# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_dab2
_database_code_depnum_ccdc_archive 'CCDC 2281681'
loop_
_audit_author_name
_audit_author_address
'Seth Brown'
;University of Notre Dame
United States of America
;
_audit_update_record             
;
2023-07-14 deposited with the CCDC.	2023-08-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
; 
 (R,R)-2,3-Dianthraniloylbutane
;
_chemical_name_common            (R,R)-2,3-Dianthraniloylbutane
_chemical_melting_point          383
_chemical_formula_moiety         'C18 H20 N2 O4'
_chemical_formula_sum            'C18 H20 N2 O4'
_chemical_formula_weight         328.36

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_H-M_alt        'P 21 21 2'
_space_group_name_Hall           'P 2 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, -y, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'

_cell_length_a                   13.6305(5)
_cell_length_b                   9.5069(3)
_cell_length_c                   12.8227(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1661.61(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9462
_cell_measurement_theta_min      3.45
_cell_measurement_theta_max      72.34

_exptl_crystal_description       tablet
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_F_000             696
_exptl_transmission_factor_min   0.8793
_exptl_transmission_factor_max   0.9883
_exptl_crystal_size_max          0.253
_exptl_crystal_size_mid          0.138
_exptl_crystal_size_min          0.054
_exptl_absorpt_coefficient_mu    0.769
_shelx_estimated_absorpt_T_min   0.829
_shelx_estimated_absorpt_T_max   0.960
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.8793
_exptl_absorpt_correction_T_max  0.9883
_exptl_absorpt_process_details   
; 
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., 
 J. Appl. Cryst. 48 (2015) 3-10 
;

_exptl_crystal_recrystallization_method 
'Crystals were grown by dissolving crude product in methanol and allowingto stand at room temperature.'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.33
_diffrn_reflns_number            29865
_diffrn_reflns_av_unetI/netI     0.0127
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.447
_diffrn_reflns_theta_max         72.352
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3283
_reflns_number_gt                3250
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.739
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 ? 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0535P)²+0.1690P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
; 
 Flack x determined using 1379 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   0.08(3)
_chemical_absolute_configuration rmad
_refine_ls_number_reflns         3283
_refine_ls_number_parameters     297
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0252
_refine_ls_R_factor_gt           0.0250
_refine_ls_wR_factor_ref         0.0744
_refine_ls_wR_factor_gt          0.0743
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.000
_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
N1 N 0.60767(11) 0.41510(16) 0.25815(11) 0.0281(3) Uani 1 1 d . . . . .
C18 C 0.60417(12) -0.05251(16) -0.10852(12) 0.0239(3) Uani 1 1 d . . . . .
N2 N 0.89197(11) 0.41014(15) 0.68922(11) 0.0283(3) Uani 1 1 d . . . . .
C28 C 1.09987(14) 0.06958(19) 0.31786(14) 0.0319(4) Uani 1 1 d . . . . .
C10 C 0.55613(10) 0.00713(15) -0.01185(11) 0.0196(3) Uani 1 1 d . . . . .
O11 O 0.57181(9) 0.16259(11) 0.16410(9) 0.0268(3) Uani 1 1 d . . . . .
C11 C 0.61598(10) 0.37106(15) 0.07023(11) 0.0189(3) Uani 1 1 d . . . . .
O12 O 0.57950(7) 0.15657(10) -0.01095(8) 0.0207(2) Uani 1 1 d . . . . .
C12 C 0.62243(10) 0.45993(15) 0.15894(12) 0.0205(3) Uani 1 1 d . . . . .
C13 C 0.64895(11) 0.60225(16) 0.14252(13) 0.0234(3) Uani 1 1 d . . . . .
C14 C 0.66949(11) 0.65245(16) 0.04490(14) 0.0249(3) Uani 1 1 d . . . . .
C15 C 0.66412(12) 0.56488(17) -0.04260(13) 0.0262(3) Uani 1 1 d . . . . .
C16 C 0.63694(11) 0.42616(16) -0.02894(12) 0.0226(3) Uani 1 1 d . . . . .
C17 C 0.58724(10) 0.22226(15) 0.08163(12) 0.0192(3) Uani 1 1 d . . . . .
C20 C 1.03586(12) 0.06184(15) 0.41421(12) 0.0248(3) Uani 1 1 d . . . . .
O21 O 0.96416(9) 0.17815(12) 0.58974(9) 0.0268(3) Uani 1 1 d . . . . .
C21 C 0.89694(11) 0.37638(14) 0.49980(12) 0.0209(3) Uani 1 1 d . . . . .
O22 O 0.97878(9) 0.19107(11) 0.41540(8) 0.0255(3) Uani 1 1 d . . . . .
C22 C 0.87381(11) 0.45579(15) 0.58964(12) 0.0222(3) Uani 1 1 d . . . . .
C23 C 0.82719(12) 0.58695(17) 0.57526(13) 0.0271(3) Uani 1 1 d . . . . .
C24 C 0.80291(12) 0.63485(18) 0.47777(14) 0.0297(4) Uani 1 1 d . . . . .
C25 C 0.82356(13) 0.55467(18) 0.38913(14) 0.0306(4) Uani 1 1 d . . . . .
C26 C 0.87109(12) 0.42796(17) 0.40065(12) 0.0258(3) Uani 1 1 d . . . . .
C27 C 0.94877(11) 0.24062(16) 0.50867(12) 0.0211(3) Uani 1 1 d . . . . .
H1B H 0.6014(18) 0.481(3) 0.3067(18) 0.042(6) Uiso 1 1 d . . . . .
H10 H 0.5826(13) -0.0356(18) 0.0517(13) 0.013(4) Uiso 1 1 d . . . . .
H16 H 0.6345(14) 0.365(2) -0.0887(16) 0.025(5) Uiso 1 1 d . . . . .
H20 H 1.0743(15) 0.060(2) 0.4770(15) 0.024(5) Uiso 1 1 d . . . . .
H2A H 0.9370(18) 0.338(3) 0.6991(18) 0.040(6) Uiso 1 1 d . . . . .
H2B H 0.8940(18) 0.479(3) 0.7400(19) 0.044(6) Uiso 1 1 d . . . . .
H18C H 0.5861(14) 0.008(2) -0.1703(14) 0.022(4) Uiso 1 1 d . . . . .
H15 H 0.6809(17) 0.600(2) -0.1132(18) 0.035(6) Uiso 1 1 d . . . . .
H1A H 0.5821(17) 0.334(3) 0.2671(19) 0.040(6) Uiso 1 1 d . . . . .
H18B H 0.5827(16) -0.147(2) -0.1191(16) 0.032(5) Uiso 1 1 d . . . . .
H14 H 0.6875(15) 0.747(2) 0.0373(15) 0.030(5) Uiso 1 1 d . . . . .
H13 H 0.6528(15) 0.659(2) 0.1999(16) 0.030(5) Uiso 1 1 d . . . . .
H25 H 0.8057(15) 0.590(2) 0.3211(17) 0.031(5) Uiso 1 1 d . . . . .
H28C H 1.0594(17) 0.085(3) 0.2569(18) 0.039(6) Uiso 1 1 d . . . . .
H26 H 0.8865(16) 0.370(2) 0.3446(18) 0.034(5) Uiso 1 1 d . . . . .
H28B H 1.1490(18) 0.142(3) 0.3258(18) 0.042(6) Uiso 1 1 d . . . . .
H28A H 1.1341(16) -0.022(3) 0.3061(18) 0.039(6) Uiso 1 1 d . . . . .
H23 H 0.8174(16) 0.642(2) 0.6375(18) 0.035(5) Uiso 1 1 d . . . . .
H18A H 0.6753(17) -0.055(2) -0.0988(17) 0.034(5) Uiso 1 1 d . . . . .
H24 H 0.7732(17) 0.722(3) 0.4708(17) 0.041(6) Uiso 1 1 d . . . . .


_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
N1 C12 1.357(2) . ?
N1 H1B 0.88(3) . ?
N1 H1A 0.85(3) . ?
C18 C10 1.512(2) . ?
C18 H18C 1.01(2) . ?
C18 H18B 0.96(2) . ?
C18 H18A 0.98(2) . ?
N2 C22 1.371(2) . ?
N2 H2A 0.93(3) . ?
N2 H2B 0.93(3) . ?
C28 C20 1.514(2) . ?
C28 H28C 0.97(2) . ?
C28 H28B 0.97(3) . ?
C28 H28A 1.00(2) . ?
C10 O12 1.4560(16) . ?
C10 C10 1.536(3) 2_655 ?
C10 H10 0.979(17) . ?
O11 C17 1.2182(19) . ?
C11 C16 1.405(2) . ?
C11 C12 1.420(2) . ?
C11 C17 1.4751(18) . ?
O12 C17 1.3456(18) . ?
C12 C13 1.416(2) . ?
C13 C14 1.369(2) . ?
C13 H13 0.92(2) . ?
C14 C15 1.399(2) . ?
C14 H14 0.94(2) . ?
C15 C16 1.381(2) . ?
C15 H15 0.99(2) . ?
C16 H16 0.96(2) . ?
C20 O22 1.4544(17) . ?
C20 C20 1.529(3) 2_755 ?
C20 H20 0.96(2) . ?
O21 C27 1.2155(19) . ?
C21 C26 1.408(2) . ?
C21 C22 1.413(2) . ?
C21 C27 1.476(2) . ?
O22 C27 1.3489(18) . ?
C22 C23 1.412(2) . ?
C23 C24 1.371(2) . ?
C23 H23 0.96(2) . ?
C24 C25 1.397(2) . ?
C24 H24 0.93(3) . ?
C25 C26 1.376(2) . ?
C25 H25 0.97(2) . ?
C26 H26 0.93(2) . ?

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
C12 N1 H1B 117.0(16) . . ?
C12 N1 H1A 118.0(16) . . ?
H1B N1 H1A 120(2) . . ?
C10 C18 H18C 108.8(11) . . ?
C10 C18 H18B 109.7(13) . . ?
H18C C18 H18B 110.6(16) . . ?
C10 C18 H18A 109.5(13) . . ?
H18C C18 H18A 110.7(16) . . ?
H18B C18 H18A 107.5(17) . . ?
C22 N2 H2A 118.7(14) . . ?
C22 N2 H2B 115.9(15) . . ?
H2A N2 H2B 114(2) . . ?
C20 C28 H28C 109.8(13) . . ?
C20 C28 H28B 110.4(14) . . ?
H28C C28 H28B 112(2) . . ?
C20 C28 H28A 110.5(13) . . ?
H28C C28 H28A 106.0(19) . . ?
H28B C28 H28A 108.3(18) . . ?
O12 C10 C18 106.11(11) . . ?
O12 C10 C10 107.70(14) . 2_655 ?
C18 C10 C10 113.47(10) . 2_655 ?
O12 C10 H10 108.5(10) . . ?
C18 C10 H10 111.5(10) . . ?
C10 C10 H10 109.3(10) 2_655 . ?
C16 C11 C12 119.40(13) . . ?
C16 C11 C17 120.10(13) . . ?
C12 C11 C17 120.51(13) . . ?
C17 O12 C10 118.49(11) . . ?
N1 C12 C13 118.52(14) . . ?
N1 C12 C11 123.72(14) . . ?
C13 C12 C11 117.73(14) . . ?
C14 C13 C12 121.42(14) . . ?
C14 C13 H13 121.1(13) . . ?
C12 C13 H13 117.5(13) . . ?
C13 C14 C15 121.02(13) . . ?
C13 C14 H14 118.9(12) . . ?
C15 C14 H14 120.1(12) . . ?
C16 C15 C14 118.73(15) . . ?
C16 C15 H15 119.7(14) . . ?
C14 C15 H15 121.5(14) . . ?
C15 C16 C11 121.70(14) . . ?
C15 C16 H16 119.0(12) . . ?
C11 C16 H16 119.3(12) . . ?
O11 C17 O12 122.42(12) . . ?
O11 C17 C11 125.34(13) . . ?
O12 C17 C11 112.24(12) . . ?
O22 C20 C28 106.01(13) . . ?
O22 C20 C20 107.91(15) . 2_755 ?
C28 C20 C20 113.93(11) . 2_755 ?
O22 C20 H20 107.4(12) . . ?
C28 C20 H20 111.8(12) . . ?
C20 C20 H20 109.5(12) 2_755 . ?
C26 C21 C22 119.63(13) . . ?
C26 C21 C27 119.61(14) . . ?
C22 C21 C27 120.76(13) . . ?
C27 O22 C20 117.81(11) . . ?
N2 C22 C23 118.85(14) . . ?
N2 C22 C21 123.36(13) . . ?
C23 C22 C21 117.77(14) . . ?
C24 C23 C22 121.41(15) . . ?
C24 C23 H23 122.9(14) . . ?
C22 C23 H23 115.6(14) . . ?
C23 C24 C25 120.79(15) . . ?
C23 C24 H24 119.3(14) . . ?
C25 C24 H24 119.9(14) . . ?
C26 C25 C24 119.03(16) . . ?
C26 C25 H25 121.4(13) . . ?
C24 C25 H25 119.5(13) . . ?
C25 C26 C21 121.33(15) . . ?
C25 C26 H26 122.9(14) . . ?
C21 C26 H26 115.8(14) . . ?
O21 C27 O22 122.37(13) . . ?
O21 C27 C21 125.16(14) . . ?
O22 C27 C21 112.48(12) . . ?

_refine_diff_density_max         0.191
_refine_diff_density_min         -0.148
_refine_diff_density_rms         0.031

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_biniqh4
_database_code_depnum_ccdc_archive 'CCDC 2281682'
loop_
_audit_author_name
_audit_author_address
'Seth Brown'
;University of Notre Dame
United States of America
;
_audit_update_record             
;
2023-07-14 deposited with the CCDC.	2023-08-28 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT234_biniqh4             
;
PROBLEM: Large Hirshfeld Difference C51--C52  .  0.32 Ang.  
RESPONSE: The toluene solvate has unresolved disorder.
;

_vrf_PLAT330_biniqh4             
;
PROBLEM: Large Aver Phenyl C-C Dist C51--C56    .   1.43 Ang.  
RESPONSE: The toluene solvate has unresolved disorder and thus
the bond distances are not well determined.
;

_vrf_PLAT340_biniqh4             
;
PROBLEM: Low Bond Precision on  C-C Bonds ....    0.01248 Ang.  
RESPONSE: The disordered solvents decrease the average precision 
of the C-C bonds.
;

_vrf_PLAT420_biniqh4             
;
PROBLEM: D-H Bond Without Acceptor  O6--H6    .   Please Check 
RESPONSE: O6 is involved in a hydrogen bonding network, accepting
hydrogen bonds from H1O and H2O.
;

# end Validation Reply Form

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
"(R)-2,2'-bis-N-(2-hydroxy-3,5-di-tert-butylphenyl)amino-1,1'-binaphthyl methanol toluene solvate"
_chemical_name_common            '(R)-BiniqH4 . CH3OH . PhCH3'
_chemical_melting_point          ?
_chemical_formula_moiety         'C48 H56 N2 O2, C7 H8, C H4 O'
_chemical_formula_sum            'C56 H68 N2 O3'
_chemical_formula_weight         817.12

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_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+1/2, -z'

_cell_length_a                   15.1059(14)
_cell_length_b                   9.4304(9)
_cell_length_c                   17.6428(16)
_cell_angle_alpha                90
_cell_angle_beta                 102.041(2)
_cell_angle_gamma                90
_cell_volume                     2458.0(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9836
_cell_measurement_theta_min      2.360
_cell_measurement_theta_max      26.341

_exptl_crystal_description       rod
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.104
_exptl_crystal_F_000             884
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.432
_exptl_crystal_size_mid          0.194
_exptl_crystal_size_min          0.126
_exptl_absorpt_coefficient_mu    0.067
_shelx_estimated_absorpt_T_min   0.972
_shelx_estimated_absorpt_T_max   0.992
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.9244
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10.
;

_exptl_crystal_recrystallization_method 
'Crystals formed on diffusion of methanol into a toluene solution of the compound.'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.33
_diffrn_reflns_number            82110
_diffrn_reflns_av_unetI/netI     0.0564
_diffrn_reflns_av_R_equivalents  0.0687
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.617
_diffrn_reflns_theta_max         26.433
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             9921
_reflns_number_gt                7691
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.859
_reflns_Friedel_fraction_max     0.969
_reflns_Friedel_fraction_full    0.984

_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 The thermal parameters of the aromatic ring of the lattice 
toluene were restrained to be similar using the SIMU command with 
an effective standard deviation of 0.05.  Hydrogens on lattice
solvents and on methyl groups were placed in calculated positions.
All other hydrogen atoms were found on the difference map and
refined isotropically, except the hydrogen on O1, which was 
placed in a calculated position. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0502P)²+5.0527P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2835 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.7(7)
_chemical_absolute_configuration rm
_refine_ls_number_reflns         9921
_refine_ls_number_parameters     630
_refine_ls_number_restraints     37
_refine_ls_R_factor_all          0.1268
_refine_ls_R_factor_gt           0.0888
_refine_ls_wR_factor_ref         0.2183
_refine_ls_wR_factor_gt          0.1977
_refine_ls_goodness_of_fit_ref   1.239
_refine_ls_restrained_S_all      1.239
_refine_ls_shift/su_max          0.000
_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
O1 O 0.7770(4) 0.3064(5) 0.4580(3) 0.0346(12) Uani 1 1 d . . . . .
H1O H 0.7788 0.3157 0.4110 0.041 Uiso 1 1 calc R U . . .
N1 N 0.6999(4) 0.1567(6) 0.3291(3) 0.0255(13) Uani 1 1 d . . . . .
O2 O 0.9269(4) 0.4855(6) 0.1901(3) 0.0373(13) Uani 1 1 d . . . . .
N2 N 0.7639(4) 0.3545(6) 0.1471(3) 0.0232(12) Uani 1 1 d . . . . .
C11 C 0.7367(4) 0.1808(7) 0.4686(4) 0.0246(14) Uani 1 1 d . . . . .
C12 C 0.6950(4) 0.1016(7) 0.4036(4) 0.0241(14) Uani 1 1 d . . . . .
C13 C 0.6556(4) -0.0283(7) 0.4116(4) 0.0256(15) Uani 1 1 d . . . . .
C14 C 0.6566(5) -0.0831(7) 0.4855(4) 0.0266(15) Uani 1 1 d . . . . .
C15 C 0.6969(4) -0.0015(7) 0.5487(4) 0.0238(14) Uani 1 1 d . . . . .
C16 C 0.7374(4) 0.1303(7) 0.5432(4) 0.0244(14) Uani 1 1 d . . . . .
C17 C 0.7832(5) 0.2139(8) 0.6155(4) 0.0316(16) Uani 1 1 d . . . . .
C18 C 0.6139(5) -0.2280(8) 0.4946(5) 0.0364(18) Uani 1 1 d . . . . .
C21 C 0.8809(4) 0.5013(7) 0.1150(4) 0.0197(13) Uani 1 1 d . . . . .
C22 C 0.7980(4) 0.4347(6) 0.0905(4) 0.0205(13) Uani 1 1 d . . . . .
C23 C 0.7502(4) 0.4488(6) 0.0150(4) 0.0191(13) Uani 1 1 d . . . . .
C24 C 0.7833(4) 0.5286(6) -0.0382(4) 0.0178(13) Uani 1 1 d . . . . .
C25 C 0.8668(4) 0.5972(7) -0.0119(4) 0.0210(13) Uani 1 1 d . . . . .
C26 C 0.9173(4) 0.5848(7) 0.0641(4) 0.0201(13) Uani 1 1 d . . . . .
C27 C 1.0091(4) 0.6599(7) 0.0894(4) 0.0250(14) Uani 1 1 d . . . . .
C28 C 0.7285(4) 0.5438(7) -0.1211(4) 0.0240(14) Uani 1 1 d . . . . .
C31 C 0.6175(4) 0.2413(6) 0.2061(4) 0.0180(13) Uani 1 1 d . . . . .
C32 C 0.6302(4) 0.2387(6) 0.2858(4) 0.0208(14) Uani 1 1 d . . . . .
C33 C 0.5749(5) 0.3237(7) 0.3239(4) 0.0245(15) Uani 1 1 d . . . . .
C34 C 0.5098(4) 0.4098(7) 0.2828(4) 0.0259(15) Uani 1 1 d . . . . .
C35 C 0.4273(4) 0.5042(7) 0.1567(4) 0.0262(15) Uani 1 1 d . . . . .
C36 C 0.4149(5) 0.5099(8) 0.0786(5) 0.0305(16) Uani 1 1 d . . . . .
C37 C 0.4681(4) 0.4268(7) 0.0390(4) 0.0272(15) Uani 1 1 d . . . . .
C38 C 0.5330(4) 0.3374(7) 0.0799(4) 0.0200(13) Uani 1 1 d . . . . .
C39 C 0.5491(4) 0.3300(6) 0.1617(4) 0.0179(13) Uani 1 1 d . . . . .
C310 C 0.4949(4) 0.4166(7) 0.2009(4) 0.0203(13) Uani 1 1 d . . . . .
C41 C 0.6747(4) 0.1509(6) 0.1661(3) 0.0155(12) Uani 1 1 d . . . . .
C42 C 0.7429(4) 0.2107(6) 0.1350(3) 0.0183(13) Uani 1 1 d . . . . .
C43 C 0.7946(4) 0.1265(7) 0.0945(4) 0.0233(14) Uani 1 1 d . . . . .
C44 C 0.7796(4) -0.0165(7) 0.0856(4) 0.0240(14) Uani 1 1 d . . . . .
C45 C 0.6962(5) -0.2309(7) 0.1105(4) 0.0276(16) Uani 1 1 d . . . . .
C46 C 0.6307(5) -0.2922(8) 0.1409(5) 0.0321(16) Uani 1 1 d . . . . .
C47 C 0.5779(5) -0.2112(8) 0.1808(4) 0.0298(16) Uani 1 1 d . . . . .
C48 C 0.5903(4) -0.0675(7) 0.1889(4) 0.0205(13) Uani 1 1 d . . . . .
C49 C 0.6592(4) 0.0014(7) 0.1584(3) 0.0178(12) Uani 1 1 d . . . . .
C410 C 0.7127(4) -0.0827(7) 0.1185(3) 0.0187(13) Uani 1 1 d . . . . .
C171 C 0.8844(6) 0.2260(11) 0.6167(5) 0.050(2) Uani 1 1 d . . . . .
H17A H 0.8931 0.2727 0.5692 0.075 Uiso 1 1 calc R U . . .
H17B H 0.9112 0.1310 0.6200 0.075 Uiso 1 1 calc R U . . .
H17C H 0.9138 0.2820 0.6618 0.075 Uiso 1 1 calc R U . . .
C172 C 0.7727(6) 0.1412(10) 0.6897(4) 0.044(2) Uani 1 1 d . . . . .
H17D H 0.8027 0.1978 0.7343 0.066 Uiso 1 1 calc R U . . .
H17E H 0.8005 0.0469 0.6925 0.066 Uiso 1 1 calc R U . . .
H17F H 0.7083 0.1319 0.6904 0.066 Uiso 1 1 calc R U . . .
C173 C 0.7424(6) 0.3627(9) 0.6141(5) 0.044(2) Uani 1 1 d . . . . .
H17G H 0.7484 0.4113 0.5663 0.066 Uiso 1 1 calc R U . . .
H17H H 0.7744 0.4167 0.6590 0.066 Uiso 1 1 calc R U . . .
H17I H 0.6782 0.3555 0.6160 0.066 Uiso 1 1 calc R U . . .
C181 C 0.5122(6) -0.2184(11) 0.4628(7) 0.067(3) Uani 1 1 d . . . . .
H18A H 0.5009 -0.1866 0.4087 0.100 Uiso 1 1 calc R U . . .
H18B H 0.4855 -0.1505 0.4936 0.100 Uiso 1 1 calc R U . . .
H18C H 0.4847 -0.3119 0.4655 0.100 Uiso 1 1 calc R U . . .
C182 C 0.6301(6) -0.2776(9) 0.5791(5) 0.046(2) Uani 1 1 d . . . . .
H18D H 0.6016 -0.3703 0.5816 0.069 Uiso 1 1 calc R U . . .
H18E H 0.6038 -0.2088 0.6097 0.069 Uiso 1 1 calc R U . . .
H18F H 0.6953 -0.2853 0.6000 0.069 Uiso 1 1 calc R U . . .
C183 C 0.6565(7) -0.3397(9) 0.4500(5) 0.052(2) Uani 1 1 d . . . . .
H18G H 0.6478 -0.3118 0.3955 0.079 Uiso 1 1 calc R U . . .
H18H H 0.6276 -0.4318 0.4538 0.079 Uiso 1 1 calc R U . . .
H18I H 0.7214 -0.3470 0.4724 0.079 Uiso 1 1 calc R U . . .
C271 C 1.0332(5) 0.7470(10) 0.0222(5) 0.046(2) Uani 1 1 d . . . . .
H27A H 1.0357 0.6838 -0.0214 0.069 Uiso 1 1 calc R U . . .
H27B H 1.0923 0.7923 0.0398 0.069 Uiso 1 1 calc R U . . .
H27C H 0.9870 0.8199 0.0057 0.069 Uiso 1 1 calc R U . . .
C272 C 1.0848(5) 0.5508(9) 0.1151(5) 0.042(2) Uani 1 1 d . . . . .
H27D H 1.0861 0.4848 0.0725 0.063 Uiso 1 1 calc R U . . .
H27E H 1.0734 0.4981 0.1600 0.063 Uiso 1 1 calc R U . . .
H27F H 1.1431 0.5999 0.1292 0.063 Uiso 1 1 calc R U . . .
C273 C 1.0060(5) 0.7634(8) 0.1555(4) 0.0339(17) Uani 1 1 d . . . . .
H27G H 0.9575 0.8326 0.1386 0.051 Uiso 1 1 calc R U . . .
H27H H 1.0642 0.8130 0.1698 0.051 Uiso 1 1 calc R U . . .
H27I H 0.9945 0.7110 0.2004 0.051 Uiso 1 1 calc R U . . .
C281 C 0.7797(6) 0.6212(11) -0.1733(4) 0.047(2) Uani 1 1 d . . . . .
H28A H 0.7419 0.6277 -0.2256 0.070 Uiso 1 1 calc R U . . .
H28B H 0.8354 0.5694 -0.1752 0.070 Uiso 1 1 calc R U . . .
H28C H 0.7949 0.7168 -0.1530 0.070 Uiso 1 1 calc R U . . .
C282 C 0.6401(5) 0.6214(9) -0.1196(4) 0.0364(18) Uani 1 1 d . . . . .
H28D H 0.6069 0.5700 -0.0860 0.055 Uiso 1 1 calc R U . . .
H28E H 0.6031 0.6262 -0.1722 0.055 Uiso 1 1 calc R U . . .
H28F H 0.6535 0.7176 -0.0995 0.055 Uiso 1 1 calc R U . . .
C283 C 0.7053(6) 0.3953(9) -0.1557(4) 0.040(2) Uani 1 1 d . . . . .
H28G H 0.6717 0.3424 -0.1230 0.060 Uiso 1 1 calc R U . . .
H28H H 0.7614 0.3446 -0.1580 0.060 Uiso 1 1 calc R U . . .
H28I H 0.6682 0.4042 -0.2081 0.060 Uiso 1 1 calc R U . . .
C51 C 0.9460(14) 0.055(2) 0.3440(12) 0.135(7) Uani 1 1 d . U . . .
C52 C 0.9937(15) 0.121(2) 0.2931(13) 0.140(8) Uani 1 1 d . U . . .
H52 H 0.9812 0.0901 0.2406 0.169 Uiso 1 1 calc R U . . .
C53 C 1.0608(15) 0.232(2) 0.3152(13) 0.133(7) Uani 1 1 d . U . . .
H53 H 1.0911 0.2760 0.2792 0.159 Uiso 1 1 calc R U . . .
C54 C 1.0773(14) 0.271(2) 0.3942(17) 0.163(8) Uani 1 1 d . U . . .
H54 H 1.1229 0.3393 0.4123 0.196 Uiso 1 1 calc R U . . .
C55 C 1.0294(12) 0.212(3) 0.4482(14) 0.150(8) Uani 1 1 d . U . . .
H55 H 1.0398 0.2465 0.4999 0.180 Uiso 1 1 calc R U . . .
C56 C 0.9631(12) 0.097(2) 0.4228(8) 0.124(7) Uani 1 1 d . U . . .
H56 H 0.9330 0.0517 0.4585 0.149 Uiso 1 1 calc R U . . .
C57 C 0.8847(9) -0.0506(17) 0.3167(11) 0.122(7) Uani 1 1 d . . . . .
H57A H 0.8424 -0.0171 0.2703 0.183 Uiso 1 1 calc R U . . .
H57B H 0.8511 -0.0755 0.3567 0.183 Uiso 1 1 calc R U . . .
H57C H 0.9170 -0.1343 0.3038 0.183 Uiso 1 1 calc R U . . .
O6 O 0.8530(5) 0.3995(8) 0.3281(5) 0.073(2) Uani 1 1 d . . . . .
H6 H 0.9015 0.3535 0.3334 0.088 Uiso 1 1 calc R U . . .
C6 C 0.8707(14) 0.533(2) 0.3624(12) 0.179(12) Uani 1 1 d . . . . .
H6A H 0.8887 0.5227 0.4187 0.269 Uiso 1 1 calc R U . . .
H6B H 0.8161 0.5920 0.3496 0.269 Uiso 1 1 calc R U . . .
H6C H 0.9197 0.5790 0.3427 0.269 Uiso 1 1 calc R U . . .
H1N H 0.731(6) 0.100(9) 0.304(5) 0.05(2) Uiso 1 1 d . . . . .
H2O H 0.901(6) 0.431(10) 0.211(5) 0.04(3) Uiso 1 1 d . . . . .
H2N H 0.738(5) 0.402(8) 0.177(4) 0.03(2) Uiso 1 1 d . . . . .
H13 H 0.623(5) -0.077(8) 0.360(4) 0.03(2) Uiso 1 1 d . . . . .
H15 H 0.700(4) -0.032(7) 0.597(4) 0.012(15) Uiso 1 1 d . . . . .
H23 H 0.691(4) 0.399(7) -0.001(3) 0.011(15) Uiso 1 1 d . . . . .
H25 H 0.894(4) 0.665(8) -0.048(4) 0.023(17) Uiso 1 1 d . . . . .
H33 H 0.584(4) 0.319(6) 0.376(4) 0.009(15) Uiso 1 1 d . . . . .
H34 H 0.480(4) 0.469(8) 0.315(4) 0.023(18) Uiso 1 1 d . . . . .
H35 H 0.394(6) 0.559(11) 0.184(5) 0.06(3) Uiso 1 1 d . . . . .
H36 H 0.371(6) 0.554(10) 0.051(5) 0.05(3) Uiso 1 1 d . . . . .
H37 H 0.453(5) 0.429(7) -0.016(4) 0.026(19) Uiso 1 1 d . . . . .
H38 H 0.564(4) 0.276(7) 0.053(4) 0.012(16) Uiso 1 1 d . . . . .
H43 H 0.837(5) 0.174(8) 0.074(4) 0.026(19) Uiso 1 1 d . . . . .
H44 H 0.820(6) -0.071(9) 0.057(5) 0.05(2) Uiso 1 1 d . . . . .
H45 H 0.729(5) -0.277(9) 0.089(5) 0.03(2) Uiso 1 1 d . . . . .
H46 H 0.619(5) -0.387(9) 0.140(4) 0.03(2) Uiso 1 1 d . . . . .
H47 H 0.531(5) -0.249(9) 0.201(5) 0.04(2) Uiso 1 1 d . . . . .
H48 H 0.557(4) -0.010(8) 0.212(4) 0.019(17) Uiso 1 1 d . . . . .


