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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_aposeg
_database_code_depnum_ccdc_archive 'CCDC 2003363'
loop_
_audit_author_name
_audit_author_address
'Seth Brown' 'University of Notre Dame'
_audit_update_record             
;
2020-05-11 deposited with the CCDC.	2020-06-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
'Bis(2-phenylimido-4,6-di-tert-butylphenoxo)ethyleneglycolato-osmium(VI) hemi-hexane solvate'
_chemical_name_common            '(Hap)2Os(OCH2CH2O) . 0.5 C6H14'
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H54 N2 O4 Os, 0.5(C6 H14)'
_chemical_formula_sum            'C45 H61 N2 O4 Os'
_chemical_formula_weight         884.15

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'
Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

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

_cell_length_a                   12.2153(6)
_cell_length_b                   13.1499(7)
_cell_length_c                   13.2104(7)
_cell_angle_alpha                103.1226(17)
_cell_angle_beta                 91.7443(16)
_cell_angle_gamma                97.8182(17)
_cell_volume                     2043.22(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9838
_cell_measurement_theta_min      2.39
_cell_measurement_theta_max      28.25

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_F_000             906
_exptl_transmission_factor_min   0.7728
_exptl_transmission_factor_max   0.9004
_exptl_crystal_size_max          0.121
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.064
_exptl_absorpt_coefficient_mu    3.164
_shelx_estimated_absorpt_T_min   0.701
_shelx_estimated_absorpt_T_max   0.823
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.7728
_exptl_absorpt_correction_T_max  0.9004
_exptl_absorpt_process_details   
;
L. Krause, R. Herbst-Irmer, G. M. Sheldrick & D. Stalke. J. Appl.
Cryst., 2015, 48, 3.
;

_exptl_special_details           
; 
 ? 
;

_exptl_crystal_recrystallization_method 
'Crystals were formed by slow evaporation of a solution of the compound dissolved in hexane.'


_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            29521
_diffrn_reflns_av_unetI/netI     0.0463
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.586
_diffrn_reflns_theta_max         28.266
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             10122
_reflns_number_gt                9073
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker 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 tert-butyl group centered at C181 was disordered over two
different orientations, as were the two carbons of the 
ethylene glycolate ligand.  In each case, the alternative 
orientations were refined by initially constraining the 
corresponding atoms in the two parts to have equal thermal
parameters and allowing the occupancies to refine.  The major
component of the tert-butyl group refined to 75.7(5)% occupancy 
and the major glycolate conformation refined to 56.2(11)% occupancy.
These occupancies were then fixed and the thermal parameters 
allowed to vary in the final refinement cycles.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0272P)²+1.7865P] 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_number_reflns         10122
_refine_ls_number_parameters     543
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0357
_refine_ls_wR_factor_ref         0.0692
_refine_ls_wR_factor_gt          0.0672
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_restrained_S_all      1.121
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Os Os 0.28448(2) 1.15981(2) 0.39823(2) 0.01426(4) Uani 1 1 d . . . . .
O1 O 0.27143(19) 1.28123(18) 0.51405(18) 0.0185(5) Uani 1 1 d . . . . .
N1 N 0.3335(2) 1.1071(2) 0.5180(2) 0.0159(6) Uani 1 1 d . . . . .
O2 O 0.15414(19) 1.04874(18) 0.38083(18) 0.0176(5) Uani 1 1 d . . . . .
N2 N 0.1789(2) 1.2180(2) 0.3194(2) 0.0179(6) Uani 1 1 d . . . . .
O3 O 0.3342(2) 1.0651(2) 0.2781(2) 0.0326(7) Uani 1 1 d . . . . .
O4 O 0.4254(2) 1.2405(2) 0.3816(2) 0.0338(7) Uani 1 1 d . . . . .
