
C6' C5' C4' 115.8(7) . . ?
C6' C5' H5'A 108.3 . . ?
C4' C5' H5'A 108.3 . . ?
C6' C5' H5'B 108.3 . . ?
C4' C5' H5'B 108.3 . . ?
H5'A C5' H5'B 107.4 . . ?
C5' C6' C7' 120.5(7) . . ?
C5' C6' H6'A 107.2 . . ?
C7' C6' H6'A 107.2 . . ?
C5' C6' H6'B 107.2 . . ?
C7' C6' H6'B 107.2 . . ?
H6'A C6' H6'B 106.8 . . ?
C8' C7' C6' 123.3(12) . . ?
C8' C7' H7'A 106.5 . . ?
C6' C7' H7'A 106.5 . . ?
C8' C7' H7'B 106.5 . . ?
C6' C7' H7'B 106.5 . . ?
H7'A C7' H7'B 106.5 . . ?
C1 C8' C7' 113.5(7) . . ?
C1 C8' H8'A 108.9 . . ?
C7' C8' H8'A 108.9 . . ?
C1 C8' H8'B 108.9 . . ?
C7' C8' H8'B 108.9 . . ?
H8'A C8' H8'B 107.7 . . ?
N4 C9 C10 122.5(3) . . ?
N4 C9 H9A 118.7 . . ?
C10 C9 H9A 118.7 . . ?
C11 C10 C9 119.0(3) . . ?
C11 C10 H10A 120.5 . . ?
C9 C10 H10A 120.5 . . ?
C10 C11 C12 119.2(3) . . ?
C10 C11 H11A 120.4 . . ?
C12 C11 H11A 120.4 . . ?
C11 C12 C13 119.2(3) . . ?
C11 C12 H12A 120.4 . . ?
C13 C12 H12A 120.4 . . ?
N4 C13 C12 121.3(2) . . ?
N4 C13 C14 115.7(2) . . ?
C12 C13 C14 123.0(3) . . ?
N5 C14 C15 121.4(2) . . ?
N5 C14 C13 115.3(2) . . ?
C15 C14 C13 123.3(2) . . ?
C16 C15 C14 119.6(3) . . ?
C16 C15 H15A 120.2 . . ?
C14 C15 H15A 120.2 . . ?
C17 C16 C15 118.5(3) . . ?
C17 C16 H16A 120.8 . . ?
C15 C16 H16A 120.8 . . ?
C18 C17 C16 119.6(3) . . ?
C18 C17 H17A 120.2 . . ?
C16 C17 H17A 120.2 . . ?
N5 C18 C17 122.7(3) . . ?
N5 C18 H18A 118.7 . . ?
C17 C18 H18A 118.7 . . ?
O1' C19 Re1 171(4) . . ?
O1 C19 Re1 174(3) . . ?
O2 C20 Re1 178.7(2) . . ?
O3 C21 Re1 178.3(3) . . ?

_refine_diff_density_max         2.374
_refine_diff_density_min         -1.877
_refine_diff_density_rms         0.113





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