_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
O1 C11 1.363(8) . ?
O1 H1O 0.8400 . ?
N1 C32 1.398(8) . ?
N1 C12 1.430(8) . ?
N1 H1N 0.89(9) . ?
O2 C21 1.369(8) . ?
O2 H2O 0.78(9) . ?
N2 C42 1.399(8) . ?
N2 C22 1.432(8) . ?
N2 H2N 0.85(8) . ?
C11 C16 1.397(9) . ?
C11 C12 1.403(9) . ?
C12 C13 1.382(10) . ?
C13 C14 1.399(10) . ?
C13 H13 1.04(8) . ?
C14 C15 1.387(10) . ?
C14 C18 1.534(10) . ?
C15 C16 1.397(10) . ?
C15 H15 0.90(7) . ?
C16 C17 1.537(9) . ?
C17 C172 1.515(11) . ?
C17 C171 1.529(11) . ?
C17 C173 1.530(11) . ?
C18 C181 1.524(12) . ?
C18 C182 1.533(11) . ?
C18 C183 1.535(11) . ?
C21 C22 1.388(8) . ?
C21 C26 1.391(8) . ?
C22 C23 1.383(9) . ?
C23 C24 1.376(9) . ?
C23 H23 1.00(6) . ?
C24 C25 1.406(9) . ?
C24 C28 1.529(9) . ?
C25 C26 1.404(9) . ?
C25 H25 1.05(7) . ?
C26 C27 1.537(8) . ?
C27 C273 1.528(10) . ?
C27 C272 1.534(10) . ?
C27 C271 1.547(10) . ?
C28 C281 1.508(10) . ?
C28 C282 1.529(9) . ?
C28 C283 1.539(10) . ?
C31 C32 1.379(9) . ?
C31 C39 1.430(8) . ?
C31 C41 1.491(8) . ?
C32 C33 1.424(9) . ?
C33 C34 1.362(10) . ?
C33 H33 0.91(6) . ?
C34 C310 1.416(10) . ?
C34 H34 0.98(7) . ?
C35 C36 1.352(11) . ?
C35 C310 1.415(9) . ?
C35 H35 0.93(9) . ?
C36 C37 1.408(11) . ?
C36 H36 0.85(9) . ?
C37 C38 1.378(9) . ?
C37 H37 0.94(7) . ?
C38 C39 1.414(9) . ?
C38 H38 0.94(6) . ?
C39 C310 1.433(8) . ?
C41 C42 1.385(8) . ?
C41 C49 1.431(8) . ?
C42 C43 1.409(9) . ?
C43 C44 1.370(10) . ?
C43 H43 0.92(7) . ?
C44 C410 1.411(9) . ?
C44 H44 1.01(9) . ?
C45 C46 1.350(10) . ?
C45 C410 1.422(9) . ?
C45 H45 0.81(8) . ?
C46 C47 1.397(11) . ?
C46 H46 0.91(8) . ?
C47 C48 1.371(10) . ?
C47 H47 0.93(8) . ?
C48 C49 1.425(9) . ?
C48 H48 0.89(7) . ?
C49 C410 1.419(8) . ?
C171 H17A 0.9800 . ?
C171 H17B 0.9800 . ?
C171 H17C 0.9800 . ?
C172 H17D 0.9800 . ?
C172 H17E 0.9800 . ?
C172 H17F 0.9800 . ?
C173 H17G 0.9800 . ?
C173 H17H 0.9800 . ?
C173 H17I 0.9800 . ?
C181 H18A 0.9800 . ?
C181 H18B 0.9800 . ?
C181 H18C 0.9800 . ?
C182 H18D 0.9800 . ?
C182 H18E 0.9800 . ?
C182 H18F 0.9800 . ?
C183 H18G 0.9800 . ?
C183 H18H 0.9800 . ?
C183 H18I 0.9800 . ?
C271 H27A 0.9800 . ?
C271 H27B 0.9800 . ?
C271 H27C 0.9800 . ?
C272 H27D 0.9800 . ?
C272 H27E 0.9800 . ?
C272 H27F 0.9800 . ?
C273 H27G 0.9800 . ?
C273 H27H 0.9800 . ?
C273 H27I 0.9800 . ?
C281 H28A 0.9800 . ?
C281 H28B 0.9800 . ?
C281 H28C 0.9800 . ?
C282 H28D 0.9800 . ?
C282 H28E 0.9800 . ?
C282 H28F 0.9800 . ?
C283 H28G 0.9800 . ?
C283 H28H 0.9800 . ?
C283 H28I 0.9800 . ?
C51 C57 1.38(2) . ?
C51 C52 1.41(2) . ?
C51 C56 1.42(2) . ?
C52 C53 1.46(3) . ?
C52 H52 0.9500 . ?
C53 C54 1.41(3) . ?
C53 H53 0.9500 . ?
C54 C55 1.42(3) . ?
C54 H54 0.9500 . ?
C55 C56 1.48(3) . ?
C55 H55 0.9500 . ?
C56 H56 0.9500 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
O6 C6 1.401(16) . ?
O6 H6 0.8400 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 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
C11 O1 H1O 109.5 . . ?
C32 N1 C12 121.7(5) . . ?
C32 N1 H1N 119(5) . . ?
C12 N1 H1N 111(5) . . ?
C21 O2 H2O 109(6) . . ?
C42 N2 C22 120.6(5) . . ?
C42 N2 H2N 119(5) . . ?
C22 N2 H2N 116(5) . . ?
O1 C11 C16 120.7(6) . . ?
O1 C11 C12 119.2(6) . . ?
C16 C11 C12 120.2(6) . . ?
C13 C12 C11 121.2(6) . . ?
C13 C12 N1 121.4(6) . . ?
C11 C12 N1 117.3(6) . . ?
C12 C13 C14 120.1(6) . . ?
C12 C13 H13 116(4) . . ?
C14 C13 H13 124(4) . . ?
C15 C14 C13 117.6(6) . . ?
C15 C14 C18 122.2(6) . . ?
C13 C14 C18 120.2(6) . . ?
C14 C15 C16 124.2(6) . . ?
C14 C15 H15 121(4) . . ?
C16 C15 H15 115(4) . . ?
C15 C16 C11 116.9(6) . . ?
C15 C16 C17 121.7(6) . . ?
C11 C16 C17 121.4(6) . . ?
C172 C17 C171 107.8(7) . . ?
C172 C17 C173 108.4(6) . . ?
C171 C17 C173 109.3(7) . . ?
C172 C17 C16 112.0(6) . . ?
C171 C17 C16 109.0(6) . . ?
C173 C17 C16 110.3(6) . . ?
C181 C18 C182 108.7(7) . . ?
C181 C18 C14 108.8(7) . . ?
C182 C18 C14 112.8(7) . . ?
C181 C18 C183 110.5(8) . . ?
C182 C18 C183 106.8(7) . . ?
C14 C18 C183 109.1(6) . . ?
O2 C21 C22 119.7(6) . . ?
O2 C21 C26 119.8(5) . . ?
C22 C21 C26 120.5(6) . . ?
C23 C22 C21 120.9(6) . . ?
C23 C22 N2 122.1(6) . . ?
C21 C22 N2 117.0(6) . . ?
C24 C23 C22 121.2(6) . . ?
C24 C23 H23 120(3) . . ?
C22 C23 H23 119(3) . . ?
C23 C24 C25 117.1(6) . . ?
C23 C24 C28 120.1(5) . . ?
C25 C24 C28 122.8(6) . . ?
C26 C25 C24 123.3(6) . . ?
C26 C25 H25 115(4) . . ?
C24 C25 H25 121(4) . . ?
C21 C26 C25 117.0(5) . . ?
C21 C26 C27 121.8(6) . . ?
C25 C26 C27 121.1(5) . . ?
C273 C27 C272 110.0(6) . . ?
C273 C27 C26 110.3(5) . . ?
C272 C27 C26 110.3(6) . . ?
C273 C27 C271 107.2(6) . . ?
C272 C27 C271 107.6(6) . . ?
C26 C27 C271 111.4(6) . . ?
C281 C28 C282 109.9(6) . . ?
C281 C28 C24 112.7(6) . . ?
C282 C28 C24 109.2(5) . . ?
C281 C28 C283 107.6(6) . . ?
C282 C28 C283 108.3(6) . . ?
C24 C28 C283 109.1(6) . . ?
C32 C31 C39 120.0(5) . . ?
C32 C31 C41 120.1(5) . . ?
C39 C31 C41 120.0(5) . . ?
C31 C32 N1 119.7(6) . . ?
C31 C32 C33 120.1(6) . . ?
N1 C32 C33 120.2(6) . . ?
C34 C33 C32 120.9(6) . . ?
C34 C33 H33 121(4) . . ?
C32 C33 H33 118(4) . . ?
C33 C34 C310 120.9(6) . . ?
C33 C34 H34 113(4) . . ?
C310 C34 H34 125(4) . . ?
C36 C35 C310 121.1(7) . . ?
C36 C35 H35 122(6) . . ?
C310 C35 H35 117(6) . . ?
C35 C36 C37 120.8(7) . . ?
C35 C36 H36 122(6) . . ?
C37 C36 H36 117(6) . . ?
C38 C37 C36 119.8(7) . . ?
C38 C37 H37 123(4) . . ?
C36 C37 H37 117(4) . . ?
C37 C38 C39 121.1(6) . . ?
C37 C38 H38 119(4) . . ?
C39 C38 H38 120(4) . . ?
C38 C39 C31 122.6(6) . . ?
C38 C39 C310 118.1(5) . . ?
C31 C39 C310 119.3(5) . . ?
C35 C310 C34 122.2(6) . . ?
C35 C310 C39 119.0(6) . . ?
C34 C310 C39 118.8(6) . . ?
C42 C41 C49 118.9(5) . . ?
C42 C41 C31 120.5(5) . . ?
C49 C41 C31 120.6(5) . . ?
C41 C42 N2 119.8(6) . . ?
C41 C42 C43 120.6(6) . . ?
N2 C42 C43 119.5(6) . . ?
C44 C43 C42 121.1(6) . . ?
C44 C43 H43 123(5) . . ?
C42 C43 H43 116(5) . . ?
C43 C44 C410 120.3(6) . . ?
C43 C44 H44 117(5) . . ?
C410 C44 H44 123(5) . . ?
C46 C45 C410 120.7(7) . . ?
C46 C45 H45 122(6) . . ?
C410 C45 H45 118(6) . . ?
C45 C46 C47 120.6(7) . . ?
C45 C46 H46 125(5) . . ?
C47 C46 H46 115(5) . . ?
C48 C47 C46 120.9(7) . . ?
C48 C47 H47 116(5) . . ?
C46 C47 H47 123(5) . . ?
C47 C48 C49 120.4(6) . . ?
C47 C48 H48 125(4) . . ?
C49 C48 H48 115(4) . . ?
C410 C49 C48 118.0(6) . . ?
C410 C49 C41 120.0(5) . . ?
C48 C49 C41 122.0(6) . . ?
C44 C410 C49 119.1(6) . . ?
C44 C410 C45 121.4(6) . . ?
C49 C410 C45 119.5(6) . . ?
C17 C171 H17A 109.5 . . ?
C17 C171 H17B 109.5 . . ?
H17A C171 H17B 109.5 . . ?
C17 C171 H17C 109.5 . . ?
H17A C171 H17C 109.5 . . ?
H17B C171 H17C 109.5 . . ?
C17 C172 H17D 109.5 . . ?
C17 C172 H17E 109.5 . . ?
H17D C172 H17E 109.5 . . ?
C17 C172 H17F 109.5 . . ?
H17D C172 H17F 109.5 . . ?
H17E C172 H17F 109.5 . . ?
C17 C173 H17G 109.5 . . ?
C17 C173 H17H 109.5 . . ?
H17G C173 H17H 109.5 . . ?
C17 C173 H17I 109.5 . . ?
H17G C173 H17I 109.5 . . ?
H17H C173 H17I 109.5 . . ?
C18 C181 H18A 109.5 . . ?
C18 C181 H18B 109.5 . . ?
H18A C181 H18B 109.5 . . ?
C18 C181 H18C 109.5 . . ?
H18A C181 H18C 109.5 . . ?
H18B C181 H18C 109.5 . . ?
C18 C182 H18D 109.5 . . ?
C18 C182 H18E 109.5 . . ?
H18D C182 H18E 109.5 . . ?
C18 C182 H18F 109.5 . . ?
H18D C182 H18F 109.5 . . ?
H18E C182 H18F 109.5 . . ?
C18 C183 H18G 109.5 . . ?
C18 C183 H18H 109.5 . . ?
H18G C183 H18H 109.5 . . ?
C18 C183 H18I 109.5 . . ?
H18G C183 H18I 109.5 . . ?
H18H C183 H18I 109.5 . . ?
C27 C271 H27A 109.5 . . ?
C27 C271 H27B 109.5 . . ?
H27A C271 H27B 109.5 . . ?
C27 C271 H27C 109.5 . . ?
H27A C271 H27C 109.5 . . ?
H27B C271 H27C 109.5 . . ?
C27 C272 H27D 109.5 . . ?
C27 C272 H27E 109.5 . . ?
H27D C272 H27E 109.5 . . ?
C27 C272 H27F 109.5 . . ?
H27D C272 H27F 109.5 . . ?
H27E C272 H27F 109.5 . . ?
C27 C273 H27G 109.5 . . ?
C27 C273 H27H 109.5 . . ?
H27G C273 H27H 109.5 . . ?
C27 C273 H27I 109.5 . . ?
H27G C273 H27I 109.5 . . ?
H27H C273 H27I 109.5 . . ?
C28 C281 H28A 109.5 . . ?
C28 C281 H28B 109.5 . . ?
H28A C281 H28B 109.5 . . ?
C28 C281 H28C 109.5 . . ?
H28A C281 H28C 109.5 . . ?
H28B C281 H28C 109.5 . . ?
C28 C282 H28D 109.5 . . ?
C28 C282 H28E 109.5 . . ?
H28D C282 H28E 109.5 . . ?
C28 C282 H28F 109.5 . . ?
H28D C282 H28F 109.5 . . ?
H28E C282 H28F 109.5 . . ?
C28 C283 H28G 109.5 . . ?
C28 C283 H28H 109.5 . . ?
H28G C283 H28H 109.5 . . ?
C28 C283 H28I 109.5 . . ?
H28G C283 H28I 109.5 . . ?
H28H C283 H28I 109.5 . . ?
C57 C51 C52 119(2) . . ?
C57 C51 C56 121(2) . . ?
C52 C51 C56 119(2) . . ?
C51 C52 C53 125(2) . . ?
C51 C52 H52 117.7 . . ?
C53 C52 H52 117.7 . . ?
C54 C53 C52 115(2) . . ?
C54 C53 H53 122.6 . . ?
C52 C53 H53 122.6 . . ?
C53 C54 C55 124(2) . . ?
C53 C54 H54 118.2 . . ?
C55 C54 H54 118.2 . . ?
C54 C55 C56 119(2) . . ?
C54 C55 H55 120.4 . . ?
C56 C55 H55 120.4 . . ?
C51 C56 C55 118(2) . . ?
C51 C56 H56 120.9 . . ?
C55 C56 H56 120.9 . . ?
C51 C57 H57A 109.5 . . ?
C51 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
C51 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C6 O6 H6 109.5 . . ?
O6 C6 H6A 109.5 . . ?
O6 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
O6 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?

_refine_diff_density_max         0.630
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.069

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_pseudorac
_database_code_depnum_ccdc_archive 'CCDC 2281684'
loop_
_audit_author_name
_audit_author_address
'Seth Brown'
;University of Notre Dame
United States of America
;
_audit_update_record             
;
2023-07-14 deposited with the CCDC.	2023-08-28 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT213_pseudorac           
;
PROBLEM: Atom C282 has ADP max/min Ratio ..... 4.1 prolat
RESPONSE: There is slight unmodeled disorder in this tert-butyl
group.
;
_vrf_PLAT220_pseudorac           
;
PROBLEM: NonSolvent Resd 1  C Ueq(max)/Ueq(min) Range 6.3 Ratio 
RESPONSE: This residue includes slightly disordered tert-butyl 
groups.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
'(A,R,R)-Oxo(2,3-butanediylbis(2-(2-oxy-3,5-di-tert-butylphenyl)amido)benzoate)osmium (C,R,R)-Oxo(2,3-butanediylbis(2-(2-oxy-3,5-di-tert-butylphenyl)amido)benzoate)osmium cocrystal'
_chemical_name_common            '(A,R,R)-(Bdan)OsO . (C,R,R)-(Bdan)OsO'
_chemical_melting_point          ?
_chemical_formula_moiety         'C46 H56 N2 O7 Os, C46 H56 N2 O7 Os'
_chemical_formula_sum            'C92 H112 N4 O14 Os2'
_chemical_formula_weight         1878.25

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Os Os -4.9801 6.2216 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_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+1/2, -z'

_cell_length_a                   12.7971(4)
_cell_length_b                   13.0573(4)
_cell_length_c                   25.7200(8)
_cell_angle_alpha                90
_cell_angle_beta                 95.8873(15)
_cell_angle_gamma                90
_cell_volume                     4275.0(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9892
_cell_measurement_theta_min      3.801
_cell_measurement_theta_max      72.404

_exptl_crystal_description       block
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_F_000             1912
_exptl_transmission_factor_min   0.6472
_exptl_transmission_factor_max   0.7536
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.083
_exptl_crystal_size_min          0.081
_exptl_absorpt_coefficient_mu    6.049
_shelx_estimated_absorpt_T_min   0.531
_shelx_estimated_absorpt_T_max   0.640
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6472
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_process_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10.
;

_exptl_crystal_recrystallization_method 
'BdanH4 was metalated with OsO(OCH2CH2O) in benzene at 80 degC, and the crude material chromatogaphed on silica gel, eluting with 1:2 hexane:dichloromethane.  Crystals were deposited from a hexane solution of the eluate.'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.33
_diffrn_reflns_number            93554
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_av_R_equivalents  0.0340
_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       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         1.727
_diffrn_reflns_theta_max         72.520
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             16870
_reflns_number_gt                15998
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.907
_reflns_Friedel_fraction_max     0.993
_reflns_Friedel_fraction_full    0.997