C1A C 0.4097(8) 1.1082(8) 0.2222(7) 0.0295(19) Uani 0.562 1 d . . P A 1
H1A1 H 0.3750 1.1468 0.1768 0.035 Uiso 0.562 1 calc R U P A 1
H1A2 H 0.4474 1.0534 0.1785 0.035 Uiso 0.562 1 calc R U P A 1
C2A C 0.4907(17) 1.1833(13) 0.3045(18) 0.031(3) Uani 0.562 1 d . . P A 1
H2A1 H 0.5387 1.1433 0.3373 0.037 Uiso 0.562 1 calc R U P A 1
H2A2 H 0.5382 1.2331 0.2725 0.037 Uiso 0.562 1 calc R U P A 1
C1B C 0.4442(11) 1.0973(10) 0.2578(10) 0.034(3) Uani 0.438 1 d . . P A 2
H1B1 H 0.4517 1.0802 0.1816 0.041 Uiso 0.438 1 calc R U P A 2
H1B2 H 0.4938 1.0578 0.2893 0.041 Uiso 0.438 1 calc R U P A 2
C2B C 0.479(2) 1.2125(16) 0.300(2) 0.026(4) Uani 0.438 1 d . . P A 2
H2B1 H 0.5596 1.2275 0.3185 0.032 Uiso 0.438 1 calc R U P A 2
H2B2 H 0.4618 1.2520 0.2476 0.032 Uiso 0.438 1 calc R U P A 2
C11 C 0.3281(3) 1.2824(3) 0.6020(3) 0.0188(7) Uani 1 1 d . . . . .
C12 C 0.3595(3) 1.1849(3) 0.6088(3) 0.0176(7) Uani 1 1 d . . . . .
C13 C 0.4129(3) 1.1735(3) 0.7011(3) 0.0225(8) Uani 1 1 d . . . . .
H13 H 0.4304 1.1067 0.7068 0.027 Uiso 1 1 calc R U . . .
C14 C 0.4392(3) 1.2608(3) 0.7829(3) 0.0244(8) Uani 1 1 d . . . . .
C15 C 0.4068(3) 1.3577(3) 0.7728(3) 0.0241(8) Uani 1 1 d . . . . .
H15 H 0.4237 1.4167 0.8303 0.029 Uiso 1 1 calc R U . . .
C16 C 0.3527(3) 1.3724(3) 0.6857(3) 0.0189(7) Uani 1 1 d . . . . .
C17 C 0.3242(3) 1.4797(3) 0.6764(3) 0.0218(7) Uani 1 1 d . . . . .
C18 C 0.5049(4) 1.2569(3) 0.8828(3) 0.0383(11) Uani 1 1 d . . . . .
C21 C 0.0801(3) 1.0508(3) 0.3050(3) 0.0171(7) Uani 1 1 d . . . . .
C22 C 0.0873(3) 1.1467(3) 0.2739(3) 0.0170(7) Uani 1 1 d . . . . .
C23 C 0.0063(3) 1.1625(3) 0.2035(3) 0.0183(7) Uani 1 1 d . . . . .
H23 H 0.0100 1.2284 0.1847 0.022 Uiso 1 1 calc R U . . .
C24 C -0.0785(3) 1.0818(3) 0.1621(3) 0.0197(7) Uani 1 1 d . . . . .
C25 C -0.0801(3) 0.9846(3) 0.1916(3) 0.0209(7) Uani 1 1 d . . . . .
H25 H -0.1382 0.9291 0.1617 0.025 Uiso 1 1 calc R U . . .
C26 C -0.0034(3) 0.9647(3) 0.2607(3) 0.0184(7) Uani 1 1 d . . . . .
C27 C -0.0029(3) 0.8563(3) 0.2854(3) 0.0227(8) Uani 1 1 d . . . . .
C28 C -0.1695(3) 1.0931(3) 0.0837(3) 0.0258(8) Uani 1 1 d . . . . .
C31 C 0.3168(3) 0.9983(3) 0.5221(3) 0.0191(7) Uani 1 1 d . . . . .
C32 C 0.2479(3) 0.9648(3) 0.5930(3) 0.0240(8) Uani 1 1 d . . . . .
H32 H 0.2146 1.0143 0.6418 0.029 Uiso 1 1 calc R U . . .
C33 C 0.2279(3) 0.8581(3) 0.5922(3) 0.0298(9) Uani 1 1 d . . . . .
H33 H 0.1797 0.8345 0.6399 0.036 Uiso 1 1 calc R U . . .
C34 C 0.2776(3) 0.7861(3) 0.5226(3) 0.0317(9) Uani 1 1 d . . . . .
H34 H 0.2637 0.7132 0.5225 0.038 Uiso 1 1 calc R U . . .
C35 C 0.3475(3) 0.8201(3) 0.4532(3) 0.0316(9) Uani 1 1 d . . . . .
H35 H 0.3829 0.7707 0.4064 0.038 Uiso 1 1 calc R U . . .
C36 C 0.3664(3) 0.9264(3) 0.4514(3) 0.0252(8) Uani 1 1 d . . . . .
H36 H 0.4128 0.9495 0.4022 0.030 Uiso 1 1 calc R U . . .
C41 C 0.1786(3) 1.3281(3) 0.3266(3) 0.0270(8) Uani 1 1 d . . . . .
C42 C 0.2721(4) 1.3874(3) 0.3028(4) 0.0443(12) Uani 1 1 d . . . . .
H42 H 0.3352 1.3549 0.2817 0.053 Uiso 1 1 calc R U . . .
C43 C 0.2743(5) 1.4950(4) 0.3095(5) 0.0612(17) Uani 1 1 d . . . . .
H43 H 0.3386 1.5356 0.2928 0.073 Uiso 1 1 calc R U . . .
C44 C 0.1840(5) 1.5418(3) 0.3402(4) 0.0573(16) Uani 1 1 d . . . . .
H44 H 0.1848 1.6147 0.3427 0.069 Uiso 1 1 calc R U . . .
C45 C 0.0926(5) 1.4845(4) 0.3672(4) 0.0484(14) Uani 1 1 d . . . . .
H45 H 0.0311 1.5185 0.3905 0.058 Uiso 1 1 calc R U . . .
C46 C 0.0878(4) 1.3766(3) 0.3610(3) 0.0341(10) Uani 1 1 d . . . . .
H46 H 0.0239 1.3371 0.3800 0.041 Uiso 1 1 calc R U . . .
C171 C 0.3556(4) 1.5641(3) 0.7770(3) 0.0312(9) Uani 1 1 d . . . . .
H17A H 0.3367 1.6317 0.7679 0.047 Uiso 1 1 calc R U . . .
H17B H 0.4353 1.5712 0.7940 0.047 Uiso 1 1 calc R U . . .
H17C H 0.3149 1.5435 0.8337 0.047 Uiso 1 1 calc R U . . .
C172 C 0.3896(3) 1.5135(3) 0.5886(3) 0.0288(9) Uani 1 1 d . . . . .
H17D H 0.3725 1.5822 0.5813 0.043 Uiso 1 1 calc R U . . .
H17E H 0.3688 1.4609 0.5230 0.043 Uiso 1 1 calc R U . . .
H17F H 0.4691 1.5188 0.6057 0.043 Uiso 1 1 calc R U . . .
C173 C 0.1997(3) 1.4738(3) 0.6510(3) 0.0281(8) Uani 1 1 d . . . . .
H17G H 0.1838 1.5433 0.6449 0.042 Uiso 1 1 calc R U . . .
H17H H 0.1583 1.4522 0.7069 0.042 Uiso 1 1 calc R U . . .
H17I H 0.1776 1.4221 0.5851 0.042 Uiso 1 1 calc R U . . .