_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0271P)²+0.5870P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     heavy
_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_abs_structure_details 
;
 Flack x determined using 7282 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.003(4)
_chemical_absolute_configuration rmad
_refine_ls_number_reflns         16870
_refine_ls_number_parameters     1009
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0213
_refine_ls_R_factor_gt           0.0195
_refine_ls_wR_factor_ref         0.0479
_refine_ls_wR_factor_gt          0.0471
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.001
_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
Os1 Os 0.29735(2) 0.18404(2) 0.38048(2) 0.01602(6) Uani 1 1 d . . . . .
Os2 Os 0.20595(2) 0.31593(2) 0.11762(2) 0.01575(6) Uani 1 1 d . . . . .
O1 O 0.4119(3) 0.1697(4) 0.35278(14) 0.0264(9) Uani 1 1 d . . . . .
O2 O 0.0931(3) 0.3321(4) 0.14661(13) 0.0238(8) Uani 1 1 d . . . . .
O11 O 0.2941(3) 0.3240(4) 0.40395(12) 0.0216(8) Uani 1 1 d . . . . .
O21 O 0.2270(3) 0.0524(3) 0.37323(13) 0.0209(7) Uani 1 1 d . . . . .
O31 O 0.2800(3) 0.4458(3) 0.12306(13) 0.0192(7) Uani 1 1 d . . . . .
O41 O 0.2071(3) 0.1743(3) 0.09425(12) 0.0194(7) Uani 1 1 d . . . . .
O3 O 0.0940(2) 0.1210(3) 0.46749(12) 0.0269(7) Uani 1 1 d . . . . .
O30 O 0.0930(3) 0.1048(4) 0.55494(16) 0.0453(12) Uani 1 1 d . . . . .
O4 O 0.0408(3) 0.2847(3) 0.40058(17) 0.0359(10) Uani 1 1 d . . . . .
O40 O -0.0994(3) 0.3635(5) 0.35976(19) 0.0482(13) Uani 1 1 d . . . . .
O7 O 0.4765(3) 0.2355(3) 0.10514(15) 0.0269(8) Uani 1 1 d . . . . .
O70 O 0.6105(3) 0.1448(4) 0.14443(17) 0.0390(10) Uani 1 1 d . . . . .
O8 O 0.3898(2) 0.3398(3) 0.01762(12) 0.0242(6) Uani 1 1 d . . . . .
O80 O 0.3883(3) 0.3789(4) -0.06763(15) 0.0386(10) Uani 1 1 d . . . . .
N11 N 0.3151(3) 0.1604(4) 0.45507(16) 0.0173(9) Uani 1 1 d . . . . .
N21 N 0.1817(3) 0.2208(4) 0.33047(16) 0.0191(9) Uani 1 1 d . . . . .
N31 N 0.3213(3) 0.2784(4) 0.16850(16) 0.0177(9) Uani 1 1 d . . . . .
N41 N 0.1812(3) 0.3372(4) 0.04288(16) 0.0177(9) Uani 1 1 d . . . . .
C1 C -0.0745(5) 0.0946(5) 0.4198(3) 0.0350(13) Uani 1 1 d . . . . .
H1A H -0.0720 0.0227 0.4308 0.052 Uiso 1 1 calc R U . . .
H1B H -0.0433 0.1015 0.3868 0.052 Uiso 1 1 calc R U . . .
H1C H -0.1478 0.1177 0.4151 0.052 Uiso 1 1 calc R U . . .
C2 C -0.0137(3) 0.1591(3) 0.46116(18) 0.0288(9) Uani 1 1 d . . . . .
H2 H -0.0451 0.1502 0.4949 0.035 Uiso 1 1 calc R U . . .
C3 C -0.0127(4) 0.2715(4) 0.4480(2) 0.0367(11) Uani 1 1 d . . . . .
H3 H -0.0868 0.2961 0.4409 0.044 Uiso 1 1 calc R U . . .
C4 C 0.0441(6) 0.3387(7) 0.4894(3) 0.059(2) Uani 1 1 d . . . . .
H4A H 0.0409 0.4101 0.4776 0.088 Uiso 1 1 calc R U . . .
H4B H 0.1177 0.3171 0.4956 0.088 Uiso 1 1 calc R U . . .
H4C H 0.0108 0.3325 0.5219 0.088 Uiso 1 1 calc R U . . .
C5 C 0.5797(5) 0.3823(5) 0.0839(2) 0.0335(13) Uani 1 1 d . . . . .
H5A H 0.6204 0.3786 0.1183 0.050 Uiso 1 1 calc R U . . .
H5B H 0.5188 0.4270 0.0859 0.050 Uiso 1 1 calc R U . . .
H5C H 0.6240 0.4100 0.0584 0.050 Uiso 1 1 calc R U . . .
C6 C 0.5426(3) 0.2757(4) 0.06716(18) 0.0275(9) Uani 1 1 d . . . . .
H6 H 0.6054 0.2303 0.0666 0.033 Uiso 1 1 calc R U . . .
C7 C 0.4784(3) 0.2696(3) 0.01448(17) 0.0265(8) Uani 1 1 d . . . . .
H7 H 0.5219 0.2936 -0.0133 0.032 Uiso 1 1 calc R U . . .
C8 C 0.4367(4) 0.1639(5) 0.0012(2) 0.0304(11) Uani 1 1 d . . . . .
H8A H 0.3960 0.1652 -0.0333 0.046 Uiso 1 1 calc R U . . .
H8B H 0.3913 0.1419 0.0275 0.046 Uiso 1 1 calc R U . . .
H8C H 0.4955 0.1160 0.0005 0.046 Uiso 1 1 calc R U . . .
C11 C 0.3166(4) 0.3400(4) 0.45656(19) 0.0188(11) Uani 1 1 d . . . . .
C12 C 0.3271(4) 0.2508(5) 0.4866(2) 0.0166(10) Uani 1 1 d . . . . .
C13 C 0.3457(4) 0.2547(5) 0.5406(2) 0.0200(11) Uani 1 1 d . . . . .
H13 H 0.3537 0.1934 0.5606 0.024 Uiso 1 1 calc R U . . .
C14 C 0.3526(4) 0.3503(5) 0.5652(2) 0.0221(11) Uani 1 1 d . . . . .
C15 C 0.3419(4) 0.4382(5) 0.5341(2) 0.0224(11) Uani 1 1 d . . . . .
H15 H 0.3465 0.5029 0.5510 0.027 Uiso 1 1 calc R U . . .
C16 C 0.3244(4) 0.4366(5) 0.4789(2) 0.0213(11) Uani 1 1 d . . . . .
C17 C 0.3159(5) 0.5342(5) 0.4459(2) 0.0245(12) Uani 1 1 d . . . . .
C18 C 0.3689(5) 0.3549(5) 0.6247(2) 0.0254(12) Uani 1 1 d . . . . .
C21 C 0.1431(4) 0.0467(5) 0.3357(2) 0.0193(10) Uani 1 1 d . . . . .
C22 C 0.1143(4) 0.1394(4) 0.31224(19) 0.0188(10) Uani 1 1 d . . . . .
C23 C 0.0286(4) 0.1486(5) 0.2743(2) 0.0228(11) Uani 1 1 d . . . . .
H23 H 0.0103 0.2129 0.2586 0.027 Uiso 1 1 calc R U . . .
C24 C -0.0296(4) 0.0608(5) 0.2599(2) 0.0239(11) Uani 1 1 d . . . . .
C25 C 0.0023(4) -0.0327(5) 0.2839(2) 0.0236(11) Uani 1 1 d . . . . .
H25 H -0.0373 -0.0923 0.2737 0.028 Uiso 1 1 calc R U . . .
C26 C 0.0879(4) -0.0435(5) 0.3215(2) 0.0223(11) Uani 1 1 d . . . . .
C27 C 0.1217(4) -0.1476(5) 0.3453(2) 0.0238(11) Uani 1 1 d . . . . .
C28 C -0.1296(4) 0.0700(5) 0.2223(2) 0.0278(12) Uani 1 1 d . . . . .
C30 C 0.1356(4) 0.0933(4) 0.5157(2) 0.0266(11) Uani 1 1 d . . . . .
C31 C 0.2362(4) 0.0369(5) 0.51287(18) 0.0198(10) Uani 1 1 d . . . . .
C32 C 0.3134(4) 0.0632(5) 0.47991(19) 0.0176(10) Uani 1 1 d . . . . .
C33 C 0.3946(4) -0.0056(5) 0.4740(2) 0.0220(11) Uani 1 1 d . . . . .
H33 H 0.4458 0.0108 0.4511 0.026 Uiso 1 1 calc R U . . .
C34 C 0.4020(5) -0.0980(5) 0.5011(2) 0.0256(12) Uani 1 1 d . . . . .
H34 H 0.4555 -0.1459 0.4954 0.031 Uiso 1 1 calc R U . . .
C35 C 0.3309(5) -0.1194(5) 0.5364(2) 0.0278(12) Uani 1 1 d . . . . .
H35 H 0.3386 -0.1800 0.5569 0.033 Uiso 1 1 calc R U . . .
C36 C 0.2484(4) -0.0534(5) 0.54226(19) 0.0249(11) Uani 1 1 d . . . . .
H36 H 0.1995 -0.0694 0.5665 0.030 Uiso 1 1 calc R U . . .
C40 C -0.0091(4) 0.3392(5) 0.3618(2) 0.0269(12) Uani 1 1 d . . . . .
C41 C 0.0646(5) 0.3731(5) 0.3237(2) 0.0251(12) Uani 1 1 d . . . . .
C42 C 0.1562(4) 0.3225(6) 0.31316(18) 0.0210(10) Uani 1 1 d . . . . .
C43 C 0.2261(5) 0.3707(5) 0.2838(2) 0.0283(13) Uani 1 1 d . . . . .
H43 H 0.2898 0.3373 0.2779 0.034 Uiso 1 1 calc R U . . .
C44 C 0.2045(6) 0.4681(5) 0.2626(2) 0.0331(14) Uani 1 1 d . . . . .
H44 H 0.2538 0.5014 0.2431 0.040 Uiso 1 1 calc R U . . .
C45 C 0.1111(6) 0.5151(6) 0.2703(2) 0.0370(15) Uani 1 1 d . . . . .
H45 H 0.0946 0.5799 0.2548 0.044 Uiso 1 1 calc R U . . .
C46 C 0.0413(5) 0.4689(6) 0.3003(2) 0.0338(14) Uani 1 1 d . . . . .
H46 H -0.0231 0.5020 0.3051 0.041 Uiso 1 1 calc R U . . .
C51 C 0.3630(4) 0.4510(5) 0.16140(19) 0.0195(10) Uani 1 1 d . . . . .
C52 C 0.3890(4) 0.3580(4) 0.18618(19) 0.0187(10) Uani 1 1 d . . . . .
C53 C 0.4725(4) 0.3510(5) 0.2248(2) 0.0224(11) Uani 1 1 d . . . . .
H53 H 0.4887 0.2874 0.2417 0.027 Uiso 1 1 calc R U . . .
C54 C 0.5326(4) 0.4373(5) 0.2388(2) 0.0241(11) Uani 1 1 d . . . . .
C55 C 0.5040(4) 0.5297(5) 0.2140(2) 0.0248(12) Uani 1 1 d . . . . .
H55 H 0.5447 0.5887 0.2239 0.030 Uiso 1 1 calc R U . . .
C56 C 0.4187(4) 0.5409(5) 0.1753(2) 0.0213(11) Uani 1 1 d . . . . .
C57 C 0.3854(4) 0.6453(5) 0.1513(2) 0.0235(11) Uani 1 1 d . . . . .
C58 C 0.6320(4) 0.4289(6) 0.2781(2) 0.0289(13) Uani 1 1 d . . . . .
C61 C 0.1797(4) 0.1590(4) 0.0419(2) 0.0199(11) Uani 1 1 d . . . . .
C62 C 0.1683(4) 0.2486(5) 0.0120(2) 0.0209(11) Uani 1 1 d . . . . .
C63 C 0.1470(4) 0.2425(5) -0.0417(2) 0.0209(11) Uani 1 1 d . . . . .
H63 H 0.1376 0.3032 -0.0620 0.025 Uiso 1 1 calc R U . . .
C64 C 0.1393(4) 0.1466(5) -0.0661(2) 0.0203(11) Uani 1 1 d . . . . .
C65 C 0.1508(4) 0.0589(5) -0.0348(2) 0.0219(11) Uani 1 1 d . . . . .
H65 H 0.1457 -0.0061 -0.0515 0.026 Uiso 1 1 calc R U . . .
C66 C 0.1694(4) 0.0616(5) 0.0192(2) 0.0200(11) Uani 1 1 d . . . . .
C67 C 0.1819(5) -0.0355(5) 0.0535(2) 0.0260(12) Uani 1 1 d . . . . .
C68 C 0.1214(4) 0.1401(5) -0.1263(2) 0.0260(12) Uani 1 1 d . . . . .
C70 C 0.5205(4) 0.1705(5) 0.14133(19) 0.0252(11) Uani 1 1 d . . . . .
C71 C 0.4424(4) 0.1282(5) 0.1752(2) 0.0219(11) Uani 1 1 d . . . . .
C72 C 0.3471(4) 0.1753(5) 0.18451(18) 0.0212(10) Uani 1 1 d . . . . .
C73 C 0.2760(5) 0.1248(5) 0.2122(2) 0.0264(12) Uani 1 1 d . . . . .
H73 H 0.2116 0.1570 0.2179 0.032 Uiso 1 1 calc R U . . .
C74 C 0.2979(6) 0.0275(5) 0.2317(2) 0.0341(14) Uani 1 1 d . . . . .
H74 H 0.2476 -0.0078 0.2497 0.041 Uiso 1 1 calc R U . . .
C75 C 0.3929(6) -0.0184(5) 0.2250(2) 0.0338(14) Uani 1 1 d . . . . .
H75 H 0.4094 -0.0836 0.2400 0.041 Uiso 1 1 calc R U . . .
C76 C 0.4639(5) 0.0307(5) 0.1965(2) 0.0287(13) Uani 1 1 d . . . . .
H76 H 0.5282 -0.0022 0.1913 0.034 Uiso 1 1 calc R U . . .
C80 C 0.3524(4) 0.3866(4) -0.0267(2) 0.0251(10) Uani 1 1 d . . . . .
C81 C 0.2617(4) 0.4554(5) -0.01771(18) 0.0205(10) Uani 1 1 d . . . . .
C82 C 0.1876(4) 0.4345(5) 0.01686(19) 0.0183(10) Uani 1 1 d . . . . .
C83 C 0.1127(4) 0.5068(5) 0.0261(2) 0.0221(11) Uani 1 1 d . . . . .
H83 H 0.0641 0.4931 0.0507 0.027 Uiso 1 1 calc R U . . .
C84 C 0.1085(4) 0.5995(5) -0.0006(2) 0.0251(12) Uani 1 1 d . . . . .
H84 H 0.0571 0.6491 0.0060 0.030 Uiso 1 1 calc R U . . .
C85 C 0.1788(5) 0.6199(5) -0.0369(2) 0.0252(12) Uani 1 1 d . . . . .
H85 H 0.1750 0.6827 -0.0556 0.030 Uiso 1 1 calc R U . . .
C86 C 0.2551(4) 0.5474(5) -0.0455(2) 0.0240(11) Uani 1 1 d . . . . .
H86 H 0.3030 0.5606 -0.0706 0.029 Uiso 1 1 calc R U . . .
C171 C 0.3355(6) 0.6300(5) 0.4794(3) 0.0346(14) Uani 1 1 d . . . . .
H17A H 0.3291 0.6908 0.4570 0.052 Uiso 1 1 calc R U . . .
H17B H 0.4063 0.6271 0.4979 0.052 Uiso 1 1 calc R U . . .
H17C H 0.2836 0.6335 0.5049 0.052 Uiso 1 1 calc R U . . .
C172 C 0.3954(5) 0.5333(5) 0.4055(2) 0.0297(13) Uani 1 1 d . . . . .
H17D H 0.3884 0.5964 0.3848 0.045 Uiso 1 1 calc R U . . .
H17E H 0.3822 0.4741 0.3824 0.045 Uiso 1 1 calc R U . . .
H17F H 0.4666 0.5290 0.4234 0.045 Uiso 1 1 calc R U . . .
C173 C 0.2036(5) 0.5410(6) 0.4182(2) 0.0325(13) Uani 1 1 d . . . . .
H17G H 0.1967 0.6032 0.3969 0.049 Uiso 1 1 calc R U . . .
H17H H 0.1532 0.5432 0.4444 0.049 Uiso 1 1 calc R U . . .
H17I H 0.1895 0.4809 0.3958 0.049 Uiso 1 1 calc R U . . .
C181 C 0.2707(5) 0.3127(8) 0.6474(2) 0.0404(14) Uani 1 1 d . . . . .
H18A H 0.2094 0.3538 0.6346 0.061 Uiso 1 1 calc R U . . .
H18B H 0.2810 0.3159 0.6856 0.061 Uiso 1 1 calc R U . . .
H18C H 0.2594 0.2413 0.6363 0.061 Uiso 1 1 calc R U . . .
C182 C 0.4634(6) 0.2909(6) 0.6449(2) 0.0430(18) Uani 1 1 d . . . . .
H18D H 0.4735 0.2947 0.6831 0.064 Uiso 1 1 calc R U . . .
H18E H 0.5262 0.3172 0.6305 0.064 Uiso 1 1 calc R U . . .
H18F H 0.4517 0.2195 0.6340 0.064 Uiso 1 1 calc R U . . .
C183 C 0.3881(6) 0.4650(6) 0.6452(2) 0.0375(15) Uani 1 1 d . . . . .
H18G H 0.3279 0.5082 0.6329 0.056 Uiso 1 1 calc R U . . .
H18H H 0.4518 0.4924 0.6323 0.056 Uiso 1 1 calc R U . . .
H18I H 0.3966 0.4644 0.6835 0.056 Uiso 1 1 calc R U . . .
C271 C 0.1291(7) -0.1425(6) 0.4043(3) 0.0489(19) Uani 1 1 d . . . . .
H27A H 0.0605 -0.1235 0.4153 0.073 Uiso 1 1 calc R U . . .
H27B H 0.1814 -0.0911 0.4170 0.073 Uiso 1 1 calc R U . . .
H27C H 0.1500 -0.2096 0.4190 0.073 Uiso 1 1 calc R U . . .
C272 C 0.0424(6) -0.2316(6) 0.3276(4) 0.056(2) Uani 1 1 d . . . . .
H27D H 0.0360 -0.2370 0.2894 0.084 Uiso 1 1 calc R U . . .
H27E H -0.0262 -0.2145 0.3391 0.084 Uiso 1 1 calc R U . . .
H27F H 0.0666 -0.2972 0.3430 0.084 Uiso 1 1 calc R U . . .
C273 C 0.2276(5) -0.1774(7) 0.3276(3) 0.0457(17) Uani 1 1 d . . . . .
H27G H 0.2218 -0.1805 0.2893 0.069 Uiso 1 1 calc R U . . .
H27H H 0.2486 -0.2447 0.3420 0.069 Uiso 1 1 calc R U . . .
H27I H 0.2804 -0.1263 0.3400 0.069 Uiso 1 1 calc R U . . .
C281 C -0.2197(6) 0.0921(12) 0.2548(3) 0.089(5) Uani 1 1 d . . . . .
H28A H -0.2044 0.1545 0.2754 0.133 Uiso 1 1 calc R U . . .
H28B H -0.2282 0.0344 0.2784 0.133 Uiso 1 1 calc R U . . .
H28C H -0.2847 0.1016 0.2316 0.133 Uiso 1 1 calc R U . . .
C282 C -0.1529(9) -0.0258(9) 0.1913(5) 0.106(5) Uani 1 1 d . . . . .
H28D H -0.0949 -0.0402 0.1702 0.159 Uiso 1 1 calc R U . . .
H28E H -0.2181 -0.0169 0.1682 0.159 Uiso 1 1 calc R U . . .
H28F H -0.1609 -0.0832 0.2151 0.159 Uiso 1 1 calc R U . . .
C283 C -0.1236(6) 0.1565(9) 0.1834(3) 0.063(3) Uani 1 1 d . . . . .
H28G H -0.1100 0.2212 0.2022 0.095 Uiso 1 1 calc R U . . .
H28H H -0.1904 0.1613 0.1611 0.095 Uiso 1 1 calc R U . . .
H28I H -0.0666 0.1430 0.1616 0.095 Uiso 1 1 calc R U . . .
C571 C 0.3804(5) 0.6400(6) 0.0916(2) 0.0372(14) Uani 1 1 d . . . . .
H57A H 0.4500 0.6228 0.0814 0.056 Uiso 1 1 calc R U . . .
H57B H 0.3582 0.7066 0.0766 0.056 Uiso 1 1 calc R U . . .
H57C H 0.3299 0.5873 0.0785 0.056 Uiso 1 1 calc R U . . .
C572 C 0.4637(6) 0.7298(6) 0.1701(3) 0.0421(16) Uani 1 1 d . . . . .
H57D H 0.4685 0.7347 0.2083 0.063 Uiso 1 1 calc R U . . .
H57E H 0.4397 0.7954 0.1547 0.063 Uiso 1 1 calc R U . . .
H57F H 0.5330 0.7132 0.1593 0.063 Uiso 1 1 calc R U . . .
C573 C 0.2768(4) 0.6723(6) 0.1671(2) 0.0357(13) Uani 1 1 d . . . . .
H57G H 0.2798 0.6758 0.2052 0.054 Uiso 1 1 calc R U . . .
H57H H 0.2262 0.6197 0.1539 0.054 Uiso 1 1 calc R U . . .
H57I H 0.2548 0.7389 0.1521 0.054 Uiso 1 1 calc R U . . .
C581 C 0.7244(6) 0.4177(11) 0.2469(3) 0.081(4) Uani 1 1 d . . . . .
H58A H 0.7272 0.4766 0.2234 0.122 Uiso 1 1 calc R U . . .
H58B H 0.7168 0.3546 0.2262 0.122 Uiso 1 1 calc R U . . .
H58C H 0.7892 0.4146 0.2706 0.122 Uiso 1 1 calc R U . . .
C582 C 0.6275(6) 0.3386(8) 0.3145(3) 0.053(2) Uani 1 1 d . . . . .
H58D H 0.5682 0.3470 0.3354 0.079 Uiso 1 1 calc R U . . .
H58E H 0.6930 0.3349 0.3378 0.079 Uiso 1 1 calc R U . . .
H58F H 0.6186 0.2754 0.2940 0.079 Uiso 1 1 calc R U . . .
C583 C 0.6455(10) 0.5260(9) 0.3125(4) 0.086(4) Uani 1 1 d . . . . .
H58G H 0.5847 0.5334 0.3325 0.129 Uiso 1 1 calc R U . . .
H58H H 0.6508 0.5862 0.2902 0.129 Uiso 1 1 calc R U . . .
H58I H 0.7096 0.5198 0.3367 0.129 Uiso 1 1 calc R U . . .
C671 C 0.1042(5) -0.0320(5) 0.0956(2) 0.0332(14) Uani 1 1 d . . . . .
H67A H 0.0322 -0.0275 0.0787 0.050 Uiso 1 1 calc R U . . .
H67B H 0.1193 0.0280 0.1181 0.050 Uiso 1 1 calc R U . . .
H67C H 0.1118 -0.0944 0.1169 0.050 Uiso 1 1 calc R U . . .
C672 C 0.1590(6) -0.1341(5) 0.0210(3) 0.0338(14) Uani 1 1 d . . . . .
H67D H 0.2072 -0.1383 -0.0062 0.051 Uiso 1 1 calc R U . . .
H67E H 0.0864 -0.1326 0.0047 0.051 Uiso 1 1 calc R U . . .
H67F H 0.1690 -0.1940 0.0440 0.051 Uiso 1 1 calc R U . . .
C673 C 0.2953(5) -0.0423(5) 0.0798(2) 0.0304(12) Uani 1 1 d . . . . .
H67G H 0.3443 -0.0443 0.0530 0.046 Uiso 1 1 calc R U . . .
H67H H 0.3033 -0.1047 0.1010 0.046 Uiso 1 1 calc R U . . .
H67I H 0.3104 0.0176 0.1023 0.046 Uiso 1 1 calc R U . . .
C681 C 0.0269(5) 0.2062(6) -0.1465(2) 0.0380(15) Uani 1 1 d . . . . .
H68A H 0.0384 0.2768 -0.1342 0.057 Uiso 1 1 calc R U . . .
H68B H -0.0368 0.1789 -0.1335 0.057 Uiso 1 1 calc R U . . .
H68C H 0.0187 0.2053 -0.1848 0.057 Uiso 1 1 calc R U . . .
C682 C 0.1022(5) 0.0308(6) -0.1459(2) 0.0361(15) Uani 1 1 d . . . . .
H68D H 0.1621 -0.0123 -0.1332 0.054 Uiso 1 1 calc R U . . .
H68E H 0.0938 0.0304 -0.1842 0.054 Uiso 1 1 calc R U . . .
H68F H 0.0382 0.0040 -0.1328 0.054 Uiso 1 1 calc R U . . .
C683 C 0.2210(5) 0.1815(8) -0.1483(2) 0.0401(15) Uani 1 1 d . . . . .
H68G H 0.2344 0.2518 -0.1361 0.060 Uiso 1 1 calc R U . . .
H68H H 0.2106 0.1808 -0.1866 0.060 Uiso 1 1 calc R U . . .
H68I H 0.2812 0.1382 -0.1363 0.060 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
Os1 O1 1.705(3) . ?
Os1 N21 1.920(4) . ?
Os1 O11 1.927(5) . ?
Os1 N11 1.933(4) . ?
Os1 O21 1.941(4) . ?
Os2 O2 1.704(3) . ?
Os2 N31 1.933(4) . ?
Os2 N41 1.936(4) . ?
Os2 O31 1.940(4) . ?
Os2 O41 1.945(4) . ?
O11 C11 1.370(6) . ?
O21 C21 1.371(6) . ?
O31 C51 1.375(6) . ?
O41 C61 1.370(6) . ?
O3 C30 1.347(6) . ?
O3 C2 1.459(5) . ?
O30 C30 1.206(6) . ?
O4 C40 1.333(7) . ?
O4 C3 1.469(6) . ?
O40 C40 1.195(7) . ?
O7 C70 1.340(7) . ?
O7 C6 1.454(5) . ?
O70 C70 1.194(7) . ?
O8 C80 1.337(6) . ?
O8 C7 1.467(5) . ?
O80 C80 1.197(6) . ?
N11 C32 1.422(7) . ?
N11 C12 1.430(7) . ?
N21 C22 1.417(7) . ?
N21 C42 1.428(8) . ?
N31 C52 1.399(7) . ?
N31 C72 1.436(8) . ?
N41 C62 1.403(7) . ?
N41 C82 1.442(7) . ?
C1 C2 1.509(8) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.506(6) . ?
C2 H2 1.0000 . ?
C3 C4 1.507(10) . ?
C3 H3 1.0000 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.519(8) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.513(6) . ?
C6 H6 1.0000 . ?
C7 C8 1.507(7) . ?
C7 H7 1.0000 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C11 C16 1.385(8) . ?
C11 C12 1.396(8) . ?
C12 C13 1.387(8) . ?
C13 C14 1.398(8) . ?
C13 H13 0.9500 . ?
C14 C15 1.398(9) . ?
C14 C18 1.525(7) . ?
C15 C16 1.415(7) . ?
C15 H15 0.9500 . ?
C16 C17 1.529(8) . ?
C17 C171 1.525(9) . ?
C17 C172 1.526(7) . ?
C17 C173 1.539(8) . ?
C18 C182 1.517(9) . ?
C18 C181 1.540(8) . ?
C18 C183 1.542(9) . ?
C21 C22 1.386(8) . ?
C21 C26 1.401(8) . ?
C22 C23 1.397(8) . ?
C23 C24 1.396(9) . ?
C23 H23 0.9500 . ?
C24 C25 1.409(9) . ?
C24 C28 1.528(8) . ?
C25 C26 1.393(8) . ?
C25 H25 0.9500 . ?
C26 C27 1.534(8) . ?
C27 C271 1.514(8) . ?
C27 C273 1.524(7) . ?
C27 C272 1.532(9) . ?
C28 C282 1.498(12) . ?
C28 C283 1.516(10) . ?
C28 C281 1.520(8) . ?
C30 C31 1.491(7) . ?
C31 C36 1.401(8) . ?
C31 C32 1.408(7) . ?
C32 C33 1.395(8) . ?
C33 C34 1.391(8) . ?
C33 H33 0.9500 . ?
C34 C35 1.377(8) . ?
C34 H34 0.9500 . ?
C35 C36 1.383(9) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C40 C41 1.496(8) . ?
C41 C42 1.396(8) . ?
C41 C46 1.408(9) . ?
C42 C43 1.381(8) . ?
C43 C44 1.401(9) . ?
C43 H43 0.9500 . ?
C44 C45 1.376(9) . ?
C44 H44 0.9500 . ?
C45 C46 1.377(10) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
C51 C52 1.396(8) . ?
C51 C56 1.400(8) . ?
C52 C53 1.384(8) . ?
C53 C54 1.391(9) . ?
C53 H53 0.9500 . ?
C54 C55 1.395(9) . ?
C54 C58 1.546(7) . ?
C55 C56 1.409(8) . ?
C55 H55 0.9500 . ?
C56 C57 1.537(8) . ?
C57 C573 1.528(7) . ?
C57 C571 1.534(7) . ?
C57 C572 1.535(9) . ?
C58 C581 1.503(9) . ?
C58 C582 1.511(10) . ?
C58 C583 1.546(11) . ?
C61 C66 1.400(8) . ?
C61 C62 1.401(8) . ?
C62 C63 1.382(8) . ?
C63 C64 1.400(8) . ?
C63 H63 0.9500 . ?
C64 C65 1.398(8) . ?
C64 C68 1.546(7) . ?
C65 C66 1.386(8) . ?
C65 H65 0.9500 . ?
C66 C67 1.542(8) . ?
C67 C673 1.539(8) . ?
C67 C671 1.546(8) . ?
C67 C672 1.546(9) . ?
C68 C682 1.526(9) . ?
C68 C681 1.532(9) . ?
C68 C683 1.544(7) . ?
C70 C71 1.497(7) . ?
C71 C76 1.403(9) . ?
C71 C72 1.408(7) . ?
C72 C73 1.380(8) . ?
C73 C74 1.384(9) . ?
C73 H73 0.9500 . ?
C74 C75 1.382(9) . ?
C74 H74 0.9500 . ?
C75 C76 1.381(9) . ?
C75 H75 0.9500 . ?
C76 H76 0.9500 . ?
C80 C81 1.504(7) . ?
C81 C82 1.392(7) . ?
C81 C86 1.396(8) . ?
C82 C83 1.383(8) . ?
C83 C84 1.390(8) . ?
C83 H83 0.9500 . ?
C84 C85 1.387(8) . ?
C84 H84 0.9500 . ?
C85 C86 1.394(9) . ?
C85 H85 0.9500 . ?
C86 H86 0.9500 . ?
C171 H17A 0.9800 . ?
C171 H17B 0.9800 . ?
C171 H17C 0.9800 . ?
C172 H17D 0.9800 . ?
C172 H17E 0.9800 . ?
C172 H17F 0.9800 . ?
C173 H17G 0.9800 . ?
C173 H17H 0.9800 . ?
C173 H17I 0.9800 . ?
C181 H18A 0.9800 . ?
C181 H18B 0.9800 . ?
C181 H18C 0.9800 . ?
C182 H18D 0.9800 . ?
C182 H18E 0.9800 . ?
C182 H18F 0.9800 . ?
C183 H18G 0.9800 . ?
C183 H18H 0.9800 . ?
C183 H18I 0.9800 . ?
C271 H27A 0.9800 . ?
C271 H27B 0.9800 . ?
C271 H27C 0.9800 . ?
C272 H27D 0.9800 . ?
C272 H27E 0.9800 . ?
C272 H27F 0.9800 . ?
C273 H27G 0.9800 . ?
C273 H27H 0.9800 . ?
C273 H27I 0.9800 . ?
C281 H28A 0.9800 . ?
C281 H28B 0.9800 . ?
C281 H28C 0.9800 . ?
C282 H28D 0.9800 . ?
C282 H28E 0.9800 . ?
C282 H28F 0.9800 . ?
C283 H28G 0.9800 . ?
C283 H28H 0.9800 . ?
C283 H28I 0.9800 . ?
C571 H57A 0.9800 . ?
C571 H57B 0.9800 . ?
C571 H57C 0.9800 . ?
C572 H57D 0.9800 . ?
C572 H57E 0.9800 . ?
C572 H57F 0.9800 . ?
C573 H57G 0.9800 . ?
C573 H57H 0.9800 . ?
C573 H57I 0.9800 . ?
C581 H58A 0.9800 . ?
C581 H58B 0.9800 . ?
C581 H58C 0.9800 . ?
C582 H58D 0.9800 . ?
C582 H58E 0.9800 . ?
C582 H58F 0.9800 . ?
C583 H58G 0.9800 . ?
C583 H58H 0.9800 . ?
C583 H58I 0.9800 . ?
C671 H67A 0.9800 . ?
C671 H67B 0.9800 . ?
C671 H67C 0.9800 . ?
C672 H67D 0.9800 . ?
C672 H67E 0.9800 . ?
C672 H67F 0.9800 . ?
C673 H67G 0.9800 . ?
C673 H67H 0.9800 . ?
C673 H67I 0.9800 . ?
C681 H68A 0.9800 . ?
C681 H68B 0.9800 . ?
C681 H68C 0.9800 . ?
C682 H68D 0.9800 . ?
C682 H68E 0.9800 . ?
C682 H68F 0.9800 . ?
C683 H68G 0.9800 . ?
C683 H68H 0.9800 . ?
C683 H68I 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
O1 Os1 N21 112.60(17) . . ?
O1 Os1 O11 106.38(19) . . ?
N21 Os1 O11 86.17(17) . . ?
O1 Os1 N11 112.25(17) . . ?
N21 Os1 N11 135.15(16) . . ?
O11 Os1 N11 81.06(17) . . ?
O1 Os1 O21 105.9(2) . . ?
N21 Os1 O21 80.70(18) . . ?
O11 Os1 O21 147.75(14) . . ?
N11 Os1 O21 87.72(17) . . ?
O2 Os2 N31 110.97(17) . . ?
O2 Os2 N41 110.90(17) . . ?
N31 Os2 N41 138.11(16) . . ?
O2 Os2 O31 106.82(18) . . ?
N31 Os2 O31 80.76(17) . . ?
N41 Os2 O31 88.58(17) . . ?
O2 Os2 O41 106.65(18) . . ?
N31 Os2 O41 86.48(17) . . ?
N41 Os2 O41 80.51(17) . . ?
O31 Os2 O41 146.51(13) . . ?
C11 O11 Os1 116.4(4) . . ?
C21 O21 Os1 116.0(4) . . ?
C51 O31 Os2 115.5(4) . . ?
C61 O41 Os2 115.7(4) . . ?
C30 O3 C2 118.3(3) . . ?
C40 O4 C3 117.1(4) . . ?
C70 O7 C6 117.6(4) . . ?
C80 O8 C7 116.7(3) . . ?
C32 N11 C12 119.2(4) . . ?
C32 N11 Os1 125.6(4) . . ?
C12 N11 Os1 115.2(3) . . ?
C22 N21 C42 118.8(4) . . ?
C22 N21 Os1 115.8(4) . . ?
C42 N21 Os1 125.2(4) . . ?
C52 N31 C72 119.1(4) . . ?
C52 N31 Os2 115.9(4) . . ?
C72 N31 Os2 124.7(4) . . ?
C62 N41 C82 118.2(4) . . ?
C62 N41 Os2 116.2(4) . . ?
C82 N41 Os2 125.2(4) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O3 C2 C3 109.1(4) . . ?
O3 C2 C1 107.5(4) . . ?
C3 C2 C1 113.7(5) . . ?
O3 C2 H2 108.8 . . ?
C3 C2 H2 108.8 . . ?
C1 C2 H2 108.8 . . ?
O4 C3 C2 108.4(4) . . ?
O4 C3 C4 106.6(4) . . ?
C2 C3 C4 115.1(5) . . ?
O4 C3 H3 108.9 . . ?
C2 C3 H3 108.9 . . ?
C4 C3 H3 108.9 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C5 H5A 109.5 . . ?
C6 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C6 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O7 C6 C7 106.5(4) . . ?
O7 C6 C5 109.1(4) . . ?
C7 C6 C5 115.3(4) . . ?
O7 C6 H6 108.6 . . ?
C7 C6 H6 108.6 . . ?
C5 C6 H6 108.6 . . ?
O8 C7 C8 109.1(3) . . ?
O8 C7 C6 105.6(3) . . ?
C8 C7 C6 113.5(4) . . ?
O8 C7 H7 109.5 . . ?
C8 C7 H7 109.5 . . ?
C6 C7 H7 109.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O11 C11 C16 123.1(5) . . ?
O11 C11 C12 114.7(5) . . ?
C16 C11 C12 122.2(5) . . ?
C13 C12 C11 121.3(5) . . ?
C13 C12 N11 126.5(6) . . ?
C11 C12 N11 112.1(4) . . ?
C12 C13 C14 118.9(5) . . ?
C12 C13 H13 120.6 . . ?
C14 C13 H13 120.6 . . ?
C15 C14 C13 118.4(5) . . ?
C15 C14 C18 122.5(5) . . ?
C13 C14 C18 119.1(5) . . ?
C14 C15 C16 124.0(6) . . ?
C14 C15 H15 118.0 . . ?
C16 C15 H15 118.0 . . ?
C11 C16 C15 115.2(5) . . ?
C11 C16 C17 122.1(5) . . ?
C15 C16 C17 122.7(5) . . ?
C171 C17 C172 107.9(5) . . ?
C171 C17 C16 111.8(5) . . ?
C172 C17 C16 110.9(5) . . ?
C171 C17 C173 107.8(5) . . ?
C172 C17 C173 110.0(5) . . ?
C16 C17 C173 108.3(5) . . ?
C182 C18 C14 110.0(5) . . ?
C182 C18 C181 109.0(6) . . ?
C14 C18 C181 109.4(5) . . ?
C182 C18 C183 107.7(5) . . ?
C14 C18 C183 112.4(5) . . ?
C181 C18 C183 108.2(5) . . ?
O21 C21 C22 114.4(5) . . ?
O21 C21 C26 124.5(5) . . ?
C22 C21 C26 121.1(5) . . ?
C21 C22 C23 122.2(5) . . ?
C21 C22 N21 112.7(5) . . ?
C23 C22 N21 125.1(5) . . ?
C24 C23 C22 118.3(5) . . ?
C24 C23 H23 120.9 . . ?
C22 C23 H23 120.9 . . ?
C23 C24 C25 118.2(5) . . ?
C23 C24 C28 119.5(6) . . ?
C25 C24 C28 122.1(6) . . ?
C26 C25 C24 124.3(6) . . ?
C26 C25 H25 117.8 . . ?
C24 C25 H25 117.8 . . ?
C25 C26 C21 115.8(5) . . ?
C25 C26 C27 122.4(5) . . ?
C21 C26 C27 121.8(5) . . ?
C271 C27 C273 110.2(6) . . ?
C271 C27 C272 107.5(6) . . ?
C273 C27 C272 108.1(6) . . ?
C271 C27 C26 110.3(5) . . ?
C273 C27 C26 109.3(5) . . ?
C272 C27 C26 111.4(5) . . ?
C282 C28 C283 107.0(7) . . ?
C282 C28 C281 109.3(9) . . ?
C283 C28 C281 108.3(7) . . ?
C282 C28 C24 112.3(6) . . ?
C283 C28 C24 112.4(5) . . ?
C281 C28 C24 107.5(5) . . ?
O30 C30 O3 124.5(5) . . ?
O30 C30 C31 124.7(5) . . ?
O3 C30 C31 110.5(4) . . ?
C36 C31 C32 118.9(5) . . ?
C36 C31 C30 116.0(4) . . ?
C32 C31 C30 124.8(5) . . ?
C33 C32 C31 119.0(5) . . ?
C33 C32 N11 118.7(4) . . ?
C31 C32 N11 122.2(5) . . ?
C34 C33 C32 121.2(5) . . ?
C34 C33 H33 119.4 . . ?
C32 C33 H33 119.4 . . ?
C35 C34 C33 119.3(6) . . ?
C35 C34 H34 120.3 . . ?
C33 C34 H34 120.3 . . ?
C34 C35 C36 120.6(6) . . ?
C34 C35 H35 119.7 . . ?
C36 C35 H35 119.7 . . ?
C35 C36 C31 120.6(5) . . ?
C35 C36 H36 119.7 . . ?
C31 C36 H36 119.7 . . ?
O40 C40 O4 124.2(5) . . ?
O40 C40 C41 124.4(6) . . ?
O4 C40 C41 111.3(4) . . ?
C42 C41 C46 118.9(6) . . ?
C42 C41 C40 125.8(6) . . ?
C46 C41 C40 115.1(5) . . ?
C43 C42 C41 119.7(6) . . ?
C43 C42 N21 117.0(5) . . ?
C41 C42 N21 123.3(5) . . ?
C42 C43 C44 120.9(6) . . ?
C42 C43 H43 119.6 . . ?
C44 C43 H43 119.6 . . ?
C45 C44 C43 119.3(6) . . ?
C45 C44 H44 120.4 . . ?
C43 C44 H44 120.4 . . ?
C44 C45 C46 120.6(6) . . ?
C44 C45 H45 119.7 . . ?
C46 C45 H45 119.7 . . ?
C45 C46 C41 120.5(6) . . ?
C45 C46 H46 119.8 . . ?
C41 C46 H46 119.8 . . ?
O31 C51 C52 114.5(5) . . ?
O31 C51 C56 124.0(5) . . ?
C52 C51 C56 121.5(5) . . ?
C53 C52 C51 121.0(5) . . ?
C53 C52 N31 126.2(5) . . ?
C51 C52 N31 112.8(5) . . ?
C52 C53 C54 119.9(5) . . ?
C52 C53 H53 120.1 . . ?
C54 C53 H53 120.1 . . ?
C53 C54 C55 118.1(5) . . ?
C53 C54 C58 120.5(6) . . ?
C55 C54 C58 121.3(6) . . ?
C54 C55 C56 124.1(6) . . ?
C54 C55 H55 118.0 . . ?
C56 C55 H55 118.0 . . ?
C51 C56 C55 115.5(5) . . ?
C51 C56 C57 121.9(5) . . ?
C55 C56 C57 122.6(5) . . ?
C573 C57 C571 109.3(5) . . ?
C573 C57 C572 109.4(5) . . ?
C571 C57 C572 107.8(5) . . ?
C573 C57 C56 108.7(5) . . ?
C571 C57 C56 110.1(5) . . ?
C572 C57 C56 111.5(5) . . ?
C581 C58 C582 109.7(7) . . ?
C581 C58 C583 109.8(9) . . ?
C582 C58 C583 107.1(6) . . ?
C581 C58 C54 107.3(5) . . ?
C582 C58 C54 112.4(5) . . ?
C583 C58 C54 110.6(6) . . ?
O41 C61 C66 123.1(5) . . ?
O41 C61 C62 114.8(5) . . ?
C66 C61 C62 122.0(5) . . ?
C63 C62 C61 119.9(6) . . ?
C63 C62 N41 127.8(6) . . ?
C61 C62 N41 112.2(5) . . ?
C62 C63 C64 119.8(6) . . ?
C62 C63 H63 120.1 . . ?
C64 C63 H63 120.1 . . ?
C65 C64 C63 118.5(5) . . ?
C65 C64 C68 121.9(5) . . ?
C63 C64 C68 119.6(5) . . ?
C66 C65 C64 123.6(6) . . ?
C66 C65 H65 118.2 . . ?
C64 C65 H65 118.2 . . ?
C65 C66 C61 116.1(5) . . ?
C65 C66 C67 123.3(5) . . ?
C61 C66 C67 120.6(5) . . ?
C673 C67 C66 109.7(5) . . ?
C673 C67 C671 109.8(5) . . ?
C66 C67 C671 109.9(5) . . ?
C673 C67 C672 107.9(5) . . ?
C66 C67 C672 111.9(5) . . ?
C671 C67 C672 107.7(5) . . ?
C682 C68 C681 108.7(5) . . ?
C682 C68 C683 108.5(5) . . ?
C681 C68 C683 109.3(6) . . ?
C682 C68 C64 112.6(5) . . ?
C681 C68 C64 109.9(5) . . ?
C683 C68 C64 107.8(4) . . ?
O70 C70 O7 123.9(5) . . ?
O70 C70 C71 123.6(5) . . ?
O7 C70 C71 112.4(4) . . ?
C76 C71 C72 117.9(5) . . ?
C76 C71 C70 116.6(5) . . ?
C72 C71 C70 125.4(5) . . ?
C73 C72 C71 120.5(6) . . ?
C73 C72 N31 116.9(5) . . ?
C71 C72 N31 122.5(5) . . ?
C72 C73 C74 120.4(6) . . ?
C72 C73 H73 119.8 . . ?
C74 C73 H73 119.8 . . ?
C75 C74 C73 120.0(6) . . ?
C75 C74 H74 120.0 . . ?
C73 C74 H74 120.0 . . ?
C76 C75 C74 120.0(6) . . ?
C76 C75 H75 120.0 . . ?
C74 C75 H75 120.0 . . ?
C75 C76 C71 121.0(6) . . ?
C75 C76 H76 119.5 . . ?
C71 C76 H76 119.5 . . ?
O80 C80 O8 125.1(5) . . ?
O80 C80 C81 123.9(5) . . ?
O8 C80 C81 110.9(4) . . ?
C82 C81 C86 119.1(5) . . ?
C82 C81 C80 124.5(5) . . ?
C86 C81 C80 116.3(4) . . ?
C83 C82 C81 120.3(5) . . ?
C83 C82 N41 116.6(4) . . ?
C81 C82 N41 123.0(5) . . ?
C82 C83 C84 120.2(5) . . ?
C82 C83 H83 119.9 . . ?
C84 C83 H83 119.9 . . ?
C85 C84 C83 120.3(5) . . ?
C85 C84 H84 119.8 . . ?
C83 C84 H84 119.8 . . ?
C84 C85 C86 119.3(6) . . ?
C84 C85 H85 120.3 . . ?
C86 C85 H85 120.3 . . ?
C85 C86 C81 120.6(5) . . ?
C85 C86 H86 119.7 . . ?
C81 C86 H86 119.7 . . ?
C17 C171 H17A 109.5 . . ?
C17 C171 H17B 109.5 . . ?
H17A C171 H17B 109.5 . . ?
C17 C171 H17C 109.5 . . ?
H17A C171 H17C 109.5 . . ?
H17B C171 H17C 109.5 . . ?
C17 C172 H17D 109.5 . . ?
C17 C172 H17E 109.5 . . ?
H17D C172 H17E 109.5 . . ?
C17 C172 H17F 109.5 . . ?
H17D C172 H17F 109.5 . . ?
H17E C172 H17F 109.5 . . ?
C17 C173 H17G 109.5 . . ?
C17 C173 H17H 109.5 . . ?
H17G C173 H17H 109.5 . . ?
C17 C173 H17I 109.5 . . ?
H17G C173 H17I 109.5 . . ?
H17H C173 H17I 109.5 . . ?
C18 C181 H18A 109.5 . . ?
C18 C181 H18B 109.5 . . ?
H18A C181 H18B 109.5 . . ?
C18 C181 H18C 109.5 . . ?
H18A C181 H18C 109.5 . . ?
H18B C181 H18C 109.5 . . ?
C18 C182 H18D 109.5 . . ?
C18 C182 H18E 109.5 . . ?
H18D C182 H18E 109.5 . . ?
C18 C182 H18F 109.5 . . ?
H18D C182 H18F 109.5 . . ?
H18E C182 H18F 109.5 . . ?
C18 C183 H18G 109.5 . . ?
C18 C183 H18H 109.5 . . ?
H18G C183 H18H 109.5 . . ?
C18 C183 H18I 109.5 . . ?
H18G C183 H18I 109.5 . . ?
H18H C183 H18I 109.5 . . ?
C27 C271 H27A 109.5 . . ?
C27 C271 H27B 109.5 . . ?
H27A C271 H27B 109.5 . . ?
C27 C271 H27C 109.5 . . ?
H27A C271 H27C 109.5 . . ?
H27B C271 H27C 109.5 . . ?
C27 C272 H27D 109.5 . . ?
C27 C272 H27E 109.5 . . ?
H27D C272 H27E 109.5 . . ?
C27 C272 H27F 109.5 . . ?
H27D C272 H27F 109.5 . . ?
H27E C272 H27F 109.5 . . ?
C27 C273 H27G 109.5 . . ?
C27 C273 H27H 109.5 . . ?
H27G C273 H27H 109.5 . . ?
C27 C273 H27I 109.5 . . ?
H27G C273 H27I 109.5 . . ?
H27H C273 H27I 109.5 . . ?
C28 C281 H28A 109.5 . . ?
C28 C281 H28B 109.5 . . ?
H28A C281 H28B 109.5 . . ?
C28 C281 H28C 109.5 . . ?
H28A C281 H28C 109.5 . . ?
H28B C281 H28C 109.5 . . ?
C28 C282 H28D 109.5 . . ?
C28 C282 H28E 109.5 . . ?
H28D C282 H28E 109.5 . . ?
C28 C282 H28F 109.5 . . ?
H28D C282 H28F 109.5 . . ?
H28E C282 H28F 109.5 . . ?
C28 C283 H28G 109.5 . . ?
C28 C283 H28H 109.5 . . ?
H28G C283 H28H 109.5 . . ?
C28 C283 H28I 109.5 . . ?
H28G C283 H28I 109.5 . . ?
H28H C283 H28I 109.5 . . ?
C57 C571 H57A 109.5 . . ?
C57 C571 H57B 109.5 . . ?
H57A C571 H57B 109.5 . . ?
C57 C571 H57C 109.5 . . ?
H57A C571 H57C 109.5 . . ?
H57B C571 H57C 109.5 . . ?
C57 C572 H57D 109.5 . . ?
C57 C572 H57E 109.5 . . ?
H57D C572 H57E 109.5 . . ?
C57 C572 H57F 109.5 . . ?
H57D C572 H57F 109.5 . . ?
H57E C572 H57F 109.5 . . ?
C57 C573 H57G 109.5 . . ?
C57 C573 H57H 109.5 . . ?
H57G C573 H57H 109.5 . . ?
C57 C573 H57I 109.5 . . ?
H57G C573 H57I 109.5 . . ?
H57H C573 H57I 109.5 . . ?
C58 C581 H58A 109.5 . . ?
C58 C581 H58B 109.5 . . ?
H58A C581 H58B 109.5 . . ?
C58 C581 H58C 109.5 . . ?
H58A C581 H58C 109.5 . . ?
H58B C581 H58C 109.5 . . ?
C58 C582 H58D 109.5 . . ?
C58 C582 H58E 109.5 . . ?
H58D C582 H58E 109.5 . . ?
C58 C582 H58F 109.5 . . ?
H58D C582 H58F 109.5 . . ?
H58E C582 H58F 109.5 . . ?
C58 C583 H58G 109.5 . . ?
C58 C583 H58H 109.5 . . ?
H58G C583 H58H 109.5 . . ?
C58 C583 H58I 109.5 . . ?
H58G C583 H58I 109.5 . . ?
H58H C583 H58I 109.5 . . ?
C67 C671 H67A 109.5 . . ?
C67 C671 H67B 109.5 . . ?
H67A C671 H67B 109.5 . . ?
C67 C671 H67C 109.5 . . ?
H67A C671 H67C 109.5 . . ?
H67B C671 H67C 109.5 . . ?
C67 C672 H67D 109.5 . . ?
C67 C672 H67E 109.5 . . ?
H67D C672 H67E 109.5 . . ?
C67 C672 H67F 109.5 . . ?
H67D C672 H67F 109.5 . . ?
H67E C672 H67F 109.5 . . ?
C67 C673 H67G 109.5 . . ?
C67 C673 H67H 109.5 . . ?
H67G C673 H67H 109.5 . . ?
C67 C673 H67I 109.5 . . ?
H67G C673 H67I 109.5 . . ?
H67H C673 H67I 109.5 . . ?
C68 C681 H68A 109.5 . . ?
C68 C681 H68B 109.5 . . ?
H68A C681 H68B 109.5 . . ?
C68 C681 H68C 109.5 . . ?
H68A C681 H68C 109.5 . . ?
H68B C681 H68C 109.5 . . ?
C68 C682 H68D 109.5 . . ?
C68 C682 H68E 109.5 . . ?
H68D C682 H68E 109.5 . . ?
C68 C682 H68F 109.5 . . ?
H68D C682 H68F 109.5 . . ?
H68E C682 H68F 109.5 . . ?
C68 C683 H68G 109.5 . . ?
C68 C683 H68H 109.5 . . ?
H68G C683 H68H 109.5 . . ?
C68 C683 H68I 109.5 . . ?
H68G C683 H68I 109.5 . . ?
H68H C683 H68I 109.5 . . ?

_refine_diff_density_max         0.894
_refine_diff_density_min         -0.708
_refine_diff_density_rms         0.056

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_bdanoso
_database_code_depnum_ccdc_archive 'CCDC 2281683'
loop_
_audit_author_name
_audit_author_address
'Seth Brown'
;University of Notre Dame
United States of America
;
_audit_update_record             
;
2023-07-14 deposited with the CCDC.	2023-08-28 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT213_bdanoso             
;
PROBLEM: Atom C672 has ADP max/min Ratio .....        4.5 prolat
RESPONSE: Atom is part of a tert-butyl group with unresolved disorder.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
'(C,R,R)-Oxo(2,3-butanediylbis(2-(2-oxy-3,5-di-tert-butylphenyl)amido)benzoate)osmium methanol solvate'
_chemical_name_common            '(C,R,R)-(Bdan)OsO . CH3OH'
_chemical_melting_point          ?
_chemical_formula_moiety         'C46 H56 N2 O7 Os, C H4 O'
_chemical_formula_sum            'C47 H60 N2 O8 Os'
_chemical_formula_weight         971.17

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Os Os -4.9801 6.2216 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_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'

_cell_length_a                   12.7929(3)
_cell_length_b                   18.4722(4)
_cell_length_c                   37.6599(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8899.5(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9416
_cell_measurement_theta_min      4.18
_cell_measurement_theta_max      72.23

_exptl_crystal_description       plate
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_F_000             3968
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.079
_exptl_crystal_size_mid          0.077
_exptl_crystal_size_min          0.029
_exptl_absorpt_coefficient_mu    5.847
_shelx_estimated_absorpt_T_min   0.655
_shelx_estimated_absorpt_T_max   0.849
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.6436
_exptl_absorpt_correction_T_max  0.9372
_exptl_absorpt_process_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10.
;

_exptl_crystal_recrystallization_method 
;
Crystals were deposited from a methanol solution of the compound.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.33
_diffrn_reflns_number            85065
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_av_R_equivalents  0.0528
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_theta_min         2.346
_diffrn_reflns_theta_max         72.247
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             17517
_reflns_number_gt                16604
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.826
_reflns_Friedel_fraction_max     0.995
_reflns_Friedel_fraction_full    0.999