C181 C 0.6037(6) 1.3401(6) 0.9054(6) 0.0476(19) Uani 0.757 1 d . . P B 1
H18A H 0.5809 1.4087 0.9053 0.071 Uiso 0.757 1 calc R U P B 1
H18B H 0.6567 1.3239 0.8519 0.071 Uiso 0.757 1 calc R U P B 1
H18C H 0.6386 1.3424 0.9738 0.071 Uiso 0.757 1 calc R U P B 1
C182 C 0.4226(6) 1.2820(5) 0.9770(4) 0.0485(17) Uani 0.757 1 d . . P B 1
H18D H 0.3571 1.2277 0.9640 0.073 Uiso 0.757 1 calc R U P B 1
H18E H 0.3997 1.3513 0.9808 0.073 Uiso 0.757 1 calc R U P B 1
H18F H 0.4614 1.2822 1.0431 0.073 Uiso 0.757 1 calc R U P B 1
C183 C 0.5353(5) 1.1510(5) 0.8823(5) 0.0382(14) Uani 0.757 1 d . . P B 1
H18G H 0.4686 1.0981 0.8671 0.057 Uiso 0.757 1 calc R U P B 1
H18H H 0.5694 1.1519 0.9507 0.057 Uiso 0.757 1 calc R U P B 1
H18I H 0.5879 1.1332 0.8288 0.057 Uiso 0.757 1 calc R U P B 1
C184 C 0.4624(19) 1.1697(17) 0.9223(14) 0.044(5) Uani 0.243 1 d . . P B 2
H18J H 0.4351 1.1096 0.8643 0.067 Uiso 0.243 1 calc R U P B 2
H18K H 0.4014 1.1879 0.9662 0.067 Uiso 0.243 1 calc R U P B 2
H18L H 0.5211 1.1510 0.9638 0.067 Uiso 0.243 1 calc R U P B 2
C185 C 0.6328(15) 1.2209(17) 0.8280(13) 0.042(5) Uani 0.243 1 d . . P B 2
H18M H 0.6690 1.2779 0.7986 0.064 Uiso 0.243 1 calc R U P B 2
H18N H 0.6161 1.1560 0.7729 0.064 Uiso 0.243 1 calc R U P B 2
H18O H 0.6822 1.2093 0.8828 0.064 Uiso 0.243 1 calc R U P B 2
C186 C 0.5510(18) 1.3591(16) 0.9458(16) 0.038(5) Uani 0.243 1 d . . P B 2
H18P H 0.5751 1.4065 0.9006 0.057 Uiso 0.243 1 calc R U P B 2
H18Q H 0.6147 1.3521 0.9894 0.057 Uiso 0.243 1 calc R U P B 2
H18R H 0.4948 1.3884 0.9904 0.057 Uiso 0.243 1 calc R U P B 2
C271 C -0.0982(4) 0.7751(3) 0.2244(3) 0.0325(9) Uani 1 1 d . . . . .
H27A H -0.0918 0.7691 0.1496 0.049 Uiso 1 1 calc R U . . .
H27B H -0.1691 0.7981 0.2445 0.049 Uiso 1 1 calc R U . . .
H27C H -0.0945 0.7063 0.2403 0.049 Uiso 1 1 calc R U . . .
C272 C -0.0145(3) 0.8626(3) 0.4015(3) 0.0290(9) Uani 1 1 d . . . . .
H27D H -0.0137 0.7925 0.4152 0.044 Uiso 1 1 calc R U . . .
H27E H -0.0845 0.8874 0.4219 0.044 Uiso 1 1 calc R U . . .
H27F H 0.0473 0.9120 0.4419 0.044 Uiso 1 1 calc R U . . .
C273 C 0.1069(3) 0.8173(3) 0.2526(3) 0.0322(9) Uani 1 1 d . . . . .
H27G H 0.1139 0.8134 0.1781 0.048 Uiso 1 1 calc R U . . .
H27H H 0.1078 0.7471 0.2660 0.048 Uiso 1 1 calc R U . . .
H27I H 0.1690 0.8665 0.2927 0.048 Uiso 1 1 calc R U . . .
C281 C -0.2817(3) 1.0757(6) 0.1286(4) 0.0610(17) Uani 1 1 d . . . . .
H28A H -0.3399 1.0818 0.0786 0.091 Uiso 1 1 calc R U . . .
H28B H -0.2836 1.1289 0.1936 0.091 Uiso 1 1 calc R U . . .
H28C H -0.2941 1.0051 0.1427 0.091 Uiso 1 1 calc R U . . .
C282 C -0.1534(4) 1.2017(4) 0.0600(4) 0.0487(13) Uani 1 1 d . . . . .
H28D H -0.2129 1.2059 0.0103 0.073 Uiso 1 1 calc R U . . .