_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 ? 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0307P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     heavy
_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_abs_structure_details 
; 
 Flack x determined using 7296 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   -0.009(4)
_chemical_absolute_configuration rmad
_refine_ls_number_reflns         17517
_refine_ls_number_parameters     1049
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0279
_refine_ls_R_factor_gt           0.0254
_refine_ls_wR_factor_ref         0.0586
_refine_ls_wR_factor_gt          0.0575
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.020
_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
Os1 Os 0.43724(2) 1.07100(2) 0.91584(2) 0.01226(5) Uani 1 1 d . . . . .
Os2 Os 0.83278(2) 1.07751(2) 0.58700(2) 0.01274(5) Uani 1 1 d . . . . .
O1 O 0.3957(3) 1.12407(19) 0.95004(8) 0.0189(6) Uani 1 1 d . . . . .
O2 O 0.7899(3) 1.1335(2) 0.55399(9) 0.0216(7) Uani 1 1 d . . . . .
O11 O 0.5750(3) 1.03432(18) 0.92723(8) 0.0168(6) Uani 1 1 d . . . . .
O21 O 0.3288(2) 1.07082(18) 0.87980(7) 0.0160(5) Uani 1 1 d . . . . .
O30 O 0.4012(4) 0.7972(2) 0.85775(13) 0.0395(10) Uani 1 1 d . . . . .
O31 O 0.4426(3) 0.91487(19) 0.85623(9) 0.0241(7) Uani 1 1 d . . . . .
O40 O 0.6712(4) 1.0789(3) 0.79200(10) 0.0394(10) Uani 1 1 d . . . . .
O41 O 0.5810(3) 1.0228(2) 0.83530(9) 0.0224(7) Uani 1 1 d . . . . .
O51 O 0.7342(2) 0.99873(17) 0.59174(8) 0.0164(6) Uani 1 1 d . . . . .
O61 O 0.9613(2) 1.11797(18) 0.60635(8) 0.0170(6) Uani 1 1 d . . . . .
O70 O 1.1139(4) 0.8571(2) 0.61552(12) 0.0348(9) Uani 1 1 d . . . . .
O71 O 0.9978(3) 0.94284(19) 0.63045(8) 0.0206(7) Uani 1 1 d . . . . .
O80 O 0.7626(4) 0.9965(3) 0.72713(11) 0.0452(12) Uani 1 1 d . . . . .
O81 O 0.8393(3) 0.9922(2) 0.67351(9) 0.0239(7) Uani 1 1 d . . . . .
N11 N 0.4014(3) 0.9710(2) 0.92519(9) 0.0155(7) Uani 1 1 d . . . . .
N21 N 0.5060(3) 1.1317(2) 0.88098(10) 0.0145(7) Uani 1 1 d . . . . .
N51 N 0.9154(3) 1.0000(2) 0.56685(9) 0.0141(7) Uani 1 1 d . . . . .
N61 N 0.7804(3) 1.1115(2) 0.63222(10) 0.0157(7) Uani 1 1 d . . . . .
C1 C 0.6234(5) 0.8772(3) 0.85520(17) 0.0354(13) Uani 1 1 d . . . . .
H1A H 0.6060 0.8337 0.8689 0.053 Uiso 1 1 calc R U . . .
H1B H 0.6412 0.9166 0.8715 0.053 Uiso 1 1 calc R U . . .
H1C H 0.6832 0.8671 0.8397 0.053 Uiso 1 1 calc R U . . .
C2 C 0.5307(4) 0.8991(3) 0.83291(14) 0.0267(11) Uani 1 1 d . . . . .
H2 H 0.5115 0.8580 0.8169 0.032 Uiso 1 1 calc R U . . .
C3 C 0.5495(4) 0.9665(3) 0.81060(13) 0.0235(10) Uani 1 1 d . . . . .
H3 H 0.6086 0.9569 0.7939 0.028 Uiso 1 1 calc R U . . .
C4 C 0.4555(5) 0.9920(3) 0.78929(14) 0.0292(11) Uani 1 1 d . . . . .
H4A H 0.4743 1.0354 0.7757 0.044 Uiso 1 1 calc R U . . .
H4B H 0.3979 1.0034 0.8055 0.044 Uiso 1 1 calc R U . . .
H4C H 0.4337 0.9536 0.7729 0.044 Uiso 1 1 calc R U . . .
C5 C 0.8856(5) 0.8445(3) 0.65050(14) 0.0295(11) Uani 1 1 d . . . . .
H5A H 0.9157 0.8118 0.6327 0.044 Uiso 1 1 calc R U . . .
H5B H 0.8247 0.8692 0.6404 0.044 Uiso 1 1 calc R U . . .
H5C H 0.8641 0.8164 0.6714 0.044 Uiso 1 1 calc R U . . .
C6 C 0.9668(4) 0.9002(3) 0.66141(13) 0.0238(10) Uani 1 1 d . . . . .
H6 H 1.0297 0.8745 0.6709 0.029 Uiso 1 1 calc R U . . .
C7 C 0.9281(4) 0.9536(3) 0.68915(12) 0.0244(10) Uani 1 1 d . . . . .
H7 H 0.9031 0.9259 0.7103 0.029 Uiso 1 1 calc R U . . .
C8 C 1.0086(5) 1.0086(3) 0.70113(15) 0.0338(12) Uani 1 1 d . . . . .
H8A H 0.9774 1.0408 0.7189 0.051 Uiso 1 1 calc R U . . .
H8B H 1.0320 1.0371 0.6807 0.051 Uiso 1 1 calc R U . . .
H8C H 1.0686 0.9834 0.7116 0.051 Uiso 1 1 calc R U . . .
C11 C 0.5784(4) 0.9665(2) 0.94114(11) 0.0163(8) Uani 1 1 d . . . . .
C12 C 0.4836(3) 0.9279(3) 0.93914(10) 0.0157(8) Uani 1 1 d . . . . .
C13 C 0.4772(4) 0.8572(3) 0.95113(12) 0.0175(8) Uani 1 1 d . . . . .
H13 H 0.4134 0.8311 0.9495 0.021 Uiso 1 1 calc R U . . .
C14 C 0.5664(4) 0.8247(3) 0.96571(11) 0.0184(8) Uani 1 1 d . . . . .
C15 C 0.6590(4) 0.8649(3) 0.96742(12) 0.0190(9) Uani 1 1 d . . . . .
H15 H 0.7190 0.8424 0.9774 0.023 Uiso 1 1 calc R U . . .
C16 C 0.6684(4) 0.9365(3) 0.95526(11) 0.0173(8) Uani 1 1 d . . . . .
C17 C 0.7710(3) 0.9793(3) 0.95723(12) 0.0175(9) Uani 1 1 d . . . . .
C18 C 0.5577(4) 0.7486(3) 0.98152(13) 0.0221(9) Uani 1 1 d . . . . .
C21 C 0.3445(4) 1.1178(2) 0.85201(11) 0.0159(8) Uani 1 1 d . . . . .
C22 C 0.4427(4) 1.1517(2) 0.85171(11) 0.0155(8) Uani 1 1 d . . . . .
C23 C 0.4709(4) 1.1999(3) 0.82532(12) 0.0182(9) Uani 1 1 d . . . . .
H23 H 0.5372 1.2230 0.8258 0.022 Uiso 1 1 calc R U . . .
C24 C 0.4004(4) 1.2139(3) 0.79795(12) 0.0207(9) Uani 1 1 d . . . . .
C25 C 0.3038(4) 1.1785(3) 0.79842(12) 0.0201(9) Uani 1 1 d . . . . .
H25 H 0.2567 1.1878 0.7795 0.024 Uiso 1 1 calc R U . . .
C26 C 0.2717(4) 1.1299(3) 0.82510(12) 0.0193(9) Uani 1 1 d . . . . .
C27 C 0.1655(4) 1.0915(3) 0.82402(12) 0.0226(10) Uani 1 1 d . . . . .
C28 C 0.4286(5) 1.2632(3) 0.76688(13) 0.0260(10) Uani 1 1 d . . . . .
C30 C 0.3865(5) 0.8575(3) 0.86702(14) 0.0277(11) Uani 1 1 d . . . . .
C31 C 0.2984(4) 0.8811(3) 0.89051(13) 0.0217(9) Uani 1 1 d . . . . .
C32 C 0.3046(3) 0.9372(2) 0.91575(12) 0.0164(8) Uani 1 1 d . . . . .
C33 C 0.2156(4) 0.9603(3) 0.93311(14) 0.0258(10) Uani 1 1 d . . . . .
H33 H 0.2199 0.9985 0.9499 0.031 Uiso 1 1 calc R U . . .
C34 C 0.1195(4) 0.9278(4) 0.92601(15) 0.0344(12) Uani 1 1 d . . . . .
H34 H 0.0581 0.9453 0.9373 0.041 Uiso 1 1 calc R U . . .
C35 C 0.1130(5) 0.8705(4) 0.90276(17) 0.0384(14) Uani 1 1 d . . . . .
H35 H 0.0478 0.8473 0.8988 0.046 Uiso 1 1 calc R U . . .
C36 C 0.2028(5) 0.8465(3) 0.88487(15) 0.0325(12) Uani 1 1 d . . . . .
H36 H 0.1986 0.8067 0.8690 0.039 Uiso 1 1 calc R U . . .
C40 C 0.6428(4) 1.0752(3) 0.82238(13) 0.0250(9) Uani 1 1 d . . . . .
C41 C 0.6781(4) 1.1247(3) 0.85129(12) 0.0197(9) Uani 1 1 d . . . . .
C42 C 0.6152(3) 1.1466(2) 0.87974(12) 0.0151(8) Uani 1 1 d . . . . .
C43 C 0.6597(4) 1.1857(2) 0.90755(12) 0.0188(8) Uani 1 1 d . . . . .
H43 H 0.6183 1.1984 0.9276 0.023 Uiso 1 1 calc R U . . .
C44 C 0.7634(4) 1.2060(3) 0.90623(13) 0.0228(10) Uani 1 1 d . . . . .
H44 H 0.7928 1.2330 0.9252 0.027 Uiso 1 1 calc R U . . .
C45 C 0.8249(4) 1.1873(3) 0.87733(15) 0.0264(10) Uani 1 1 d . . . . .
H45 H 0.8960 1.2022 0.8764 0.032 Uiso 1 1 calc R U . . .
C46 C 0.7828(4) 1.1472(3) 0.84999(14) 0.0249(10) Uani 1 1 d . . . . .
H46 H 0.8249 1.1347 0.8301 0.030 Uiso 1 1 calc R U . . .
C51 C 0.7631(3) 0.9343(3) 0.57635(10) 0.0168(8) Uani 1 1 d . . . . .
C52 C 0.8647(3) 0.9331(3) 0.56309(10) 0.0146(8) Uani 1 1 d . . . . .
C53 C 0.9057(4) 0.8710(3) 0.54761(11) 0.0170(8) Uani 1 1 d . . . . .
H53 H 0.9751 0.8705 0.5387 0.020 Uiso 1 1 calc R U . . .
C54 C 0.8428(4) 0.8095(3) 0.54551(11) 0.0184(9) Uani 1 1 d . . . . .
C55 C 0.7402(4) 0.8125(3) 0.55905(12) 0.0197(9) Uani 1 1 d . . . . .
H55 H 0.6979 0.7704 0.5575 0.024 Uiso 1 1 calc R U . . .
C56 C 0.6977(4) 0.8747(3) 0.57461(11) 0.0175(9) Uani 1 1 d . . . . .
C57 C 0.5854(4) 0.8783(3) 0.58911(13) 0.0214(9) Uani 1 1 d . . . . .
C58 C 0.8825(4) 0.7387(3) 0.52895(12) 0.0209(9) Uani 1 1 d . . . . .
C61 C 0.9512(4) 1.1559(2) 0.63752(12) 0.0166(8) Uani 1 1 d . . . . .
C62 C 0.8504(4) 1.1532(2) 0.65238(12) 0.0158(8) Uani 1 1 d . . . . .
C63 C 0.8256(4) 1.1890(3) 0.68308(12) 0.0182(8) Uani 1 1 d . . . . .
H63 H 0.7571 1.1862 0.6927 0.022 Uiso 1 1 calc R U . . .
C64 C 0.9037(4) 1.2299(3) 0.70007(13) 0.0204(9) Uani 1 1 d . . . . .
C65 C 1.0040(4) 1.2298(3) 0.68547(13) 0.0232(10) Uani 1 1 d . . . . .
H65 H 1.0568 1.2567 0.6973 0.028 Uiso 1 1 calc R U . . .
C66 C 1.0317(4) 1.1923(3) 0.65420(13) 0.0209(9) Uani 1 1 d . . . . .
C67 C 1.1436(4) 1.1945(3) 0.63953(14) 0.0241(10) Uani 1 1 d . . . . .
C68 C 0.8743(4) 1.2723(3) 0.73345(13) 0.0247(10) Uani 1 1 d . . . . .
C70 C 1.0710(4) 0.9141(3) 0.60944(12) 0.0233(10) Uani 1 1 d . . . . .
C71 C 1.0982(4) 0.9609(3) 0.57861(12) 0.0191(9) Uani 1 1 d . . . . .
C72 C 1.0256(3) 1.0030(2) 0.55994(11) 0.0143(8) Uani 1 1 d . . . . .
C73 C 1.0592(4) 1.0472(3) 0.53229(12) 0.0208(9) Uani 1 1 d . . . . .
H73 H 1.0098 1.0756 0.5196 0.025 Uiso 1 1 calc R U . . .
C74 C 1.1640(4) 1.0501(3) 0.52307(14) 0.0275(10) Uani 1 1 d . . . . .
H74 H 1.1865 1.0815 0.5046 0.033 Uiso 1 1 calc R U . . .
C75 C 1.2363(4) 1.0070(3) 0.54089(16) 0.0299(11) Uani 1 1 d . . . . .
H75 H 1.3080 1.0081 0.5343 0.036 Uiso 1 1 calc R U . . .
C76 C 1.2032(4) 0.9626(3) 0.56816(15) 0.0277(11) Uani 1 1 d . . . . .
H76 H 1.2525 0.9328 0.5800 0.033 Uiso 1 1 calc R U . . .
C80 C 0.7633(5) 1.0110(3) 0.69595(13) 0.0246(10) Uani 1 1 d . . . . .
C81 C 0.6746(4) 1.0492(3) 0.67816(12) 0.0212(9) Uani 1 1 d . . . . .
C82 C 0.6823(4) 1.0919(2) 0.64759(12) 0.0176(9) Uani 1 1 d . . . . .
C83 C 0.5925(4) 1.1196(3) 0.63196(14) 0.0259(10) Uani 1 1 d . . . . .
H83 H 0.5979 1.1485 0.6112 0.031 Uiso 1 1 calc R U . . .
C84 C 0.4946(4) 1.1054(4) 0.64651(17) 0.0329(12) Uani 1 1 d . . . . .
H84 H 0.4332 1.1230 0.6352 0.039 Uiso 1 1 calc R U . . .
C85 C 0.4873(5) 1.0656(4) 0.67747(17) 0.0379(14) Uani 1 1 d . . . . .
H85 H 0.4208 1.0573 0.6879 0.045 Uiso 1 1 calc R U . . .
C86 C 0.5754(5) 1.0380(3) 0.69321(15) 0.0302(12) Uani 1 1 d . . . . .
H86 H 0.5692 1.0109 0.7146 0.036 Uiso 1 1 calc R U . . .
C171 C 0.8562(4) 0.9374(3) 0.97756(14) 0.0267(11) Uani 1 1 d . . . . .
H17A H 0.8687 0.8908 0.9659 0.040 Uiso 1 1 calc R U . . .
H17B H 0.8332 0.9290 1.0020 0.040 Uiso 1 1 calc R U . . .
H17C H 0.9210 0.9657 0.9777 0.040 Uiso 1 1 calc R U . . .
C172 C 0.7549(4) 1.0513(3) 0.97667(13) 0.0246(10) Uani 1 1 d . . . . .
H17D H 0.8213 1.0777 0.9776 0.037 Uiso 1 1 calc R U . . .
H17E H 0.7302 1.0419 1.0009 0.037 Uiso 1 1 calc R U . . .
H17F H 0.7029 1.0804 0.9639 0.037 Uiso 1 1 calc R U . . .
C173 C 0.8111(4) 0.9937(3) 0.91936(13) 0.0237(9) Uani 1 1 d . . . . .
H17G H 0.8213 0.9475 0.9070 0.036 Uiso 1 1 calc R U . . .
H17H H 0.8777 1.0197 0.9205 0.036 Uiso 1 1 calc R U . . .
H17I H 0.7598 1.0229 0.9064 0.036 Uiso 1 1 calc R U . . .
C181 C 0.6657(5) 0.7170(3) 0.99113(16) 0.0316(11) Uani 1 1 d . . . . .
H18A H 0.6568 0.6684 1.0011 0.047 Uiso 1 1 calc R U . . .
H18B H 0.6998 0.7483 1.0087 0.047 Uiso 1 1 calc R U . . .
H18C H 0.7090 0.7142 0.9697 0.047 Uiso 1 1 calc R U . . .
C182 C 0.5045(6) 0.6964(3) 0.95544(17) 0.0357(13) Uani 1 1 d . . . . .
H18D H 0.4999 0.6482 0.9662 0.054 Uiso 1 1 calc R U . . .
H18E H 0.5456 0.6937 0.9335 0.054 Uiso 1 1 calc R U . . .
H18F H 0.4341 0.7141 0.9500 0.054 Uiso 1 1 calc R U . . .
C183 C 0.4933(4) 0.7525(3) 1.01582(15) 0.0274(11) Uani 1 1 d . . . . .
H18G H 0.4872 0.7040 1.0261 0.041 Uiso 1 1 calc R U . . .
H18H H 0.4234 0.7713 1.0105 0.041 Uiso 1 1 calc R U . . .
H18I H 0.5280 0.7847 1.0328 0.041 Uiso 1 1 calc R U . . .
C271 C 0.1813(4) 1.0097(3) 0.82081(16) 0.0293(11) Uani 1 1 d . . . . .
H27A H 0.1131 0.9856 0.8201 0.044 Uiso 1 1 calc R U . . .
H27B H 0.2211 0.9921 0.8413 0.044 Uiso 1 1 calc R U . . .
H27C H 0.2198 0.9989 0.7989 0.044 Uiso 1 1 calc R U . . .
C272 C 0.0988(5) 1.1176(4) 0.79276(18) 0.0385(14) Uani 1 1 d . . . . .
H27D H 0.0317 1.0921 0.7929 0.058 Uiso 1 1 calc R U . . .
H27E H 0.1355 1.1077 0.7704 0.058 Uiso 1 1 calc R U . . .
H27F H 0.0866 1.1698 0.7950 0.058 Uiso 1 1 calc R U . . .
C273 C 0.1055(4) 1.1085(3) 0.85828(16) 0.0308(11) Uani 1 1 d . . . . .
H27G H 0.0375 1.0841 0.8578 0.046 Uiso 1 1 calc R U . . .
H27H H 0.0950 1.1609 0.8602 0.046 Uiso 1 1 calc R U . . .
H27I H 0.1457 1.0913 0.8788 0.046 Uiso 1 1 calc R U . . .
C281 C 0.4526(6) 1.2145(4) 0.73472(15) 0.0403(14) Uani 1 1 d . . . . .
H28A H 0.4712 1.2447 0.7143 0.060 Uiso 1 1 calc R U . . .
H28B H 0.3908 1.1854 0.7289 0.060 Uiso 1 1 calc R U . . .
H28C H 0.5112 1.1823 0.7405 0.060 Uiso 1 1 calc R U . . .
C282 C 0.5255(6) 1.3090(4) 0.77436(15) 0.0387(14) Uani 1 1 d . . . . .
H28D H 0.5406 1.3396 0.7537 0.058 Uiso 1 1 calc R U . . .
H28E H 0.5853 1.2771 0.7790 0.058 Uiso 1 1 calc R U . . .
H28F H 0.5129 1.3396 0.7952 0.058 Uiso 1 1 calc R U . . .
C283 C 0.3378(6) 1.3139(4) 0.7582(2) 0.0461(16) Uani 1 1 d . . . . .
H28G H 0.3572 1.3452 0.7382 0.069 Uiso 1 1 calc R U . . .
H28H H 0.3218 1.3438 0.7789 0.069 Uiso 1 1 calc R U . . .
H28I H 0.2761 1.2853 0.7517 0.069 Uiso 1 1 calc R U . . .
C571 C 0.5890(5) 0.8933(3) 0.62957(14) 0.0311(12) Uani 1 1 d . . . . .
H57A H 0.6263 0.9388 0.6339 0.047 Uiso 1 1 calc R U . . .
H57B H 0.6254 0.8535 0.6416 0.047 Uiso 1 1 calc R U . . .
H57C H 0.5175 0.8971 0.6388 0.047 Uiso 1 1 calc R U . . .
C572 C 0.5266(4) 0.8070(3) 0.58407(15) 0.0283(10) Uani 1 1 d . . . . .
H57D H 0.5643 0.7680 0.5962 0.042 Uiso 1 1 calc R U . . .
H57E H 0.5214 0.7960 0.5587 0.042 Uiso 1 1 calc R U . . .
H57F H 0.4562 0.8114 0.5941 0.042 Uiso 1 1 calc R U . . .
C573 C 0.5246(4) 0.9383(3) 0.56999(17) 0.0332(12) Uani 1 1 d . . . . .
H57G H 0.5613 0.9845 0.5730 0.050 Uiso 1 1 calc R U . . .
H57H H 0.4543 0.9420 0.5801 0.050 Uiso 1 1 calc R U . . .
H57I H 0.5195 0.9267 0.5447 0.050 Uiso 1 1 calc R U . . .
C581 C 0.9959(4) 0.7458(3) 0.51570(15) 0.0272(11) Uani 1 1 d . . . . .
H58A H 0.9998 0.7842 0.4978 0.041 Uiso 1 1 calc R U . . .
H58B H 1.0184 0.6999 0.5052 0.041 Uiso 1 1 calc R U . . .
H58C H 1.0417 0.7580 0.5357 0.041 Uiso 1 1 calc R U . . .
C582 C 0.8119(5) 0.7175(3) 0.49781(14) 0.0291(11) Uani 1 1 d . . . . .
H58D H 0.8130 0.7559 0.4799 0.044 Uiso 1 1 calc R U . . .
H58E H 0.7402 0.7107 0.5064 0.044 Uiso 1 1 calc R U . . .
H58F H 0.8371 0.6723 0.4873 0.044 Uiso 1 1 calc R U . . .
C583 C 0.8803(5) 0.6786(3) 0.55682(16) 0.0323(12) Uani 1 1 d . . . . .
H58G H 0.9253 0.6920 0.5768 0.048 Uiso 1 1 calc R U . . .
H58H H 0.9055 0.6334 0.5462 0.048 Uiso 1 1 calc R U . . .
H58I H 0.8085 0.6719 0.5653 0.048 Uiso 1 1 calc R U . . .
C671 C 1.1484(5) 1.2468(6) 0.6087(2) 0.066(3) Uani 1 1 d . . . . .
H67A H 1.1247 1.2946 0.6165 0.099 Uiso 1 1 calc R U . . .
H67B H 1.1031 1.2294 0.5895 0.099 Uiso 1 1 calc R U . . .
H67C H 1.2205 1.2501 0.6001 0.099 Uiso 1 1 calc R U . . .
C672 C 1.1803(5) 1.1194(5) 0.6281(3) 0.069(3) Uani 1 1 d . . . . .
H67D H 1.1766 1.0863 0.6484 0.104 Uiso 1 1 calc R U . . .
H67E H 1.2526 1.1222 0.6196 0.104 Uiso 1 1 calc R U . . .
H67F H 1.1352 1.1014 0.6090 0.104 Uiso 1 1 calc R U . . .
C673 C 1.2212(4) 1.2193(4) 0.66827(17) 0.0349(12) Uani 1 1 d . . . . .
H67G H 1.2187 1.1857 0.6884 0.052 Uiso 1 1 calc R U . . .
H67H H 1.2024 1.2680 0.6764 0.052 Uiso 1 1 calc R U . . .
H67I H 1.2921 1.2200 0.6584 0.052 Uiso 1 1 calc R U . . .
C681 C 0.8317(5) 1.2207(3) 0.76173(13) 0.0317(11) Uani 1 1 d . . . . .
H68A H 0.8131 1.2483 0.7830 0.048 Uiso 1 1 calc R U . . .
H68B H 0.8851 1.1847 0.7677 0.048 Uiso 1 1 calc R U . . .
H68C H 0.7694 1.1961 0.7526 0.048 Uiso 1 1 calc R U . . .
C682 C 0.7894(6) 1.3280(3) 0.72390(15) 0.0347(13) Uani 1 1 d . . . . .
H68D H 0.7702 1.3555 0.7452 0.052 Uiso 1 1 calc R U . . .
H68E H 0.7277 1.3028 0.7147 0.052 Uiso 1 1 calc R U . . .
H68F H 0.8163 1.3611 0.7057 0.052 Uiso 1 1 calc R U . . .
C683 C 0.9676(6) 1.3132(4) 0.74930(17) 0.0450(17) Uani 1 1 d . . . . .
H68G H 0.9450 1.3395 0.7706 0.067 Uiso 1 1 calc R U . . .
H68H H 0.9948 1.3475 0.7318 0.067 Uiso 1 1 calc R U . . .
H68I H 1.0225 1.2786 0.7557 0.067 Uiso 1 1 calc R U . . .
O91 O 0.8193(5) 0.9125(3) 0.78922(13) 0.0517(12) Uani 1 1 d . . . . .
H91 H 0.8064 0.9379 0.7712 0.062 Uiso 1 1 calc R U . . .
C91 C 0.8744(7) 0.9529(5) 0.8135(3) 0.057(2) Uani 1 1 d . . . . .
H91A H 0.9087 0.9934 0.8014 0.085 Uiso 1 1 calc R U . . .
H91B H 0.9275 0.9224 0.8249 0.085 Uiso 1 1 calc R U . . .
H91C H 0.8265 0.9716 0.8316 0.085 Uiso 1 1 calc R U . . .
O92 O 1.3043(12) 0.8414(6) 0.6562(5) 0.169(7) Uani 1 1 d . . . . .
H92 H 1.2512 0.8294 0.6445 0.203 Uiso 1 1 calc R U . . .
C92 C 1.2899(8) 0.9101(6) 0.6702(3) 0.067(2) Uani 1 1 d . . . . .
H92A H 1.3101 0.9103 0.6953 0.101 Uiso 1 1 calc R U . . .
H92B H 1.2162 0.9239 0.6680 0.101 Uiso 1 1 calc R U . . .
H92C H 1.3333 0.9448 0.6571 0.101 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
Os1 O1 1.704(3) . ?
Os1 O11 1.936(3) . ?
Os1 N11 1.936(4) . ?
Os1 N21 1.937(4) . ?
Os1 O21 1.941(3) . ?
Os2 O2 1.707(4) . ?
Os2 O51 1.934(3) . ?
Os2 N61 1.935(4) . ?
Os2 N51 1.935(4) . ?
Os2 O61 1.947(3) . ?
O11 C11 1.359(6) . ?
O21 C21 1.375(5) . ?
O30 C30 1.182(8) . ?
O31 C30 1.342(7) . ?
O31 C2 1.458(6) . ?
O40 C40 1.202(6) . ?
O41 C40 1.342(6) . ?
O41 C3 1.451(6) . ?
O51 C51 1.374(6) . ?
O61 C61 1.373(5) . ?
O70 C70 1.210(7) . ?
O71 C70 1.336(6) . ?
O71 C6 1.462(6) . ?
O80 C80 1.204(7) . ?
O81 C80 1.334(6) . ?
O81 C7 1.465(6) . ?
N11 C12 1.419(6) . ?
N11 C32 1.431(5) . ?
N21 C22 1.417(5) . ?
N21 C42 1.425(6) . ?
N51 C52 1.402(6) . ?
N51 C72 1.434(6) . ?
N61 C62 1.404(6) . ?
N61 C82 1.428(6) . ?
C1 C2 1.508(9) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.522(7) . ?
C2 H2 1.0000 . ?
C3 C4 1.520(8) . ?
C3 H3 1.0000 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.519(8) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.520(7) . ?
C6 H6 1.0000 . ?
C7 C8 1.516(8) . ?
C7 H7 1.0000 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C11 C16 1.383(6) . ?
C11 C12 1.409(6) . ?
C12 C13 1.385(7) . ?
C13 C14 1.401(7) . ?
C13 H13 0.9500 . ?
C14 C15 1.399(7) . ?
C14 C18 1.532(6) . ?
C15 C16 1.405(7) . ?
C15 H15 0.9500 . ?
C16 C17 1.534(6) . ?
C17 C172 1.532(7) . ?
C17 C173 1.539(6) . ?
C17 C171 1.541(6) . ?
C18 C183 1.534(7) . ?
C18 C182 1.535(7) . ?
C18 C181 1.543(7) . ?
C21 C26 1.395(6) . ?
C21 C22 1.403(7) . ?
C22 C23 1.382(6) . ?
C23 C24 1.394(7) . ?
C23 H23 0.9500 . ?
C24 C25 1.398(7) . ?
C24 C28 1.526(6) . ?
C25 C26 1.409(7) . ?
C25 H25 0.9500 . ?
C26 C27 1.532(7) . ?
C27 C271 1.529(7) . ?
C27 C272 1.532(7) . ?
C27 C273 1.534(7) . ?
C28 C282 1.528(8) . ?
C28 C283 1.528(8) . ?
C28 C281 1.539(8) . ?
C30 C31 1.497(8) . ?
C31 C36 1.397(7) . ?
C31 C32 1.408(7) . ?
C32 C33 1.381(7) . ?
C33 C34 1.395(8) . ?
C33 H33 0.9500 . ?
C34 C35 1.375(10) . ?
C34 H34 0.9500 . ?
C35 C36 1.404(10) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C40 C41 1.491(7) . ?
C41 C42 1.400(6) . ?
C41 C46 1.403(7) . ?
C42 C43 1.393(7) . ?
C43 C44 1.380(7) . ?
C43 H43 0.9500 . ?
C44 C45 1.387(7) . ?
C44 H44 0.9500 . ?
C45 C46 1.379(8) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
C51 C56 1.386(6) . ?
C51 C52 1.393(6) . ?
C52 C53 1.390(6) . ?
C53 C54 1.394(7) . ?
C53 H53 0.9500 . ?
C54 C55 1.410(7) . ?
C54 C58 1.535(6) . ?
C55 C56 1.398(7) . ?
C55 H55 0.9500 . ?
C56 C57 1.538(6) . ?
C57 C572 1.528(6) . ?
C57 C573 1.533(8) . ?
C57 C571 1.549(7) . ?
C58 C583 1.528(7) . ?
C58 C582 1.532(7) . ?
C58 C581 1.539(7) . ?
C61 C66 1.381(7) . ?
C61 C62 1.407(7) . ?
C62 C63 1.369(7) . ?
C63 C64 1.406(7) . ?
C63 H63 0.9500 . ?
C64 C65 1.396(7) . ?
C64 C68 1.528(7) . ?
C65 C66 1.412(7) . ?
C65 H65 0.9500 . ?
C66 C67 1.536(7) . ?
C67 C671 1.511(9) . ?
C67 C672 1.526(8) . ?
C67 C673 1.539(7) . ?
C68 C681 1.529(7) . ?
C68 C683 1.533(7) . ?
C68 C682 1.539(8) . ?
C70 C71 1.489(7) . ?
C71 C72 1.401(6) . ?
C71 C76 1.401(7) . ?
C72 C73 1.391(7) . ?
C73 C74 1.386(7) . ?
C73 H73 0.9500 . ?
C74 C75 1.394(8) . ?
C74 H74 0.9500 . ?
C75 C76 1.380(8) . ?
C75 H75 0.9500 . ?
C76 H76 0.9500 . ?
C80 C81 1.495(8) . ?
C81 C82 1.400(7) . ?
C81 C86 1.405(7) . ?
C82 C83 1.389(7) . ?
C83 C84 1.392(8) . ?
C83 H83 0.9500 . ?
C84 C85 1.382(10) . ?
C84 H84 0.9500 . ?
C85 C86 1.371(10) . ?
C85 H85 0.9500 . ?
C86 H86 0.9500 . ?
C171 H17A 0.9800 . ?
C171 H17B 0.9800 . ?
C171 H17C 0.9800 . ?
C172 H17D 0.9800 . ?
C172 H17E 0.9800 . ?
C172 H17F 0.9800 . ?
C173 H17G 0.9800 . ?
C173 H17H 0.9800 . ?
C173 H17I 0.9800 . ?
C181 H18A 0.9800 . ?
C181 H18B 0.9800 . ?
C181 H18C 0.9800 . ?
C182 H18D 0.9800 . ?
C182 H18E 0.9800 . ?
C182 H18F 0.9800 . ?
C183 H18G 0.9800 . ?
C183 H18H 0.9800 . ?
C183 H18I 0.9800 . ?
C271 H27A 0.9800 . ?
C271 H27B 0.9800 . ?
C271 H27C 0.9800 . ?
C272 H27D 0.9800 . ?
C272 H27E 0.9800 . ?
C272 H27F 0.9800 . ?
C273 H27G 0.9800 . ?
C273 H27H 0.9800 . ?
C273 H27I 0.9800 . ?
C281 H28A 0.9800 . ?
C281 H28B 0.9800 . ?
C281 H28C 0.9800 . ?
C282 H28D 0.9800 . ?
C282 H28E 0.9800 . ?
C282 H28F 0.9800 . ?
C283 H28G 0.9800 . ?
C283 H28H 0.9800 . ?
C283 H28I 0.9800 . ?
C571 H57A 0.9800 . ?
C571 H57B 0.9800 . ?
C571 H57C 0.9800 . ?
C572 H57D 0.9800 . ?
C572 H57E 0.9800 . ?
C572 H57F 0.9800 . ?
C573 H57G 0.9800 . ?
C573 H57H 0.9800 . ?
C573 H57I 0.9800 . ?
C581 H58A 0.9800 . ?
C581 H58B 0.9800 . ?
C581 H58C 0.9800 . ?
C582 H58D 0.9800 . ?
C582 H58E 0.9800 . ?
C582 H58F 0.9800 . ?
C583 H58G 0.9800 . ?
C583 H58H 0.9800 . ?
C583 H58I 0.9800 . ?
C671 H67A 0.9800 . ?
C671 H67B 0.9800 . ?
C671 H67C 0.9800 . ?
C672 H67D 0.9800 . ?
C672 H67E 0.9800 . ?
C672 H67F 0.9800 . ?
C673 H67G 0.9800 . ?
C673 H67H 0.9800 . ?
C673 H67I 0.9800 . ?
C681 H68A 0.9800 . ?
C681 H68B 0.9800 . ?
C681 H68C 0.9800 . ?
C682 H68D 0.9800 . ?
C682 H68E 0.9800 . ?
C682 H68F 0.9800 . ?
C683 H68G 0.9800 . ?
C683 H68H 0.9800 . ?
C683 H68I 0.9800 . ?
O91 C91 1.376(10) . ?
O91 H91 0.8400 . ?
C91 H91A 0.9800 . ?
C91 H91B 0.9800 . ?
C91 H91C 0.9800 . ?
O92 C92 1.388(13) . ?
O92 H92 0.8400 . ?
C92 H92A 0.9800 . ?
C92 H92B 0.9800 . ?
C92 H92C 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
O1 Os1 O11 108.52(15) . . ?
O1 Os1 N11 109.73(16) . . ?
O11 Os1 N11 80.89(15) . . ?
O1 Os1 N21 108.73(17) . . ?
O11 Os1 N21 86.52(15) . . ?
N11 Os1 N21 141.53(16) . . ?
O1 Os1 O21 107.88(15) . . ?
O11 Os1 O21 143.60(13) . . ?
N11 Os1 O21 87.49(15) . . ?
N21 Os1 O21 81.46(14) . . ?
O2 Os2 O51 108.27(16) . . ?
O2 Os2 N61 109.47(17) . . ?
O51 Os2 N61 86.38(15) . . ?
O2 Os2 N51 109.78(16) . . ?
O51 Os2 N51 80.53(15) . . ?
N61 Os2 N51 140.74(16) . . ?
O2 Os2 O61 108.14(16) . . ?
O51 Os2 O61 143.58(14) . . ?
N61 Os2 O61 80.71(15) . . ?
N51 Os2 O61 88.25(15) . . ?
C11 O11 Os1 115.9(3) . . ?
C21 O21 Os1 115.3(3) . . ?
C30 O31 C2 116.0(4) . . ?
C40 O41 C3 116.6(4) . . ?
C51 O51 Os2 115.9(3) . . ?
C61 O61 Os2 115.9(3) . . ?
C70 O71 C6 116.6(4) . . ?
C80 O81 C7 115.9(4) . . ?
C12 N11 C32 119.3(4) . . ?
C12 N11 Os1 115.2(3) . . ?
C32 N11 Os1 125.2(3) . . ?
C22 N21 C42 119.0(4) . . ?
C22 N21 Os1 114.8(3) . . ?
C42 N21 Os1 125.4(3) . . ?
C52 N51 C72 118.1(4) . . ?
C52 N51 Os2 116.0(3) . . ?
C72 N51 Os2 125.4(3) . . ?
C62 N61 C82 118.7(4) . . ?
C62 N61 Os2 115.7(3) . . ?
C82 N61 Os2 125.4(3) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O31 C2 C1 109.0(4) . . ?
O31 C2 C3 106.9(4) . . ?
C1 C2 C3 113.7(5) . . ?
O31 C2 H2 109.0 . . ?
C1 C2 H2 109.0 . . ?
C3 C2 H2 109.0 . . ?
O41 C3 C4 109.6(4) . . ?
O41 C3 C2 106.0(4) . . ?
C4 C3 C2 114.8(5) . . ?
O41 C3 H3 108.7 . . ?
C4 C3 H3 108.7 . . ?
C2 C3 H3 108.7 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C5 H5A 109.5 . . ?
C6 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C6 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O71 C6 C5 109.6(4) . . ?
O71 C6 C7 106.7(4) . . ?
C5 C6 C7 113.7(5) . . ?
O71 C6 H6 108.9 . . ?
C5 C6 H6 108.9 . . ?
C7 C6 H6 108.9 . . ?
O81 C7 C8 108.7(4) . . ?
O81 C7 C6 107.0(4) . . ?
C8 C7 C6 114.7(5) . . ?
O81 C7 H7 108.8 . . ?
C8 C7 H7 108.8 . . ?
C6 C7 H7 108.8 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O11 C11 C16 123.0(4) . . ?
O11 C11 C12 114.7(4) . . ?
C16 C11 C12 122.3(4) . . ?
C13 C12 C11 120.6(4) . . ?
C13 C12 N11 127.3(4) . . ?
C11 C12 N11 112.1(4) . . ?
C12 C13 C14 118.9(4) . . ?
C12 C13 H13 120.5 . . ?
C14 C13 H13 120.5 . . ?
C15 C14 C13 118.8(4) . . ?
C15 C14 C18 122.0(4) . . ?
C13 C14 C18 119.1(4) . . ?
C14 C15 C16 123.8(4) . . ?
C14 C15 H15 118.1 . . ?
C16 C15 H15 118.1 . . ?
C11 C16 C15 115.5(4) . . ?
C11 C16 C17 121.6(4) . . ?
C15 C16 C17 122.9(4) . . ?
C172 C17 C16 110.8(4) . . ?
C172 C17 C173 109.7(4) . . ?
C16 C17 C173 109.2(4) . . ?
C172 C17 C171 107.1(4) . . ?
C16 C17 C171 111.8(4) . . ?
C173 C17 C171 108.1(4) . . ?
C14 C18 C183 108.8(4) . . ?
C14 C18 C182 111.1(4) . . ?
C183 C18 C182 109.3(5) . . ?
C14 C18 C181 112.0(4) . . ?
C183 C18 C181 107.5(4) . . ?
C182 C18 C181 108.0(5) . . ?
O21 C21 C26 123.8(4) . . ?
O21 C21 C22 114.8(4) . . ?
C26 C21 C22 121.4(4) . . ?
C23 C22 C21 121.8(4) . . ?
C23 C22 N21 125.3(4) . . ?
C21 C22 N21 112.9(4) . . ?
C22 C23 C24 118.9(5) . . ?
C22 C23 H23 120.6 . . ?
C24 C23 H23 120.6 . . ?
C23 C24 C25 118.4(4) . . ?
C23 C24 C28 121.7(5) . . ?
C25 C24 C28 119.9(4) . . ?
C24 C25 C26 124.4(4) . . ?
C24 C25 H25 117.8 . . ?
C26 C25 H25 117.8 . . ?
C21 C26 C25 115.1(4) . . ?
C21 C26 C27 122.5(4) . . ?
C25 C26 C27 122.3(4) . . ?
C271 C27 C272 108.9(5) . . ?
C271 C27 C26 110.0(4) . . ?
C272 C27 C26 111.6(4) . . ?
C271 C27 C273 109.6(4) . . ?
C272 C27 C273 107.6(5) . . ?
C26 C27 C273 109.1(4) . . ?
C24 C28 C282 112.4(4) . . ?
C24 C28 C283 110.5(5) . . ?
C282 C28 C283 108.5(5) . . ?
C24 C28 C281 107.6(4) . . ?
C282 C28 C281 107.8(5) . . ?
C283 C28 C281 109.9(5) . . ?
O30 C30 O31 124.7(5) . . ?
O30 C30 C31 124.6(5) . . ?
O31 C30 C31 110.6(5) . . ?
C36 C31 C32 119.3(5) . . ?
C36 C31 C30 115.8(5) . . ?
C32 C31 C30 124.8(5) . . ?
C33 C32 C31 120.0(4) . . ?
C33 C32 N11 117.4(4) . . ?
C31 C32 N11 122.5(4) . . ?
C32 C33 C34 120.2(5) . . ?
C32 C33 H33 119.9 . . ?
C34 C33 H33 119.9 . . ?
C35 C34 C33 120.4(5) . . ?
C35 C34 H34 119.8 . . ?
C33 C34 H34 119.8 . . ?
C34 C35 C36 120.0(5) . . ?
C34 C35 H35 120.0 . . ?
C36 C35 H35 120.0 . . ?
C31 C36 C35 119.9(6) . . ?
C31 C36 H36 120.1 . . ?
C35 C36 H36 120.1 . . ?
O40 C40 O41 124.3(5) . . ?
O40 C40 C41 124.7(5) . . ?
O41 C40 C41 110.9(4) . . ?
C42 C41 C46 119.3(5) . . ?
C42 C41 C40 124.2(4) . . ?
C46 C41 C40 116.4(4) . . ?
C43 C42 C41 119.4(4) . . ?
C43 C42 N21 118.4(4) . . ?
C41 C42 N21 122.2(4) . . ?
C44 C43 C42 120.4(4) . . ?
C44 C43 H43 119.8 . . ?
C42 C43 H43 119.8 . . ?
C43 C44 C45 120.4(5) . . ?
C43 C44 H44 119.8 . . ?
C45 C44 H44 119.8 . . ?
C46 C45 C44 119.9(5) . . ?
C46 C45 H45 120.1 . . ?
C44 C45 H45 120.1 . . ?
C45 C46 C41 120.4(5) . . ?
C45 C46 H46 119.8 . . ?
C41 C46 H46 119.8 . . ?
O51 C51 C56 123.1(4) . . ?
O51 C51 C52 114.6(4) . . ?
C56 C51 C52 122.3(4) . . ?
C53 C52 C51 121.0(4) . . ?
C53 C52 N51 126.5(4) . . ?
C51 C52 N51 112.5(4) . . ?
C52 C53 C54 118.6(4) . . ?
C52 C53 H53 120.7 . . ?
C54 C53 H53 120.7 . . ?
C53 C54 C55 118.9(4) . . ?
C53 C54 C58 121.8(4) . . ?
C55 C54 C58 119.3(4) . . ?
C56 C55 C54 123.1(4) . . ?
C56 C55 H55 118.4 . . ?
C54 C55 H55 118.4 . . ?
C51 C56 C55 115.9(4) . . ?
C51 C56 C57 120.8(4) . . ?
C55 C56 C57 123.2(4) . . ?
C572 C57 C573 108.4(4) . . ?
C572 C57 C56 112.2(4) . . ?
C573 C57 C56 109.8(4) . . ?
C572 C57 C571 106.9(4) . . ?
C573 C57 C571 110.3(5) . . ?
C56 C57 C571 109.2(4) . . ?
C583 C58 C582 109.2(5) . . ?
C583 C58 C54 109.5(4) . . ?
C582 C58 C54 109.5(4) . . ?
C583 C58 C581 107.6(4) . . ?
C582 C58 C581 109.3(4) . . ?
C54 C58 C581 111.8(4) . . ?
O61 C61 C66 124.5(4) . . ?
O61 C61 C62 114.1(4) . . ?
C66 C61 C62 121.3(4) . . ?
C63 C62 N61 125.1(4) . . ?
C63 C62 C61 122.1(4) . . ?
N61 C62 C61 112.9(4) . . ?
C62 C63 C64 118.7(5) . . ?
C62 C63 H63 120.7 . . ?
C64 C63 H63 120.7 . . ?
C65 C64 C63 118.2(5) . . ?
C65 C64 C68 123.4(5) . . ?
C63 C64 C68 118.4(4) . . ?
C64 C65 C66 124.0(5) . . ?
C64 C65 H65 118.0 . . ?
C66 C65 H65 118.0 . . ?
C61 C66 C65 115.6(4) . . ?
C61 C66 C67 123.0(4) . . ?
C65 C66 C67 121.4(5) . . ?
C671 C67 C672 110.7(7) . . ?
C671 C67 C66 109.3(5) . . ?
C672 C67 C66 111.3(5) . . ?
C671 C67 C673 108.9(6) . . ?
C672 C67 C673 105.7(5) . . ?
C66 C67 C673 110.9(4) . . ?
C64 C68 C681 109.9(4) . . ?
C64 C68 C683 112.5(5) . . ?
C681 C68 C683 108.2(5) . . ?
C64 C68 C682 108.9(4) . . ?
C681 C68 C682 109.1(5) . . ?
C683 C68 C682 108.1(5) . . ?
O70 C70 O71 123.5(5) . . ?
O70 C70 C71 123.2(5) . . ?
O71 C70 C71 113.2(4) . . ?
C72 C71 C76 118.8(4) . . ?
C72 C71 C70 124.0(4) . . ?
C76 C71 C70 117.2(4) . . ?
C73 C72 C71 119.8(4) . . ?
C73 C72 N51 117.6(4) . . ?
C71 C72 N51 122.6(4) . . ?
C74 C73 C72 120.6(5) . . ?
C74 C73 H73 119.7 . . ?
C72 C73 H73 119.7 . . ?
C73 C74 C75 120.0(5) . . ?
C73 C74 H74 120.0 . . ?
C75 C74 H74 120.0 . . ?
C76 C75 C74 119.6(5) . . ?
C76 C75 H75 120.2 . . ?
C74 C75 H75 120.2 . . ?
C75 C76 C71 121.1(5) . . ?
C75 C76 H76 119.4 . . ?
C71 C76 H76 119.4 . . ?
O80 C80 O81 124.4(5) . . ?
O80 C80 C81 122.5(5) . . ?
O81 C80 C81 113.1(4) . . ?
C82 C81 C86 118.6(5) . . ?
C82 C81 C80 125.5(4) . . ?
C86 C81 C80 115.8(5) . . ?
C83 C82 C81 119.9(5) . . ?
C83 C82 N61 117.5(4) . . ?
C81 C82 N61 122.6(4) . . ?
C82 C83 C84 120.5(5) . . ?
C82 C83 H83 119.7 . . ?
C84 C83 H83 119.7 . . ?
C85 C84 C83 119.5(5) . . ?
C85 C84 H84 120.2 . . ?
C83 C84 H84 120.2 . . ?
C86 C85 C84 120.5(5) . . ?
C86 C85 H85 119.7 . . ?
C84 C85 H85 119.7 . . ?
C85 C86 C81 120.8(5) . . ?
C85 C86 H86 119.6 . . ?
C81 C86 H86 119.6 . . ?
C17 C171 H17A 109.5 . . ?
C17 C171 H17B 109.5 . . ?
H17A C171 H17B 109.5 . . ?
C17 C171 H17C 109.5 . . ?
H17A C171 H17C 109.5 . . ?
H17B C171 H17C 109.5 . . ?
C17 C172 H17D 109.5 . . ?
C17 C172 H17E 109.5 . . ?
H17D C172 H17E 109.5 . . ?
C17 C172 H17F 109.5 . . ?
H17D C172 H17F 109.5 . . ?
H17E C172 H17F 109.5 . . ?
C17 C173 H17G 109.5 . . ?
C17 C173 H17H 109.5 . . ?
H17G C173 H17H 109.5 . . ?
C17 C173 H17I 109.5 . . ?
H17G C173 H17I 109.5 . . ?
H17H C173 H17I 109.5 . . ?
C18 C181 H18A 109.5 . . ?
C18 C181 H18B 109.5 . . ?
H18A C181 H18B 109.5 . . ?
C18 C181 H18C 109.5 . . ?
H18A C181 H18C 109.5 . . ?
H18B C181 H18C 109.5 . . ?
C18 C182 H18D 109.5 . . ?
C18 C182 H18E 109.5 . . ?
H18D C182 H18E 109.5 . . ?
C18 C182 H18F 109.5 . . ?
H18D C182 H18F 109.5 . . ?
H18E C182 H18F 109.5 . . ?
C18 C183 H18G 109.5 . . ?
C18 C183 H18H 109.5 . . ?
H18G C183 H18H 109.5 . . ?
C18 C183 H18I 109.5 . . ?
H18G C183 H18I 109.5 . . ?
H18H C183 H18I 109.5 . . ?
C27 C271 H27A 109.5 . . ?
C27 C271 H27B 109.5 . . ?
H27A C271 H27B 109.5 . . ?
C27 C271 H27C 109.5 . . ?
H27A C271 H27C 109.5 . . ?
H27B C271 H27C 109.5 . . ?
C27 C272 H27D 109.5 . . ?
C27 C272 H27E 109.5 . . ?
H27D C272 H27E 109.5 . . ?
C27 C272 H27F 109.5 . . ?
H27D C272 H27F 109.5 . . ?
H27E C272 H27F 109.5 . . ?
C27 C273 H27G 109.5 . . ?
C27 C273 H27H 109.5 . . ?
H27G C273 H27H 109.5 . . ?
C27 C273 H27I 109.5 . . ?
H27G C273 H27I 109.5 . . ?
H27H C273 H27I 109.5 . . ?
C28 C281 H28A 109.5 . . ?
C28 C281 H28B 109.5 . . ?
H28A C281 H28B 109.5 . . ?
C28 C281 H28C 109.5 . . ?
H28A C281 H28C 109.5 . . ?
H28B C281 H28C 109.5 . . ?
C28 C282 H28D 109.5 . . ?
C28 C282 H28E 109.5 . . ?
H28D C282 H28E 109.5 . . ?
C28 C282 H28F 109.5 . . ?
H28D C282 H28F 109.5 . . ?
H28E C282 H28F 109.5 . . ?
C28 C283 H28G 109.5 . . ?
C28 C283 H28H 109.5 . . ?
H28G C283 H28H 109.5 . . ?
C28 C283 H28I 109.5 . . ?
H28G C283 H28I 109.5 . . ?
H28H C283 H28I 109.5 . . ?
C57 C571 H57A 109.5 . . ?
C57 C571 H57B 109.5 . . ?
H57A C571 H57B 109.5 . . ?
C57 C571 H57C 109.5 . . ?
H57A C571 H57C 109.5 . . ?
H57B C571 H57C 109.5 . . ?
C57 C572 H57D 109.5 . . ?
C57 C572 H57E 109.5 . . ?
H57D C572 H57E 109.5 . . ?
C57 C572 H57F 109.5 . . ?
H57D C572 H57F 109.5 . . ?
H57E C572 H57F 109.5 . . ?
C57 C573 H57G 109.5 . . ?
C57 C573 H57H 109.5 . . ?
H57G C573 H57H 109.5 . . ?
C57 C573 H57I 109.5 . . ?
H57G C573 H57I 109.5 . . ?
H57H C573 H57I 109.5 . . ?
C58 C581 H58A 109.5 . . ?
C58 C581 H58B 109.5 . . ?
H58A C581 H58B 109.5 . . ?
C58 C581 H58C 109.5 . . ?
H58A C581 H58C 109.5 . . ?
H58B C581 H58C 109.5 . . ?
C58 C582 H58D 109.5 . . ?
C58 C582 H58E 109.5 . . ?
H58D C582 H58E 109.5 . . ?
C58 C582 H58F 109.5 . . ?
H58D C582 H58F 109.5 . . ?
H58E C582 H58F 109.5 . . ?
C58 C583 H58G 109.5 . . ?
C58 C583 H58H 109.5 . . ?
H58G C583 H58H 109.5 . . ?
C58 C583 H58I 109.5 . . ?
H58G C583 H58I 109.5 . . ?
H58H C583 H58I 109.5 . . ?
C67 C671 H67A 109.5 . . ?
C67 C671 H67B 109.5 . . ?
H67A C671 H67B 109.5 . . ?
C67 C671 H67C 109.5 . . ?
H67A C671 H67C 109.5 . . ?
H67B C671 H67C 109.5 . . ?
C67 C672 H67D 109.5 . . ?
C67 C672 H67E 109.5 . . ?
H67D C672 H67E 109.5 . . ?
C67 C672 H67F 109.5 . . ?
H67D C672 H67F 109.5 . . ?
H67E C672 H67F 109.5 . . ?
C67 C673 H67G 109.5 . . ?
C67 C673 H67H 109.5 . . ?
H67G C673 H67H 109.5 . . ?
C67 C673 H67I 109.5 . . ?
H67G C673 H67I 109.5 . . ?
H67H C673 H67I 109.5 . . ?
C68 C681 H68A 109.5 . . ?
C68 C681 H68B 109.5 . . ?
H68A C681 H68B 109.5 . . ?
C68 C681 H68C 109.5 . . ?
H68A C681 H68C 109.5 . . ?
H68B C681 H68C 109.5 . . ?
C68 C682 H68D 109.5 . . ?
C68 C682 H68E 109.5 . . ?
H68D C682 H68E 109.5 . . ?
C68 C682 H68F 109.5 . . ?
H68D C682 H68F 109.5 . . ?
H68E C682 H68F 109.5 . . ?
C68 C683 H68G 109.5 . . ?
C68 C683 H68H 109.5 . . ?
H68G C683 H68H 109.5 . . ?
C68 C683 H68I 109.5 . . ?
H68G C683 H68I 109.5 . . ?
H68H C683 H68I 109.5 . . ?
C91 O91 H91 109.5 . . ?
O91 C91 H91A 109.5 . . ?
O91 C91 H91B 109.5 . . ?
H91A C91 H91B 109.5 . . ?
O91 C91 H91C 109.5 . . ?
H91A C91 H91C 109.5 . . ?
H91B C91 H91C 109.5 . . ?
C92 O92 H92 109.5 . . ?
O92 C92 H92A 109.5 . . ?
O92 C92 H92B 109.5 . . ?
H92A C92 H92B 109.5 . . ?
O92 C92 H92C 109.5 . . ?
H92A C92 H92C 109.5 . . ?
H92B C92 H92C 109.5 . . ?

_refine_diff_density_max         0.706
_refine_diff_density_min         -0.687
_refine_diff_density_rms         0.078

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_bdanpd
_database_code_depnum_ccdc_archive 'CCDC 2281685'
loop_
_audit_author_name
_audit_author_address
'Seth Brown'
;University of Notre Dame
United States of America
;
_audit_update_record             
;
2023-07-14 deposited with the CCDC.	2023-08-28 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT213_bdanpd              
;
PROBLEM: Atom C281 has ADP max/min Ratio .....        4.8 prolat
RESPONSE: Atom is part of a disordered tert-butyl group.
;
_vrf_PLAT220_bdanpd              
;
PROBLEM: NonSolvent Resd 1 C Ueq(max)/Ueq(min) Range   6.4 Ratio 
RESPONSE: Presence of disordered tert-butyl group leads to a 
large range of thermal parameters.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
'(C,R,R)-[2,3-butanediyl-di-2-(2-oxy-3,5-di-tert-butylphenyl-imino)benzoate]palladium hemidemimethanol solvate'
_chemical_name_common            '(C,R,R)-(Bdan)Pd . 0.25 CH3OH'
_chemical_melting_point          ?
_chemical_formula_moiety         'C46 H56 N2 O6 Pd, 0.25(C H4 O)'
_chemical_formula_sum            'C46.25 H57 N2 O6.25 Pd'
_chemical_formula_weight         847.34

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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_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'

_cell_length_a                   14.7503(5)
_cell_length_b                   19.4021(6)
_cell_length_c                   31.1892(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8925.9(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9863
_cell_measurement_theta_min      2.17
_cell_measurement_theta_max      28.02

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_F_000             3556
_exptl_transmission_factor_min   0.7721
_exptl_transmission_factor_max   0.8576
_exptl_crystal_size_max          0.162
_exptl_crystal_size_mid          0.084
_exptl_crystal_size_min          0.065
_exptl_absorpt_coefficient_mu    0.463
_shelx_estimated_absorpt_T_min   0.929
_shelx_estimated_absorpt_T_max   0.971
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.7721
_exptl_absorpt_correction_T_max  0.8576
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. 
& Stalke D., J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_recrystallization_method 
'Crystals deposited from a solution of the crude reactionmixture in methanol.'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.33
_diffrn_reflns_number            287291
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_av_R_equivalents  0.1088
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_theta_min         1.306
_diffrn_reflns_theta_max         28.319
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             22201
_reflns_number_gt                19585
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.846
_reflns_Friedel_fraction_max     0.997
_reflns_Friedel_fraction_full    1.000