H28E H -0.0818 1.2137 0.0301 0.073 Uiso 1 1 calc R U . . .
H28F H -0.1554 1.2556 0.1245 0.073 Uiso 1 1 calc R U . . .
C283 C -0.1683(4) 1.0104(4) -0.0175(3) 0.0438(12) Uani 1 1 d . . . . .
H28G H -0.2270 1.0170 -0.0668 0.066 Uiso 1 1 calc R U . . .
H28H H -0.1807 0.9398 -0.0036 0.066 Uiso 1 1 calc R U . . .
H28I H -0.0964 1.0213 -0.0474 0.066 Uiso 1 1 calc R U . . .
C51 C -0.219(3) 1.644(2) 0.9578(17) 0.211(17) Uani 0.5 1 d . . P C -1
H51A H -0.2515 1.6327 0.8868 0.316 Uiso 0.5 1 calc R U P C -1
H51B H -0.1851 1.7178 0.9827 0.316 Uiso 0.5 1 calc R U P C -1
H51C H -0.2762 1.6266 1.0037 0.316 Uiso 0.5 1 calc R U P C -1
C52 C -0.149(2) 1.588(3) 0.958(2) 0.159(17) Uani 0.5 1 d . . P C -1
H52A H -0.1232 1.5902 0.8879 0.190 Uiso 0.5 1 calc R U P C -1
H52B H -0.1997 1.5203 0.9452 0.190 Uiso 0.5 1 calc R U P C -1
C53 C -0.028(2) 1.5397(14) 1.0052(14) 0.113(12) Uani 0.5 1 d . . P C -1
H53A H 0.0150 1.5958 1.0608 0.136 Uiso 0.5 1 calc R U P C -1
H53B H -0.0518 1.4782 1.0348 0.136 Uiso 0.5 1 calc R U P C -1
C54 C 0.0358(18) 1.5121(15) 0.9263(17) 0.117(7) Uani 0.5 1 d . . P C -1
H54A H 0.0663 1.5729 0.8981 0.140 Uiso 0.5 1 calc R U P C -1
H54B H -0.0036 1.4551 0.8696 0.140 Uiso 0.5 1 calc R U P C -1
C55 C 0.135(2) 1.4688(19) 0.994(3) 0.147(14) Uani 0.5 1 d . . P C -1
H55A H 0.1689 1.4115 0.9494 0.176 Uiso 0.5 1 calc R U P C -1
H55B H 0.1939 1.5268 1.0289 0.176 Uiso 0.5 1 calc R U P C -1
C56 C 0.082(3) 1.441(3) 1.048(2) 0.142(12) Uani 0.5 1 d . . P C -1
H56A H 0.1257 1.4138 1.0972 0.214 Uiso 0.5 1 calc R U P C -1
H56B H 0.0249 1.3838 1.0105 0.214 Uiso 0.5 1 calc R U P C -1
H56C H 0.0462 1.4987 1.0872 0.214 Uiso 0.5 1 calc R U P C -1


_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
Os O4 1.941(3) . ?
Os O3 1.951(3) . ?
Os N2 1.970(3) . ?
Os O1 1.972(2) . ?
Os N1 1.974(3) . ?
Os O2 1.978(2) . ?
O1 C11 1.330(4) . ?
N1 C12 1.385(4) . ?
N1 C31 1.431(4) . ?
O2 C21 1.336(4) . ?
N2 C22 1.382(4) . ?
N2 C41 1.430(4) . ?
O3 C1A 1.344(10) . ?
O3 C1B 1.406(14) . ?
O4 C2B 1.28(3) . ?
O4 C2A 1.45(2) . ?
C1A C2A 1.52(2) . ?
C1A H1A1 0.9900 . ?
C1A H1A2 0.9900 . ?
C2A H2A1 0.9900 . ?
C2A H2A2 0.9900 . ?
C1B C2B 1.49(3) . ?
C1B H1B1 0.9900 . ?
C1B H1B2 0.9900 . ?
C2B H2B1 0.9900 . ?
C2B H2B2 0.9900 . ?
C11 C12 1.408(5) . ?
C11 C16 1.416(5) . ?