_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 One tert-butyl group (attached to C28) was observed in two different
orientations.  Opposing methyl groups were constrained to have 
equal thermal displacement parameters, and the major orientation 
was refined to an occupancy of 56.4(7)%.  One lattice methanol 
was identified in the asymmetric unit.  Its occupancy was fixed at 
50%, in agreement with NMR measurements that indicate 0.25 mol methanol
per palladium.  
The carbon and oxygen atom of the lattice methanol were refined 
isotropically, while all other nonhydrogen atoms were refined 
anisotropically.  The hydrogen atoms on the disordered tert-butyl 
group and the lattice methanol were placed in calculated positions.  
All other hydrogen atoms were found on difference Fourier maps and 
refined isotropically.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0197P)²+5.6145P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
; 
 Flack x determined using 8077 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   0.020(7)
_chemical_absolute_configuration rmad
_refine_ls_number_reflns         22201
_refine_ls_number_parameters     1422
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0384
_refine_ls_wR_factor_ref         0.0693
_refine_ls_wR_factor_gt          0.0661
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_restrained_S_all      1.070
_refine_ls_shift/su_max          0.001
_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
Pd1 Pd -0.44871(2) -0.07567(2) -0.02939(2) 0.01294(6) Uani 1 1 d . . . . .
Pd2 Pd -0.13158(2) -0.21630(2) -0.33519(2) 0.01367(6) Uani 1 1 d . . . . .
O1 O -0.43484(18) 0.02494(13) -0.01692(8) 0.0175(6) Uani 1 1 d . . . . .
N1 N -0.3224(2) -0.07680(17) -0.01011(9) 0.0133(6) Uani 1 1 d . . . . .
O2 O -0.45267(19) -0.17481(13) -0.04319(9) 0.0173(6) Uani 1 1 d . . . . .
N2 N -0.5670(2) -0.07722(18) -0.05985(10) 0.0165(6) Uani 1 1 d . . . . .
C1 C -0.2851(3) 0.0504(2) -0.11701(15) 0.0210(9) Uani 1 1 d . . . . .
C2 C -0.2986(3) -0.0226(2) -0.13276(13) 0.0179(8) Uani 1 1 d . . . . .
C3 C -0.3904(3) -0.0379(2) -0.15207(12) 0.0160(8) Uani 1 1 d . . . . .
C4 C -0.4018(3) -0.1121(2) -0.16589(17) 0.0219(9) Uani 1 1 d . . . . .
O5 O -0.26293(18) -0.22433(14) -0.32150(9) 0.0180(6) Uani 1 1 d . . . . .
N5 N -0.1320(2) -0.31135(15) -0.31431(11) 0.0170(7) Uani 1 1 d . . . . .
O6 O -0.00028(17) -0.20960(14) -0.34816(8) 0.0169(6) Uani 1 1 d . . . . .
N6 N -0.1272(2) -0.11794(16) -0.35062(10) 0.0144(6) Uani 1 1 d . . . . .
C5 C -0.1862(4) -0.2154(3) -0.20044(17) 0.0313(10) Uani 1 1 d . . . . .
C6 C -0.0900(3) -0.1954(2) -0.21101(14) 0.0243(10) Uani 1 1 d . . . . .
C7 C -0.0767(3) -0.1213(2) -0.22514(14) 0.0226(9) Uani 1 1 d . . . . .
C8 C 0.0204(4) -0.1016(3) -0.2343(2) 0.0370(12) Uani 1 1 d . . . . .
O10 O -0.1391(2) -0.08307(17) -0.10975(10) 0.0312(7) Uani 1 1 d . . . . .
O11 O -0.28772(17) -0.06952(14) -0.09638(8) 0.0175(6) Uani 1 1 d . . . . .
C11 C -0.3505(3) 0.04145(19) -0.00754(12) 0.0142(8) Uani 1 1 d . . . . .
C12 C -0.2857(3) -0.01338(19) -0.00487(12) 0.0132(8) Uani 1 1 d . . . . .
C13 C -0.1923(3) 0.00027(19) 0.00098(13) 0.0153(8) Uani 1 1 d . . . . .
C14 C -0.1631(3) 0.0672(2) 0.00444(12) 0.0160(8) Uani 1 1 d . . . . .
C15 C -0.2287(3) 0.1209(2) 0.00311(13) 0.0182(8) Uani 1 1 d . . . . .
C16 C -0.3209(3) 0.11139(19) -0.00195(12) 0.0156(8) Uani 1 1 d . . . . .
C17 C -0.3883(3) 0.1713(2) -0.00295(13) 0.0195(9) Uani 1 1 d . . . . .
C18 C -0.0621(3) 0.08639(19) 0.00770(13) 0.0195(8) Uani 1 1 d . . . . .
O20 O -0.48646(19) 0.08205(15) -0.14574(9) 0.0259(7) Uani 1 1 d . . . . .
O21 O -0.46335(18) -0.02551(14) -0.12141(8) 0.0174(6) Uani 1 1 d . . . . .
C21 C -0.5191(2) -0.1911(2) -0.06906(12) 0.0149(8) Uani 1 1 d . . . . .
C22 C -0.5841(2) -0.1388(2) -0.07918(13) 0.0159(8) Uani 1 1 d . . . . .
C23 C -0.6568(3) -0.1529(2) -0.10776(14) 0.0205(9) Uani 1 1 d . . . . .
C24 C -0.6657(3) -0.2172(2) -0.12499(13) 0.0244(9) Uani 1 1 d . . . . .
C25 C -0.6000(3) -0.2683(2) -0.11484(14) 0.0225(9) Uani 1 1 d . . . . .
C26 C -0.5272(3) -0.2579(2) -0.08808(13) 0.0167(8) Uani 1 1 d . . . . .
C27 C -0.4543(3) -0.3124(2) -0.07907(14) 0.0221(9) Uani 1 1 d . . . . .
C28 C -0.7444(4) -0.2359(3) -0.15516(16) 0.0378(13) Uani 1 1 d . . . . .
C30 C -0.2050(3) -0.0945(2) -0.08816(13) 0.0179(8) Uani 1 1 d . . . . .
C31 C -0.2063(3) -0.14269(19) -0.05078(13) 0.0146(8) Uani 1 1 d . . . . .
C32 C -0.2651(3) -0.13544(19) -0.01539(12) 0.0149(8) Uani 1 1 d . . . . .
C33 C -0.2682(3) -0.1868(2) 0.01584(14) 0.0204(9) Uani 1 1 d . . . . .
C34 C -0.2107(3) -0.2434(2) 0.01287(15) 0.0242(10) Uani 1 1 d . . . . .
C35 C -0.1501(3) -0.2490(2) -0.02026(15) 0.0233(10) Uani 1 1 d . . . . .
C36 C -0.1480(3) -0.1996(2) -0.05203(14) 0.0202(9) Uani 1 1 d . . . . .
C40 C -0.5096(3) 0.0339(2) -0.12360(13) 0.0178(8) Uani 1 1 d . . . . .
C41 C -0.5936(3) 0.0339(2) -0.09724(13) 0.0170(8) Uani 1 1 d . . . . .
C42 C -0.6214(3) -0.0182(2) -0.06913(13) 0.0180(8) Uani 1 1 d . . . . .
C43 C -0.7052(3) -0.0124(2) -0.04787(15) 0.0270(10) Uani 1 1 d . . . . .
C44 C -0.7602(3) 0.0441(3) -0.05533(18) 0.0356(12) Uani 1 1 d . . . . .
C45 C -0.7327(3) 0.0960(3) -0.08240(17) 0.0321(11) Uani 1 1 d . . . . .
C46 C -0.6507(3) 0.0908(2) -0.10353(15) 0.0255(10) Uani 1 1 d . . . . .
O50 O 0.0068(3) -0.31129(18) -0.19892(12) 0.0445(10) Uani 1 1 d . . . . .
O51 O -0.0580(2) -0.23982(15) -0.24581(9) 0.0293(7) Uani 1 1 d . . . . .
C51 C -0.2848(2) -0.2849(2) -0.30563(12) 0.0163(7) Uani 1 1 d . . . . .
C52 C -0.2133(3) -0.3336(2) -0.29968(13) 0.0158(8) Uani 1 1 d . . . . .
C53 C -0.2297(3) -0.3983(2) -0.28005(14) 0.0173(8) Uani 1 1 d . . . . .
C54 C -0.3159(3) -0.4154(2) -0.26800(12) 0.0182(8) Uani 1 1 d . . . . .
C55 C -0.3871(3) -0.3667(2) -0.27595(14) 0.0187(9) Uani 1 1 d . . . . .
C56 C -0.3748(3) -0.30233(19) -0.29377(12) 0.0182(8) Uani 1 1 d . . . . .
C57 C -0.4531(3) -0.2515(2) -0.30096(14) 0.0216(9) Uani 1 1 d . . . . .
C58 C -0.3396(3) -0.4848(2) -0.24729(14) 0.0229(9) Uani 1 1 d . . . . .
O60 O -0.24273(19) -0.05913(15) -0.23096(9) 0.0216(7) Uani 1 1 d . . . . .
O61 O -0.1257(2) -0.10838(14) -0.26529(8) 0.0200(6) Uani 1 1 d . . . . .
C61 C 0.0243(3) -0.1476(2) -0.35928(12) 0.0145(8) Uani 1 1 d . . . . .
C62 C -0.0438(3) -0.09468(18) -0.36065(12) 0.0148(8) Uani 1 1 d . . . . .
C63 C -0.0208(3) -0.0261(2) -0.37168(13) 0.0161(8) Uani 1 1 d . . . . .
C64 C 0.0669(3) -0.0103(2) -0.38237(13) 0.0176(8) Uani 1 1 d . . . . .
C65 C 0.1330(3) -0.0631(2) -0.38027(13) 0.0190(8) Uani 1 1 d . . . . .
C66 C 0.1169(3) -0.1310(2) -0.36939(12) 0.0166(8) Uani 1 1 d . . . . .
C67 C 0.1901(3) -0.1871(2) -0.36833(14) 0.0207(9) Uani 1 1 d . . . . .
C68 C 0.0956(3) 0.0625(2) -0.39639(14) 0.0233(9) Uani 1 1 d . . . . .
C70 C -0.0153(3) -0.2976(2) -0.23486(14) 0.0223(9) Uani 1 1 d . . . . .
C71 C 0.0036(3) -0.3444(2) -0.27211(14) 0.0191(9) Uani 1 1 d . . . . .
C72 C -0.0517(3) -0.35191(19) -0.30841(13) 0.0179(8) Uani 1 1 d . . . . .
C73 C -0.0282(3) -0.3989(2) -0.34017(15) 0.0259(10) Uani 1 1 d . . . . .
C74 C 0.0492(3) -0.4388(2) -0.33639(16) 0.0310(10) Uani 1 1 d . . . . .
C75 C 0.1044(3) -0.4312(2) -0.30093(17) 0.0307(11) Uani 1 1 d . . . . .
C76 C 0.0817(3) -0.3853(2) -0.26895(16) 0.0256(10) Uani 1 1 d . . . . .
C80 C -0.2046(2) -0.0747(2) -0.26389(12) 0.0157(7) Uani 1 1 d . . . . .
C81 C -0.2400(3) -0.05506(19) -0.30707(12) 0.0138(8) Uani 1 1 d . . . . .
C82 C -0.2020(2) -0.0724(2) -0.34676(11) 0.0150(7) Uani 1 1 d . . . . .
C83 C -0.2408(3) -0.0467(2) -0.38454(14) 0.0209(9) Uani 1 1 d . . . . .
C84 C -0.3160(3) -0.0044(2) -0.38288(14) 0.0249(10) Uani 1 1 d . . . . .
C85 C -0.3558(3) 0.0115(2) -0.34373(14) 0.0279(10) Uani 1 1 d . . . . .
C86 C -0.3175(3) -0.0137(2) -0.30650(14) 0.0207(9) Uani 1 1 d . . . . .
C171 C -0.3409(4) 0.2404(2) 0.0057(2) 0.0321(12) Uani 1 1 d . . . . .
C172 C -0.4336(3) 0.1756(2) -0.04720(15) 0.0264(10) Uani 1 1 d . . . . .
C173 C -0.4596(4) 0.1610(2) 0.03225(17) 0.0319(11) Uani 1 1 d . . . . .
C181 C -0.0346(3) 0.1219(3) -0.03406(17) 0.0308(10) Uani 1 1 d . . . . .
C182 C -0.0453(4) 0.1345(3) 0.04580(16) 0.0316(10) Uani 1 1 d . . . . .
C183 C -0.0022(3) 0.0225(2) 0.01355(19) 0.0291(11) Uani 1 1 d . . . . .
C271 C -0.4501(4) -0.3291(2) -0.03088(16) 0.0272(9) Uani 1 1 d . . . . .
C272 C -0.4743(3) -0.3793(2) -0.10311(18) 0.0298(11) Uani 1 1 d . . . . .
C273 C -0.3612(3) -0.2863(3) -0.09418(17) 0.0291(10) Uani 1 1 d . . . . .
C281 C -0.7959(9) -0.1777(6) -0.1703(5) 0.085(5) Uani 0.564(6) 1 d . . P A 1
H28A H -0.7544 -0.1418 -0.1804 0.127 Uiso 0.564(6) 1 calc R U P A 1
H28B H -0.8329 -0.1594 -0.1468 0.127 Uiso 0.564(6) 1 calc R U P A 1
H28C H -0.8355 -0.1922 -0.1938 0.127 Uiso 0.564(6) 1 calc R U P A 1
C282 C -0.6946(7) -0.2658(7) -0.1991(3) 0.058(3) Uani 0.564(6) 1 d . . P A 1
H28D H -0.6576 -0.3061 -0.1918 0.087 Uiso 0.564(6) 1 calc R U P A 1
H28E H -0.6559 -0.2299 -0.2114 0.087 Uiso 0.564(6) 1 calc R U P A 1
H28F H -0.7410 -0.2792 -0.2200 0.087 Uiso 0.564(6) 1 calc R U P A 1
C283 C -0.7959(8) -0.2955(8) -0.1379(4) 0.051(3) Uani 0.564(6) 1 d . . P A 1
H28G H -0.7535 -0.3317 -0.1291 0.077 Uiso 0.564(6) 1 calc R U P A 1
H28H H -0.8364 -0.3135 -0.1602 0.077 Uiso 0.564(6) 1 calc R U P A 1
H28I H -0.8319 -0.2807 -0.1132 0.077 Uiso 0.564(6) 1 calc R U P A 1
C284 C -0.7654(14) -0.3092(9) -0.1573(7) 0.085(5) Uani 0.436(6) 1 d . . P A 2
H28J H -0.7658 -0.3285 -0.1282 0.127 Uiso 0.436(6) 1 calc R U P A 2
H28K H -0.7194 -0.3328 -0.1745 0.127 Uiso 0.436(6) 1 calc R U P A 2
H28L H -0.8251 -0.3156 -0.1705 0.127 Uiso 0.436(6) 1 calc R U P A 2
C285 C -0.8397(9) -0.2083(9) -0.1306(4) 0.058(3) Uani 0.436(6) 1 d . . P A 2
H28M H -0.8462 -0.2318 -0.1029 0.087 Uiso 0.436(6) 1 calc R U P A 2
H28N H -0.8923 -0.2187 -0.1487 0.087 Uiso 0.436(6) 1 calc R U P A 2
H28O H -0.8359 -0.1585 -0.1259 0.087 Uiso 0.436(6) 1 calc R U P A 2
C286 C -0.7411(10) -0.2008(9) -0.1947(4) 0.051(3) Uani 0.436(6) 1 d . . P A 2
H28P H -0.7269 -0.1521 -0.1897 0.077 Uiso 0.436(6) 1 calc R U P A 2
H28Q H -0.8000 -0.2045 -0.2091 0.077 Uiso 0.436(6) 1 calc R U P A 2
H28R H -0.6941 -0.2214 -0.2129 0.077 Uiso 0.436(6) 1 calc R U P A 2
C571 C -0.4350(3) -0.1866(3) -0.2738(2) 0.0326(12) Uani 1 1 d . . . . .
C572 C -0.4595(4) -0.2313(3) -0.34841(17) 0.0334(11) Uani 1 1 d . . . . .
C573 C -0.5443(3) -0.2816(3) -0.28720(19) 0.0333(11) Uani 1 1 d . . . . .
C581 C -0.4001(4) -0.5257(3) -0.27856(19) 0.0339(12) Uani 1 1 d . . . . .
C582 C -0.2555(3) -0.5285(3) -0.23810(17) 0.0294(11) Uani 1 1 d . . . . .
C583 C -0.3905(4) -0.4733(3) -0.20529(18) 0.0358(12) Uani 1 1 d . . . . .
C671 C 0.1962(3) -0.2175(3) -0.32282(15) 0.0270(10) Uani 1 1 d . . . . .
C672 C 0.1657(3) -0.2444(3) -0.40044(18) 0.0286(11) Uani 1 1 d . . . . .
C673 C 0.2832(3) -0.1589(3) -0.38071(19) 0.0293(11) Uani 1 1 d . . . . .
C681 C 0.0143(3) 0.1102(3) -0.40197(19) 0.0308(11) Uani 1 1 d . . . . .
C682 C 0.1596(4) 0.0929(3) -0.3626(2) 0.0347(12) Uani 1 1 d . . . . .
C683 C 0.1451(4) 0.0576(3) -0.43972(17) 0.0350(12) Uani 1 1 d . . . . .
O9 O -0.9624(18) -0.1155(12) -0.1156(8) 0.224(10) Uiso 0.5 1 d . . P . .
H9 H -1.0146 -0.0983 -0.1140 0.268 Uiso 0.5 1 calc R U P . .
C9 C -0.921(2) -0.1137(18) -0.0754(12) 0.225(16) Uiso 0.5 1 d . . P . .
H9A H -0.8942 -0.0682 -0.0707 0.338 Uiso 0.5 1 calc R U P . .
H9B H -0.8738 -0.1490 -0.0740 0.338 Uiso 0.5 1 calc R U P . .
H9C H -0.9667 -0.1227 -0.0532 0.338 Uiso 0.5 1 calc R U P . .
H1A H -0.328(3) 0.060(2) -0.0952(16) 0.030(13) Uiso 1 1 d . . . . .
H1B H -0.224(3) 0.060(2) -0.1037(14) 0.025(12) Uiso 1 1 d . . . . .
H1C H -0.295(3) 0.083(2) -0.1433(14) 0.023(12) Uiso 1 1 d . . . . .
H2 H -0.252(3) -0.0342(19) -0.1518(12) 0.006(10) Uiso 1 1 d . . . . .
H3 H -0.399(3) -0.008(2) -0.1786(14) 0.020(12) Uiso 1 1 d . . . . .
H4A H -0.462(4) -0.120(3) -0.1772(16) 0.043(15) Uiso 1 1 d . . . . .
H4B H -0.395(3) -0.140(2) -0.1430(15) 0.017(11) Uiso 1 1 d . . . . .
H4C H -0.359(4) -0.124(3) -0.1877(17) 0.041(15) Uiso 1 1 d . . . . .
H5A H -0.187(3) -0.265(3) -0.1924(15) 0.032(14) Uiso 1 1 d . . . . .
H5B H -0.214(3) -0.190(2) -0.1784(15) 0.028(13) Uiso 1 1 d . . . . .
H5C H -0.216(3) -0.213(3) -0.2261(16) 0.031(13) Uiso 1 1 d . . . . .
H6 H -0.050(3) -0.202(2) -0.1869(13) 0.019(11) Uiso 1 1 d . . . . .
H7 H -0.102(3) -0.094(2) -0.2047(14) 0.018(12) Uiso 1 1 d . . . . .
H8A H 0.027(4) -0.052(3) -0.2435(18) 0.052(18) Uiso 1 1 d . . . . .
H8B H 0.053(3) -0.104(2) -0.2108(16) 0.026(12) Uiso 1 1 d . . . . .
H8C H 0.048(4) -0.131(3) -0.2540(18) 0.046(16) Uiso 1 1 d . . . . .
H13 H -0.150(3) -0.034(2) 0.0031(14) 0.020(11) Uiso 1 1 d . . . . .
H15 H -0.206(3) 0.1687(19) 0.0081(12) 0.005(9) Uiso 1 1 d . . . . .
H17A H -0.298(4) 0.249(3) -0.017(2) 0.06(2) Uiso 1 1 d . . . . .
H17B H -0.308(3) 0.241(2) 0.0344(16) 0.028(13) Uiso 1 1 d . . . . .
H17C H -0.388(3) 0.277(2) 0.0045(13) 0.018(11) Uiso 1 1 d . . . . .
H17D H -0.391(3) 0.182(2) -0.0701(15) 0.026(13) Uiso 1 1 d . . . . .
H17E H -0.469(3) 0.135(3) -0.0552(15) 0.028(13) Uiso 1 1 d . . . . .
H17F H -0.481(3) 0.213(2) -0.0466(13) 0.023(11) Uiso 1 1 d . . . . .
H17G H -0.493(3) 0.121(3) 0.0275(18) 0.040(15) Uiso 1 1 d . . . . .
H17H H -0.502(3) 0.202(3) 0.0294(16) 0.037(13) Uiso 1 1 d . . . . .
H17I H -0.425(4) 0.166(3) 0.0649(18) 0.049(16) Uiso 1 1 d . . . . .
H18A H 0.030(4) 0.132(3) -0.0337(17) 0.040(14) Uiso 1 1 d . . . . .
H18B H -0.046(3) 0.093(2) -0.0571(14) 0.018(11) Uiso 1 1 d . . . . .
H18C H -0.071(3) 0.166(3) -0.0385(16) 0.036(14) Uiso 1 1 d . . . . .
H18D H -0.068(3) 0.114(2) 0.0707(14) 0.014(11) Uiso 1 1 d . . . . .
H18E H 0.021(3) 0.145(2) 0.0517(13) 0.017(11) Uiso 1 1 d . . . . .
H18F H -0.084(3) 0.174(3) 0.0423(16) 0.038(15) Uiso 1 1 d . . . . .
H18G H -0.018(4) -0.004(3) 0.0374(18) 0.045(16) Uiso 1 1 d . . . . .
H18H H -0.005(3) -0.009(3) -0.0106(16) 0.029(13) Uiso 1 1 d . . . . .
H18I H 0.061(3) 0.039(2) 0.0163(14) 0.029(13) Uiso 1 1 d . . . . .
H23 H -0.698(3) -0.115(2) -0.1132(13) 0.013(10) Uiso 1 1 d . . . . .
H25 H -0.608(3) -0.312(2) -0.1267(15) 0.026(13) Uiso 1 1 d . . . . .
H27A H -0.508(3) -0.345(2) -0.0191(15) 0.028(13) Uiso 1 1 d . . . . .
H27B H -0.398(3) -0.361(3) -0.0269(16) 0.033(13) Uiso 1 1 d . . . . .
H27C H -0.431(4) -0.289(3) -0.0142(17) 0.054(17) Uiso 1 1 d . . . . .
H27D H -0.535(3) -0.395(2) -0.0921(13) 0.017(11) Uiso 1 1 d . . . . .
H27E H -0.478(3) -0.373(2) -0.1322(16) 0.024(13) Uiso 1 1 d . . . . .
H27F H -0.427(4) -0.414(3) -0.0962(17) 0.046(16) Uiso 1 1 d . . . . .
H27G H -0.362(3) -0.275(3) -0.1238(16) 0.035(14) Uiso 1 1 d . . . . .
H27H H -0.314(3) -0.322(2) -0.0899(13) 0.015(11) Uiso 1 1 d . . . . .
H27I H -0.344(3) -0.243(3) -0.0812(16) 0.035(14) Uiso 1 1 d . . . . .
H33 H -0.311(3) -0.185(2) 0.0378(14) 0.015(11) Uiso 1 1 d . . . . .
H34 H -0.211(3) -0.274(3) 0.0330(16) 0.036(14) Uiso 1 1 d . . . . .
H35 H -0.111(3) -0.283(2) -0.0212(14) 0.027(12) Uiso 1 1 d . . . . .
H36 H -0.108(3) -0.204(2) -0.0742(12) 0.009(10) Uiso 1 1 d . . . . .
H43 H -0.721(3) -0.050(2) -0.0282(14) 0.017(11) Uiso 1 1 d . . . . .
H44 H -0.805(4) 0.046(3) -0.039(2) 0.06(2) Uiso 1 1 d . . . . .
H45 H -0.771(3) 0.132(3) -0.0864(16) 0.033(14) Uiso 1 1 d . . . . .
H46 H -0.636(3) 0.125(2) -0.1227(13) 0.016(11) Uiso 1 1 d . . . . .
H53 H -0.184(3) -0.427(2) -0.2758(14) 0.026(12) Uiso 1 1 d . . . . .
H55 H -0.446(3) -0.3806(18) -0.2695(11) 0.006(9) Uiso 1 1 d . . . . .
H57A H -0.484(3) -0.153(2) -0.2766(14) 0.017(11) Uiso 1 1 d . . . . .
H57B H -0.438(4) -0.196(3) -0.2452(18) 0.040(16) Uiso 1 1 d . . . . .
H57C H -0.383(4) -0.164(3) -0.2820(16) 0.036(15) Uiso 1 1 d . . . . .
H57D H -0.472(3) -0.271(3) -0.3639(17) 0.041(16) Uiso 1 1 d . . . . .
H57E H -0.510(3) -0.198(3) -0.3530(16) 0.037(14) Uiso 1 1 d . . . . .
H57F H -0.403(4) -0.218(3) -0.361(2) 0.07(2) Uiso 1 1 d . . . . .
H57G H -0.591(3) -0.246(2) -0.2919(14) 0.020(12) Uiso 1 1 d . . . . .
H57H H -0.543(3) -0.291(3) -0.2565(16) 0.036(14) Uiso 1 1 d . . . . .
H57I H -0.555(4) -0.321(3) -0.3056(17) 0.045(15) Uiso 1 1 d . . . . .
H58A H -0.371(4) -0.535(3) -0.3050(19) 0.049(17) Uiso 1 1 d . . . . .
H58B H -0.420(3) -0.567(3) -0.2666(16) 0.036(14) Uiso 1 1 d . . . . .
H58C H -0.459(5) -0.505(3) -0.2843(19) 0.064(19) Uiso 1 1 d . . . . .
H58D H -0.273(3) -0.572(3) -0.2255(14) 0.025(12) Uiso 1 1 d . . . . .
H58E H -0.215(3) -0.508(2) -0.2157(16) 0.032(14) Uiso 1 1 d . . . . .
H58F H -0.220(3) -0.540(2) -0.2644(16) 0.027(13) Uiso 1 1 d . . . . .
H58G H -0.353(4) -0.450(3) -0.1854(19) 0.053(18) Uiso 1 1 d . . . . .
H58H H -0.451(4) -0.452(2) -0.2089(15) 0.036(14) Uiso 1 1 d . . . . .
H58I H -0.404(3) -0.517(3) -0.1919(17) 0.041(15) Uiso 1 1 d . . . . .
H63 H -0.064(3) 0.006(2) -0.3726(13) 0.017(11) Uiso 1 1 d . . . . .
H65 H 0.191(3) -0.052(2) -0.3857(14) 0.019(12) Uiso 1 1 d . . . . .
H67A H 0.216(3) -0.186(3) -0.3037(17) 0.035(15) Uiso 1 1 d . . . . .
H67B H 0.243(3) -0.258(2) -0.3229(14) 0.026(12) Uiso 1 1 d . . . . .
H67C H 0.141(4) -0.240(3) -0.3114(17) 0.047(16) Uiso 1 1 d . . . . .
H67D H 0.165(3) -0.227(3) -0.4284(17) 0.038(15) Uiso 1 1 d . . . . .
H67E H 0.109(3) -0.262(2) -0.3933(15) 0.026(13) Uiso 1 1 d . . . . .
H67F H 0.213(3) -0.281(2) -0.3977(13) 0.017(10) Uiso 1 1 d . . . . .
H67G H 0.301(3) -0.124(2) -0.3623(15) 0.020(12) Uiso 1 1 d . . . . .
H67H H 0.286(3) -0.139(2) -0.4078(16) 0.026(13) Uiso 1 1 d . . . . .
H67I H 0.332(4) -0.193(3) -0.3788(16) 0.046(16) Uiso 1 1 d . . . . .
H68A H 0.040(4) 0.153(3) -0.4108(17) 0.044(15) Uiso 1 1 d . . . . .
H68B H -0.031(4) 0.096(3) -0.4255(17) 0.046(16) Uiso 1 1 d . . . . .
H68C H -0.015(3) 0.114(2) -0.3761(14) 0.011(11) Uiso 1 1 d . . . . .
H68D H 0.173(4) 0.137(3) -0.3693(17) 0.043(16) Uiso 1 1 d . . . . .
H68E H 0.136(4) 0.093(2) -0.3323(18) 0.043(15) Uiso 1 1 d . . . . .
H68F H 0.210(4) 0.064(3) -0.3617(18) 0.051(17) Uiso 1 1 d . . . . .
H68G H 0.098(4) 0.040(3) -0.4594(18) 0.049(17) Uiso 1 1 d . . . . .
H68H H 0.162(3) 0.100(2) -0.4516(15) 0.028(13) Uiso 1 1 d . . . . .
H68I H 0.200(3) 0.029(2) -0.4374(15) 0.028(13) Uiso 1 1 d . . . . .
H73 H -0.069(3) -0.405(2) -0.3655(14) 0.016(11) Uiso 1 1 d . . . . .
H74 H 0.067(4) -0.468(3) -0.3602(17) 0.044(15) Uiso 1 1 d . . . . .
H75 H 0.155(3) -0.456(2) -0.2984(15) 0.026(13) Uiso 1 1 d . . . . .
H76 H 0.116(3) -0.380(2) -0.2414(15) 0.028(13) Uiso 1 1 d . . . . .
H83 H -0.216(3) -0.057(2) -0.4123(14) 0.020(12) Uiso 1 1 d . . . . .
H84 H -0.341(3) 0.013(2) -0.4070(15) 0.028(13) Uiso 1 1 d . . . . .
H85 H -0.408(3) 0.038(2) -0.3422(14) 0.022(12) Uiso 1 1 d . . . . .
H86 H -0.345(3) -0.002(2) -0.2807(14) 0.017(11) Uiso 1 1 d . . . . .


_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
Pd1 N1 1.959(3) . ?
Pd1 O2 1.972(3) . ?
Pd1 N2 1.987(3) . ?
Pd1 O1 2.001(3) . ?
Pd2 N5 1.956(3) . ?
Pd2 N6 1.969(3) . ?
Pd2 O6 1.983(3) . ?
Pd2 O5 1.990(3) . ?
O1 C11 1.318(5) . ?
N1 C12 1.354(5) . ?
N1 C32 1.427(5) . ?
O2 C21 1.308(5) . ?
N2 C22 1.362(5) . ?
N2 C42 1.428(5) . ?
C1 C2 1.513(6) . ?
C1 H1A 0.95(5) . ?
C1 H1B 1.00(5) . ?
C1 H1C 1.04(5) . ?
C2 O11 1.464(5) . ?
C2 C3 1.512(6) . ?
C2 H2 0.93(4) . ?
C3 O21 1.459(4) . ?
C3 C4 1.512(6) . ?
C3 H3 1.02(4) . ?
C4 H4A 0.96(6) . ?
C4 H4B 0.90(5) . ?
C4 H4C 0.96(6) . ?
O5 C51 1.316(5) . ?
N5 C52 1.354(5) . ?
N5 C72 1.433(5) . ?
O6 C61 1.303(5) . ?
N6 C62 1.347(5) . ?
N6 C82 1.418(5) . ?
C5 C6 1.507(7) . ?
C5 H5A 0.99(5) . ?
C5 H5B 0.94(5) . ?
C5 H5C 0.92(5) . ?
C6 O51 1.464(5) . ?
C6 C7 1.515(6) . ?
C6 H6 0.97(4) . ?
C7 O61 1.467(5) . ?
C7 C8 1.511(7) . ?
C7 H7 0.91(4) . ?
C8 H8A 1.01(6) . ?
C8 H8B 0.88(5) . ?
C8 H8C 0.93(6) . ?
O10 C30 1.203(5) . ?
O11 C30 1.338(5) . ?
C11 C12 1.433(5) . ?
C11 C16 1.436(5) . ?
C12 C13 1.414(5) . ?
C13 C14 1.373(5) . ?
C13 H13 0.92(4) . ?
C14 C15 1.422(5) . ?
C14 C18 1.539(6) . ?
C15 C16 1.381(6) . ?
C15 H15 1.00(4) . ?
C16 C17 1.530(5) . ?
C17 C173 1.533(6) . ?
C17 C172 1.535(6) . ?
C17 C171 1.536(6) . ?
C18 C181 1.528(6) . ?
C18 C182 1.531(6) . ?
C18 C183 1.533(6) . ?
O20 C40 1.210(5) . ?
O21 C40 1.342(5) . ?
C21 C26 1.429(5) . ?
C21 C22 1.432(5) . ?
C22 C23 1.421(5) . ?
C23 C24 1.366(6) . ?
C23 H23 0.97(4) . ?
C24 C25 1.421(6) . ?
C24 C28 1.538(6) . ?
C25 C26 1.374(6) . ?
C25 H25 0.93(5) . ?
C26 C27 1.535(6) . ?
C27 C272 1.527(6) . ?
C27 C273 1.537(6) . ?
C27 C271 1.539(6) . ?
C28 C286 1.411(14) . ?
C28 C281 1.440(12) . ?
C28 C284 1.456(18) . ?
C28 C283 1.485(13) . ?
C28 C282 1.659(12) . ?
C28 C285 1.688(15) . ?
C30 C31 1.494(6) . ?
C31 C36 1.400(5) . ?
C31 C32 1.410(5) . ?
C32 C33 1.394(5) . ?
C33 C34 1.391(6) . ?
C33 H33 0.94(4) . ?
C34 C35 1.370(7) . ?
C34 H34 0.86(5) . ?
C35 C36 1.378(6) . ?
C35 H35 0.88(5) . ?
C36 H36 0.92(4) . ?
C40 C41 1.488(5) . ?
C41 C42 1.400(6) . ?
C41 C46 1.401(6) . ?
C42 C43 1.407(6) . ?
C43 C44 1.384(6) . ?
C43 H43 0.98(4) . ?
C44 C45 1.375(7) . ?
C44 H44 0.84(6) . ?
C45 C46 1.381(6) . ?
C45 H45 0.90(5) . ?
C46 H46 0.92(4) . ?
O50 C70 1.197(5) . ?
O51 C70 1.330(5) . ?
C51 C56 1.419(5) . ?
C51 C52 1.429(5) . ?
C52 C53 1.417(5) . ?
C53 C54 1.366(5) . ?
C53 H53 0.88(5) . ?
C54 C55 1.435(6) . ?
C54 C58 1.534(6) . ?
C55 C56 1.379(6) . ?
C55 H55 0.93(4) . ?
C56 C57 1.535(5) . ?
C57 C573 1.528(6) . ?
C57 C572 1.534(7) . ?
C57 C571 1.540(6) . ?
C58 C583 1.526(7) . ?
C58 C582 1.529(6) . ?
C58 C581 1.542(7) . ?
O60 C80 1.209(4) . ?
O61 C80 1.337(5) . ?
C61 C62 1.437(5) . ?
C61 C66 1.438(5) . ?
C62 C63 1.416(5) . ?
C63 C64 1.370(6) . ?
C63 H63 0.89(4) . ?
C64 C65 1.417(6) . ?
C64 C68 1.538(5) . ?
C65 C66 1.382(6) . ?
C65 H65 0.90(4) . ?
C66 C67 1.533(6) . ?
C67 C673 1.528(6) . ?
C67 C672 1.539(6) . ?
C67 C671 1.540(6) . ?
C68 C681 1.525(6) . ?
C68 C682 1.534(7) . ?
C68 C683 1.539(7) . ?
C70 C71 1.501(6) . ?
C71 C76 1.402(5) . ?
C71 C72 1.403(6) . ?
C72 C73 1.390(6) . ?
C73 C74 1.385(6) . ?
C73 H73 1.00(4) . ?
C74 C75 1.382(7) . ?
C74 H74 0.97(5) . ?
C75 C76 1.377(7) . ?
C75 H75 0.90(5) . ?
C76 H76 1.00(5) . ?
C80 C81 1.494(5) . ?
C81 C86 1.397(5) . ?
C81 C82 1.400(5) . ?
C82 C83 1.402(5) . ?
C83 C84 1.380(6) . ?
C83 H83 0.96(4) . ?
C84 C85 1.390(6) . ?
C84 H84 0.91(5) . ?
C85 C86 1.381(6) . ?
C85 H85 0.94(4) . ?
C86 H86 0.93(4) . ?
C171 H17A 0.95(6) . ?
C171 H17B 1.02(5) . ?
C171 H17C 0.99(4) . ?
C172 H17D 0.96(5) . ?
C172 H17E 0.98(5) . ?
C172 H17F 1.01(5) . ?
C173 H17G 0.92(5) . ?
C173 H17H 1.01(5) . ?
C173 H17I 1.14(6) . ?
C181 H18A 0.97(5) . ?
C181 H18B 0.93(4) . ?
C181 H18C 1.01(5) . ?
C182 H18D 0.93(4) . ?
C182 H18E 1.02(4) . ?
C182 H18F 0.96(5) . ?
C183 H18G 0.93(6) . ?
C183 H18H 0.97(5) . ?
C183 H18I 0.98(5) . ?
C271 H27A 0.98(5) . ?
C271 H27B 1.00(5) . ?
C271 H27C 0.98(6) . ?
C272 H27D 1.01(4) . ?
C272 H27E 0.92(5) . ?
C272 H27F 0.99(5) . ?
C273 H27G 0.95(5) . ?
C273 H27H 0.99(4) . ?
C273 H27I 0.96(5) . ?
C281 H28A 0.9800 . ?
C281 H28B 0.9800 . ?
C281 H28C 0.9800 . ?
C282 H28D 0.9800 . ?
C282 H28E 0.9800 . ?
C282 H28F 0.9800 . ?
C283 H28G 0.9800 . ?
C283 H28H 0.9800 . ?
C283 H28I 0.9800 . ?
C284 H28J 0.9800 . ?
C284 H28K 0.9800 . ?
C284 H28L 0.9800 . ?
C285 H28M 0.9800 . ?
C285 H28N 0.9800 . ?
C285 H28O 0.9800 . ?
C286 H28P 0.9800 . ?
C286 H28Q 0.9800 . ?
C286 H28R 0.9800 . ?
C571 H57A 0.97(4) . ?
C571 H57B 0.91(5) . ?
C571 H57C 0.92(5) . ?
C572 H57D 0.92(6) . ?
C572 H57E 1.00(5) . ?
C572 H57F 0.96(6) . ?
C573 H57G 0.99(4) . ?
C573 H57H 0.97(5) . ?
C573 H57I 0.97(5) . ?
C581 H58A 0.95(6) . ?
C581 H58B 0.94(5) . ?
C581 H58C 0.98(7) . ?
C582 H58D 0.96(5) . ?
C582 H58E 1.01(5) . ?
C582 H58F 1.00(5) . ?
C583 H58G 0.95(6) . ?
C583 H58H 0.98(5) . ?
C583 H58I 0.97(6) . ?
C671 H67A 0.90(5) . ?
C671 H67B 1.04(5) . ?
C671 H67C 1.00(6) . ?
C672 H67D 0.94(5) . ?
C672 H67E 0.93(5) . ?
C672 H67F 1.00(4) . ?
C673 H67G 0.93(5) . ?
C673 H67H 0.93(5) . ?
C673 H67I 0.98(6) . ?
C681 H68A 0.96(5) . ?
C681 H68B 1.03(6) . ?
C681 H68C 0.92(4) . ?
C682 H68D 0.91(6) . ?
C682 H68E 1.01(5) . ?
C682 H68F 0.93(6) . ?
C683 H68G 0.99(6) . ?
C683 H68H 0.94(5) . ?
C683 H68I 0.98(5) . ?
O9 C9 1.39(3) . ?
O9 H9 0.8400 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 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
N1 Pd1 O2 94.83(13) . . ?
N1 Pd1 N2 169.21(12) . . ?
O2 Pd1 N2 81.65(13) . . ?
N1 Pd1 O1 81.61(12) . . ?
O2 Pd1 O1 175.62(12) . . ?
N2 Pd1 O1 101.39(12) . . ?
N5 Pd2 N6 174.44(14) . . ?
N5 Pd2 O6 97.62(13) . . ?
N6 Pd2 O6 81.62(13) . . ?
N5 Pd2 O5 81.48(13) . . ?
N6 Pd2 O5 99.23(13) . . ?
O6 Pd2 O5 179.04(12) . . ?
C11 O1 Pd1 112.1(2) . . ?
C12 N1 C32 120.1(3) . . ?
C12 N1 Pd1 114.0(3) . . ?
C32 N1 Pd1 122.5(2) . . ?
C21 O2 Pd1 113.1(2) . . ?
C22 N2 C42 120.6(3) . . ?
C22 N2 Pd1 112.8(3) . . ?
C42 N2 Pd1 125.3(3) . . ?
C2 C1 H1A 110(3) . . ?
C2 C1 H1B 115(3) . . ?
H1A C1 H1B 105(4) . . ?
C2 C1 H1C 107(2) . . ?
H1A C1 H1C 111(4) . . ?
H1B C1 H1C 110(3) . . ?
O11 C2 C3 106.5(3) . . ?
O11 C2 C1 108.4(3) . . ?
C3 C2 C1 115.5(3) . . ?
O11 C2 H2 105(2) . . ?
C3 C2 H2 111(2) . . ?
C1 C2 H2 110(2) . . ?
O21 C3 C2 111.5(3) . . ?
O21 C3 C4 105.2(3) . . ?
C2 C3 C4 113.6(3) . . ?
O21 C3 H3 110(2) . . ?
C2 C3 H3 109(2) . . ?
C4 C3 H3 108(2) . . ?
C3 C4 H4A 110(3) . . ?
C3 C4 H4B 109(3) . . ?
H4A C4 H4B 108(4) . . ?
C3 C4 H4C 111(3) . . ?
H4A C4 H4C 108(4) . . ?
H4B C4 H4C 110(4) . . ?
C51 O5 Pd2 112.9(2) . . ?
C52 N5 C72 120.8(3) . . ?
C52 N5 Pd2 114.6(3) . . ?
C72 N5 Pd2 123.9(3) . . ?
C61 O6 Pd2 112.8(2) . . ?
C62 N6 C82 121.4(3) . . ?
C62 N6 Pd2 114.3(3) . . ?
C82 N6 Pd2 123.9(3) . . ?
C6 C5 H5A 108(3) . . ?
C6 C5 H5B 116(3) . . ?
H5A C5 H5B 109(4) . . ?
C6 C5 H5C 105(3) . . ?
H5A C5 H5C 105(4) . . ?
H5B C5 H5C 114(4) . . ?
O51 C6 C5 108.3(4) . . ?
O51 C6 C7 107.5(3) . . ?
C5 C6 C7 115.4(4) . . ?
O51 C6 H6 107(2) . . ?
C5 C6 H6 112(3) . . ?
C7 C6 H6 106(3) . . ?
O61 C7 C8 105.1(4) . . ?
O61 C7 C6 110.3(3) . . ?
C8 C7 C6 114.7(4) . . ?
O61 C7 H7 107(3) . . ?
C8 C7 H7 113(3) . . ?
C6 C7 H7 107(3) . . ?
C7 C8 H8A 113(3) . . ?
C7 C8 H8B 110(3) . . ?
H8A C8 H8B 104(4) . . ?
C7 C8 H8C 112(4) . . ?
H8A C8 H8C 111(5) . . ?
H8B C8 H8C 106(5) . . ?
C30 O11 C2 118.3(3) . . ?
O1 C11 C12 117.6(3) . . ?
O1 C11 C16 122.9(3) . . ?
C12 C11 C16 119.4(3) . . ?
N1 C12 C13 125.1(3) . . ?
N1 C12 C11 113.6(3) . . ?
C13 C12 C11 121.2(3) . . ?
C14 C13 C12 119.5(4) . . ?
C14 C13 H13 118(3) . . ?
C12 C13 H13 122(3) . . ?
C13 C14 C15 118.5(4) . . ?
C13 C14 C18 122.5(3) . . ?
C15 C14 C18 118.9(3) . . ?
C16 C15 C14 125.2(4) . . ?
C16 C15 H15 118(2) . . ?
C14 C15 H15 117(2) . . ?
C15 C16 C11 116.0(3) . . ?
C15 C16 C17 122.7(4) . . ?
C11 C16 C17 121.2(4) . . ?
C16 C17 C173 109.4(3) . . ?
C16 C17 C172 110.0(3) . . ?
C173 C17 C172 110.6(4) . . ?
C16 C17 C171 111.3(4) . . ?
C173 C17 C171 107.4(4) . . ?
C172 C17 C171 108.0(4) . . ?
C181 C18 C182 110.1(4) . . ?
C181 C18 C183 108.3(4) . . ?
C182 C18 C183 107.9(4) . . ?
C181 C18 C14 108.0(3) . . ?
C182 C18 C14 110.8(4) . . ?
C183 C18 C14 111.8(3) . . ?
C40 O21 C3 118.9(3) . . ?
O2 C21 C26 122.5(3) . . ?
O2 C21 C22 117.8(3) . . ?
C26 C21 C22 119.7(3) . . ?
N2 C22 C23 125.9(4) . . ?
N2 C22 C21 113.6(3) . . ?
C23 C22 C21 120.5(4) . . ?
C24 C23 C22 119.7(4) . . ?
C24 C23 H23 124(2) . . ?
C22 C23 H23 116(2) . . ?
C23 C24 C25 118.9(4) . . ?
C23 C24 C28 121.9(4) . . ?
C25 C24 C28 119.2(4) . . ?
C26 C25 C24 124.4(4) . . ?
C26 C25 H25 118(3) . . ?
C24 C25 H25 118(3) . . ?
C25 C26 C21 116.8(4) . . ?
C25 C26 C27 123.8(4) . . ?
C21 C26 C27 119.4(3) . . ?
C272 C27 C26 111.1(4) . . ?
C272 C27 C273 107.6(4) . . ?
C26 C27 C273 110.0(3) . . ?
C272 C27 C271 108.0(4) . . ?
C26 C27 C271 110.6(4) . . ?
C273 C27 C271 109.5(4) . . ?
C286 C28 C284 116.1(11) . . ?
C281 C28 C283 117.3(9) . . ?
C286 C28 C24 113.3(6) . . ?
C281 C28 C24 114.4(5) . . ?
C284 C28 C24 114.7(7) . . ?
C283 C28 C24 110.4(6) . . ?
C281 C28 C282 103.8(9) . . ?
C283 C28 C282 104.6(7) . . ?
C24 C28 C282 104.7(5) . . ?
C286 C28 C285 105.8(9) . . ?
C284 C28 C285 98.8(12) . . ?
C24 C28 C285 106.0(5) . . ?
O10 C30 O11 124.2(4) . . ?
O10 C30 C31 124.3(4) . . ?
O11 C30 C31 111.4(3) . . ?
C36 C31 C32 118.6(4) . . ?
C36 C31 C30 117.6(4) . . ?
C32 C31 C30 123.8(3) . . ?
C33 C32 C31 119.8(4) . . ?
C33 C32 N1 118.0(4) . . ?
C31 C32 N1 122.3(3) . . ?
C34 C33 C32 119.8(4) . . ?
C34 C33 H33 119(3) . . ?
C32 C33 H33 121(3) . . ?
C35 C34 C33 120.7(4) . . ?
C35 C34 H34 119(3) . . ?
C33 C34 H34 120(3) . . ?
C34 C35 C36 120.1(4) . . ?
C34 C35 H35 121(3) . . ?
C36 C35 H35 119(3) . . ?
C35 C36 C31 120.9(4) . . ?
C35 C36 H36 119(2) . . ?
C31 C36 H36 120(3) . . ?
O20 C40 O21 123.3(4) . . ?
O20 C40 C41 123.4(4) . . ?
O21 C40 C41 113.3(3) . . ?
C42 C41 C46 118.7(4) . . ?
C42 C41 C40 126.2(4) . . ?
C46 C41 C40 115.0(4) . . ?
C41 C42 C43 119.6(4) . . ?
C41 C42 N2 122.8(4) . . ?
C43 C42 N2 117.6(4) . . ?
C44 C43 C42 120.0(4) . . ?
C44 C43 H43 124(2) . . ?
C42 C43 H43 116(2) . . ?
C45 C44 C43 120.6(5) . . ?
C45 C44 H44 125(4) . . ?
C43 C44 H44 113(4) . . ?
C44 C45 C46 119.9(4) . . ?
C44 C45 H45 117(3) . . ?
C46 C45 H45 123(3) . . ?
C45 C46 C41 121.1(4) . . ?
C45 C46 H46 118(3) . . ?
C41 C46 H46 121(3) . . ?
C70 O51 C6 117.3(3) . . ?
O5 C51 C56 122.7(3) . . ?
O5 C51 C52 117.3(3) . . ?
C56 C51 C52 120.0(4) . . ?
N5 C52 C53 125.4(4) . . ?
N5 C52 C51 113.5(3) . . ?
C53 C52 C51 121.0(4) . . ?
C54 C53 C52 119.6(4) . . ?
C54 C53 H53 121(3) . . ?
C52 C53 H53 119(3) . . ?
C53 C54 C55 118.3(4) . . ?
C53 C54 C58 122.8(4) . . ?
C55 C54 C58 118.9(4) . . ?
C56 C55 C54 124.7(4) . . ?
C56 C55 H55 118(2) . . ?
C54 C55 H55 117(2) . . ?
C55 C56 C51 116.3(4) . . ?
C55 C56 C57 122.8(4) . . ?
C51 C56 C57 120.9(4) . . ?
C573 C57 C572 108.3(4) . . ?
C573 C57 C56 112.1(4) . . ?
C572 C57 C56 110.6(4) . . ?
C573 C57 C571 108.1(4) . . ?
C572 C57 C571 109.4(4) . . ?
C56 C57 C571 108.3(3) . . ?
C583 C58 C582 108.6(4) . . ?
C583 C58 C54 110.2(4) . . ?
C582 C58 C54 112.3(4) . . ?
C583 C58 C581 109.5(4) . . ?
C582 C58 C581 107.7(4) . . ?
C54 C58 C581 108.5(4) . . ?
C80 O61 C7 119.0(3) . . ?
O6 C61 C62 118.2(3) . . ?
O6 C61 C66 122.0(3) . . ?
C62 C61 C66 119.8(4) . . ?
N6 C62 C63 126.2(4) . . ?
N6 C62 C61 113.1(3) . . ?
C63 C62 C61 120.8(4) . . ?
C64 C63 C62 119.7(4) . . ?
C64 C63 H63 120(3) . . ?
C62 C63 H63 120(3) . . ?
C63 C64 C65 118.5(4) . . ?
C63 C64 C68 122.3(4) . . ?
C65 C64 C68 119.2(4) . . ?
C66 C65 C64 125.6(4) . . ?
C66 C65 H65 117(3) . . ?
C64 C65 H65 118(3) . . ?
C65 C66 C61 115.5(4) . . ?
C65 C66 C67 124.1(4) . . ?
C61 C66 C67 120.3(4) . . ?
C673 C67 C66 112.0(4) . . ?
C673 C67 C672 107.7(4) . . ?
C66 C67 C672 109.5(3) . . ?
C673 C67 C671 108.5(4) . . ?
C66 C67 C671 109.4(3) . . ?
C672 C67 C671 109.7(4) . . ?
C681 C68 C682 109.3(4) . . ?
C681 C68 C64 111.9(4) . . ?
C682 C68 C64 109.0(4) . . ?
C681 C68 C683 108.1(4) . . ?
C682 C68 C683 109.6(4) . . ?
C64 C68 C683 108.9(4) . . ?
O50 C70 O51 123.8(4) . . ?
O50 C70 C71 122.6(4) . . ?
O51 C70 C71 113.6(4) . . ?
C76 C71 C72 118.4(4) . . ?
C76 C71 C70 116.2(4) . . ?
C72 C71 C70 125.4(3) . . ?
C73 C72 C71 119.8(4) . . ?
C73 C72 N5 118.3(4) . . ?
C71 C72 N5 121.8(3) . . ?
C74 C73 C72 120.8(5) . . ?
C74 C73 H73 120(2) . . ?
C72 C73 H73 119(2) . . ?
C75 C74 C73 119.6(4) . . ?
C75 C74 H74 121(3) . . ?
C73 C74 H74 119(3) . . ?
C76 C75 C74 120.3(4) . . ?
C76 C75 H75 120(3) . . ?
C74 C75 H75 120(3) . . ?
C75 C76 C71 121.0(4) . . ?
C75 C76 H76 124(3) . . ?
C71 C76 H76 115(3) . . ?
O60 C80 O61 123.7(4) . . ?
O60 C80 C81 122.7(3) . . ?
O61 C80 C81 113.6(3) . . ?
C86 C81 C82 118.5(4) . . ?
C86 C81 C80 114.9(3) . . ?
C82 C81 C80 126.6(3) . . ?
C81 C82 C83 119.6(4) . . ?
C81 C82 N6 122.4(3) . . ?
C83 C82 N6 117.9(3) . . ?
C84 C83 C82 120.5(4) . . ?
C84 C83 H83 118(3) . . ?
C82 C83 H83 122(3) . . ?
C83 C84 C85 120.3(4) . . ?
C83 C84 H84 122(3) . . ?
C85 C84 H84 118(3) . . ?
C86 C85 C84 119.2(4) . . ?
C86 C85 H85 120(3) . . ?
C84 C85 H85 121(3) . . ?
C85 C86 C81 121.8(4) . . ?
C85 C86 H86 118(3) . . ?
C81 C86 H86 120(3) . . ?
C17 C171 H17A 109(4) . . ?
C17 C171 H17B 112(3) . . ?
H17A C171 H17B 109(5) . . ?
C17 C171 H17C 107(2) . . ?
H17A C171 H17C 108(4) . . ?
H17B C171 H17C 111(4) . . ?
C17 C172 H17D 113(3) . . ?
C17 C172 H17E 115(3) . . ?
H17D C172 H17E 105(4) . . ?
C17 C172 H17F 109(2) . . ?
H17D C172 H17F 113(4) . . ?
H17E C172 H17F 102(4) . . ?
C17 C173 H17G 111(3) . . ?
C17 C173 H17H 105(3) . . ?
H17G C173 H17H 108(4) . . ?
C17 C173 H17I 109(3) . . ?
H17G C173 H17I 116(4) . . ?
H17H C173 H17I 107(4) . . ?
C18 C181 H18A 110(3) . . ?
C18 C181 H18B 110(3) . . ?
H18A C181 H18B 108(4) . . ?
C18 C181 H18C 111(3) . . ?
H18A C181 H18C 111(4) . . ?
H18B C181 H18C 108(4) . . ?
C18 C182 H18D 109(3) . . ?
C18 C182 H18E 114(2) . . ?
H18D C182 H18E 106(4) . . ?
C18 C182 H18F 108(3) . . ?
H18D C182 H18F 103(4) . . ?
H18E C182 H18F 116(4) . . ?
C18 C183 H18G 113(3) . . ?
C18 C183 H18H 113(3) . . ?
H18G C183 H18H 105(4) . . ?
C18 C183 H18I 107(3) . . ?
H18G C183 H18I 110(4) . . ?
H18H C183 H18I 108(4) . . ?
C27 C271 H27A 113(3) . . ?
C27 C271 H27B 107(3) . . ?
H27A C271 H27B 115(4) . . ?
C27 C271 H27C 111(3) . . ?
H27A C271 H27C 108(4) . . ?
H27B C271 H27C 102(4) . . ?
C27 C272 H27D 105(2) . . ?
C27 C272 H27E 113(3) . . ?
H27D C272 H27E 109(4) . . ?
C27 C272 H27F 109(3) . . ?
H27D C272 H27F 111(4) . . ?
H27E C272 H27F 110(4) . . ?
C27 C273 H27G 111(3) . . ?
C27 C273 H27H 111(2) . . ?
H27G C273 H27H 108(4) . . ?
C27 C273 H27I 114(3) . . ?
H27G C273 H27I 102(4) . . ?
H27H C273 H27I 111(4) . . ?
C28 C281 H28A 109.5 . . ?
C28 C281 H28B 109.5 . . ?
H28A C281 H28B 109.5 . . ?
C28 C281 H28C 109.5 . . ?
H28A C281 H28C 109.5 . . ?
H28B C281 H28C 109.5 . . ?
C28 C282 H28D 109.5 . . ?
C28 C282 H28E 109.5 . . ?
H28D C282 H28E 109.5 . . ?
C28 C282 H28F 109.5 . . ?
H28D C282 H28F 109.5 . . ?
H28E C282 H28F 109.5 . . ?
C28 C283 H28G 109.5 . . ?
C28 C283 H28H 109.5 . . ?
H28G C283 H28H 109.5 . . ?
C28 C283 H28I 109.5 . . ?
H28G C283 H28I 109.5 . . ?
H28H C283 H28I 109.5 . . ?
C28 C284 H28J 109.5 . . ?
C28 C284 H28K 109.5 . . ?
H28J C284 H28K 109.5 . . ?
C28 C284 H28L 109.5 . . ?
H28J C284 H28L 109.5 . . ?
H28K C284 H28L 109.5 . . ?
C28 C285 H28M 109.5 . . ?
C28 C285 H28N 109.5 . . ?
H28M C285 H28N 109.5 . . ?
C28 C285 H28O 109.5 . . ?
H28M C285 H28O 109.5 . . ?
H28N C285 H28O 109.5 . . ?
C28 C286 H28P 109.5 . . ?
C28 C286 H28Q 109.5 . . ?
H28P C286 H28Q 109.5 . . ?
C28 C286 H28R 109.5 . . ?
H28P C286 H28R 109.5 . . ?
H28Q C286 H28R 109.5 . . ?
C57 C571 H57A 112(3) . . ?
C57 C571 H57B 111(3) . . ?
H57A C571 H57B 101(4) . . ?
C57 C571 H57C 112(3) . . ?
H57A C571 H57C 106(4) . . ?
H57B C571 H57C 114(5) . . ?
C57 C572 H57D 108(3) . . ?
C57 C572 H57E 110(3) . . ?
H57D C572 H57E 108(4) . . ?
C57 C572 H57F 114(4) . . ?
H57D C572 H57F 101(5) . . ?
H57E C572 H57F 115(5) . . ?
C57 C573 H57G 107(3) . . ?
C57 C573 H57H 109(3) . . ?
H57G C573 H57H 107(4) . . ?
C57 C573 H57I 106(3) . . ?
H57G C573 H57I 111(4) . . ?
H57H C573 H57I 116(4) . . ?
C58 C581 H58A 113(4) . . ?
C58 C581 H58B 112(3) . . ?
H58A C581 H58B 109(4) . . ?
C58 C581 H58C 115(4) . . ?
H58A C581 H58C 109(5) . . ?
H58B C581 H58C 98(4) . . ?
C58 C582 H58D 110(3) . . ?
C58 C582 H58E 113(3) . . ?
H58D C582 H58E 103(4) . . ?
C58 C582 H58F 113(3) . . ?
H58D C582 H58F 106(4) . . ?
H58E C582 H58F 110(4) . . ?
C58 C583 H58G 110(3) . . ?
C58 C583 H58H 114(3) . . ?
H58G C583 H58H 114(4) . . ?
C58 C583 H58I 110(3) . . ?
H58G C583 H58I 105(5) . . ?
H58H C583 H58I 104(4) . . ?
C67 C671 H67A 112(3) . . ?
C67 C671 H67B 109(2) . . ?
H67A C671 H67B 107(4) . . ?
C67 C671 H67C 117(3) . . ?
H67A C671 H67C 109(4) . . ?
H67B C671 H67C 103(4) . . ?
C67 C672 H67D 110(3) . . ?
C67 C672 H67E 109(3) . . ?
H67D C672 H67E 110(4) . . ?
C67 C672 H67F 107(2) . . ?
H67D C672 H67F 110(4) . . ?
H67E C672 H67F 110(4) . . ?
C67 C673 H67G 111(3) . . ?
C67 C673 H67H 115(3) . . ?
H67G C673 H67H 104(4) . . ?
C67 C673 H67I 113(3) . . ?
H67G C673 H67I 105(4) . . ?
H67H C673 H67I 108(4) . . ?
C68 C681 H68A 104(3) . . ?
C68 C681 H68B 115(3) . . ?
H68A C681 H68B 107(4) . . ?
C68 C681 H68C 108(3) . . ?
H68A C681 H68C 112(4) . . ?
H68B C681 H68C 110(4) . . ?
C68 C682 H68D 110(3) . . ?
C68 C682 H68E 115(3) . . ?
H68D C682 H68E 107(4) . . ?
C68 C682 H68F 106(3) . . ?
H68D C682 H68F 114(5) . . ?
H68E C682 H68F 105(4) . . ?
C68 C683 H68G 103(3) . . ?
C68 C683 H68H 114(3) . . ?
H68G C683 H68H 104(4) . . ?
C68 C683 H68I 111(3) . . ?
H68G C683 H68I 116(4) . . ?
H68H C683 H68I 108(4) . . ?
C9 O9 H9 109.5 . . ?
O9 C9 H9A 109.5 . . ?
O9 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
O9 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?

_refine_diff_density_max         0.380
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.068

_shelxl_version_number           2013-4