C12 C13 1.413(5) . ?
C13 C14 1.380(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.418(5) . ?
C14 C18 1.537(5) . ?
C15 C16 1.374(5) . ?
C15 H15 0.9500 . ?
C16 C17 1.529(5) . ?
C17 C171 1.526(5) . ?
C17 C173 1.534(5) . ?
C17 C172 1.541(5) . ?
C18 C184 1.41(2) . ?
C18 C186 1.44(2) . ?
C18 C181 1.487(8) . ?
C18 C183 1.489(7) . ?
C18 C182 1.628(8) . ?
C18 C185 1.817(18) . ?
C21 C22 1.405(5) . ?
C21 C26 1.419(5) . ?
C22 C23 1.404(4) . ?
C23 C24 1.379(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.417(5) . ?
C24 C28 1.540(5) . ?
C25 C26 1.379(5) . ?
C25 H25 0.9500 . ?
C26 C27 1.534(5) . ?
C27 C272 1.530(5) . ?
C27 C271 1.536(5) . ?
C27 C273 1.540(5) . ?
C28 C282 1.519(6) . ?
C28 C281 1.520(6) . ?
C28 C283 1.521(6) . ?
C31 C32 1.383(5) . ?
C31 C36 1.386(5) . ?
C32 C33 1.389(5) . ?
C32 H32 0.9500 . ?
C33 C34 1.380(6) . ?
C33 H33 0.9500 . ?
C34 C35 1.377(6) . ?
C34 H34 0.9500 . ?
C35 C36 1.391(5) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C41 C42 1.379(6) . ?
C41 C46 1.391(6) . ?
C42 C43 1.393(6) . ?
C42 H42 0.9500 . ?
C43 C44 1.363(8) . ?
C43 H43 0.9500 . ?
C44 C45 1.364(8) . ?
C44 H44 0.9500 . ?
C45 C46 1.395(6) . ?
C45 H45 0.9500 . ?
C46 H46 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 . ?
C184 H18J 0.9800 . ?
C184 H18K 0.9800 . ?
C184 H18L 0.9800 . ?
C185 H18M 0.9800 . ?
C185 H18N 0.9800 . ?
C185 H18O 0.9800 . ?
C186 H18P 0.9800 . ?
C186 H18Q 0.9800 . ?
C186 H18R 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 C52 1.20(3) . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 C53 1.83(4) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 C54 1.33(3) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 C55 1.72(3) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C55 C56 1.08(4) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 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
O4 Os O3 79.59(12) . . ?
O4 Os N2 102.67(12) . . ?
O3 Os N2 96.37(12) . . ?
O4 Os O1 84.56(11) . . ?
O3 Os O1 164.09(11) . . ?
N2 Os O1 85.60(11) . . ?
O4 Os N1 97.05(12) . . ?
O3 Os N1 103.98(12) . . ?
N2 Os N1 153.86(12) . . ?
O1 Os N1 79.32(10) . . ?
O4 Os O2 163.59(10) . . ?
O3 Os O2 84.00(11) . . ?
N2 Os O2 79.34(10) . . ?
O1 Os O2 111.85(10) . . ?
N1 Os O2 86.58(10) . . ?
C11 O1 Os 114.5(2) . . ?
C12 N1 C31 119.9(3) . . ?
C12 N1 Os 114.0(2) . . ?
C31 N1 Os 124.1(2) . . ?
C21 O2 Os 113.9(2) . . ?
C22 N2 C41 119.4(3) . . ?
C22 N2 Os 114.5(2) . . ?
C41 N2 Os 124.5(2) . . ?
C1A O3 Os 117.0(4) . . ?
C1B O3 Os 112.6(5) . . ?
C2B O4 Os 120.5(12) . . ?
C2A O4 Os 113.6(8) . . ?
O3 C1A C2A 103.8(10) . . ?
O3 C1A H1A1 111.0 . . ?
C2A C1A H1A1 111.0 . . ?
O3 C1A H1A2 111.0 . . ?
C2A C1A H1A2 111.0 . . ?
H1A1 C1A H1A2 109.0 . . ?
O4 C2A C1A 107.1(13) . . ?
O4 C2A H2A1 110.3 . . ?
C1A C2A H2A1 110.3 . . ?
O4 C2A H2A2 110.3 . . ?
C1A C2A H2A2 110.3 . . ?
H2A1 C2A H2A2 108.5 . . ?
O3 C1B C2B 111.8(13) . . ?
O3 C1B H1B1 109.2 . . ?
C2B C1B H1B1 109.2 . . ?
O3 C1B H1B2 109.2 . . ?
C2B C1B H1B2 109.2 . . ?
H1B1 C1B H1B2 107.9 . . ?
O4 C2B C1B 107.6(18) . . ?
O4 C2B H2B1 110.2 . . ?
C1B C2B H2B1 110.2 . . ?
O4 C2B H2B2 110.2 . . ?
C1B C2B H2B2 110.2 . . ?
H2B1 C2B H2B2 108.5 . . ?
O1 C11 C12 115.1(3) . . ?
O1 C11 C16 123.8(3) . . ?
C12 C11 C16 121.0(3) . . ?
N1 C12 C11 113.1(3) . . ?
N1 C12 C13 126.2(3) . . ?
C11 C12 C13 120.7(3) . . ?
C14 C13 C12 119.0(3) . . ?
C14 C13 H13 120.5 . . ?
C12 C13 H13 120.5 . . ?
C13 C14 C15 118.5(3) . . ?
C13 C14 C18 122.3(3) . . ?
C15 C14 C18 119.3(3) . . ?
C16 C15 C14 124.8(3) . . ?
C16 C15 H15 117.6 . . ?
C14 C15 H15 117.6 . . ?
C15 C16 C11 115.9(3) . . ?
C15 C16 C17 122.9(3) . . ?
C11 C16 C17 121.2(3) . . ?
C171 C17 C16 111.8(3) . . ?
C171 C17 C173 107.6(3) . . ?
C16 C17 C173 111.1(3) . . ?
C171 C17 C172 108.5(3) . . ?
C16 C17 C172 108.1(3) . . ?
C173 C17 C172 109.6(3) . . ?
C184 C18 C186 124.7(12) . . ?
C181 C18 C183 111.5(5) . . ?
C184 C18 C14 111.9(8) . . ?
C186 C18 C14 114.1(8) . . ?
C181 C18 C14 110.9(4) . . ?
C183 C18 C14 113.6(4) . . ?
C181 C18 C182 108.1(5) . . ?
C183 C18 C182 106.0(5) . . ?
C14 C18 C182 106.3(4) . . ?
C184 C18 C185 103.6(12) . . ?
C186 C18 C185 97.2(12) . . ?
C14 C18 C185 99.8(6) . . ?
O2 C21 C22 115.3(3) . . ?
O2 C21 C26 123.3(3) . . ?
C22 C21 C26 121.3(3) . . ?
N2 C22 C23 126.6(3) . . ?
N2 C22 C21 112.9(3) . . ?
C23 C22 C21 120.5(3) . . ?
C24 C23 C22 119.6(3) . . ?
C24 C23 H23 120.2 . . ?
C22 C23 H23 120.2 . . ?
C23 C24 C25 118.3(3) . . ?
C23 C24 C28 122.4(3) . . ?
C25 C24 C28 119.2(3) . . ?
C26 C25 C24 124.7(3) . . ?
C26 C25 H25 117.7 . . ?
C24 C25 H25 117.7 . . ?
C25 C26 C21 115.5(3) . . ?
C25 C26 C27 123.4(3) . . ?
C21 C26 C27 121.1(3) . . ?
C272 C27 C26 111.1(3) . . ?
C272 C27 C271 108.1(3) . . ?
C26 C27 C271 111.4(3) . . ?
C272 C27 C273 109.9(3) . . ?
C26 C27 C273 108.4(3) . . ?
C271 C27 C273 108.0(3) . . ?
C282 C28 C281 108.5(4) . . ?
C282 C28 C283 108.7(4) . . ?
C281 C28 C283 108.8(4) . . ?
C282 C28 C24 111.9(3) . . ?
C281 C28 C24 109.2(3) . . ?
C283 C28 C24 109.7(3) . . ?
C32 C31 C36 120.5(3) . . ?
C32 C31 N1 120.1(3) . . ?
C36 C31 N1 119.3(3) . . ?
C31 C32 C33 119.4(4) . . ?
C31 C32 H32 120.3 . . ?
C33 C32 H32 120.3 . . ?
C34 C33 C32 120.5(4) . . ?
C34 C33 H33 119.8 . . ?
C32 C33 H33 119.8 . . ?
C35 C34 C33 119.9(4) . . ?
C35 C34 H34 120.1 . . ?
C33 C34 H34 120.1 . . ?
C34 C35 C36 120.3(4) . . ?
C34 C35 H35 119.8 . . ?
C36 C35 H35 119.8 . . ?
C31 C36 C35 119.4(4) . . ?
C31 C36 H36 120.3 . . ?
C35 C36 H36 120.3 . . ?
C42 C41 C46 119.9(4) . . ?
C42 C41 N2 119.0(4) . . ?
C46 C41 N2 121.1(4) . . ?
C41 C42 C43 120.2(5) . . ?
C41 C42 H42 119.9 . . ?
C43 C42 H42 119.9 . . ?
C44 C43 C42 120.0(5) . . ?
C44 C43 H43 120.0 . . ?
C42 C43 H43 120.0 . . ?
C43 C44 C45 120.2(4) . . ?
C43 C44 H44 119.9 . . ?
C45 C44 H44 119.9 . . ?
C44 C45 C46 121.1(5) . . ?
C44 C45 H45 119.4 . . ?
C46 C45 H45 119.4 . . ?
C41 C46 C45 118.6(5) . . ?
C41 C46 H46 120.7 . . ?
C45 C46 H46 120.7 . . ?
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 . . ?
C18 C184 H18J 109.5 . . ?
C18 C184 H18K 109.5 . . ?
H18J C184 H18K 109.5 . . ?
C18 C184 H18L 109.5 . . ?
H18J C184 H18L 109.5 . . ?
H18K C184 H18L 109.5 . . ?
C18 C185 H18M 109.5 . . ?
C18 C185 H18N 109.5 . . ?
H18M C185 H18N 109.5 . . ?
C18 C185 H18O 109.5 . . ?
H18M C185 H18O 109.5 . . ?
H18N C185 H18O 109.5 . . ?
C18 C186 H18P 109.5 . . ?
C18 C186 H18Q 109.5 . . ?
H18P C186 H18Q 109.5 . . ?
C18 C186 H18R 109.5 . . ?
H18P C186 H18R 109.5 . . ?
H18Q C186 H18R 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 . . ?
C52 C51 H51A 109.5 . . ?
C52 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C52 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C51 C52 C53 158(2) . . ?
C51 C52 H52A 96.8 . . ?
C53 C52 H52A 96.8 . . ?
C51 C52 H52B 96.8 . . ?
C53 C52 H52B 96.8 . . ?
H52A C52 H52B 103.5 . . ?
C54 C53 C52 109(2) . . ?
C54 C53 H53A 109.9 . . ?
C52 C53 H53A 109.9 . . ?
C54 C53 H53B 109.9 . . ?
C52 C53 H53B 109.9 . . ?
H53A C53 H53B 108.3 . . ?
C53 C54 C55 97(2) . . ?
C53 C54 H54A 112.3 . . ?
C55 C54 H54A 112.3 . . ?
C53 C54 H54B 112.3 . . ?
C55 C54 H54B 112.3 . . ?
H54A C54 H54B 109.9 . . ?
C56 C55 C54 97(3) . . ?
C56 C55 H55A 112.3 . . ?
C54 C55 H55A 112.3 . . ?
C56 C55 H55B 112.3 . . ?
C54 C55 H55B 112.3 . . ?
H55A C55 H55B 109.9 . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?

_refine_diff_density_max         1.537
_refine_diff_density_min         -2.931
_refine_diff_density_rms         0.124

_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_ospin
_database_code_depnum_ccdc_archive 'CCDC 2003366'
loop_
_audit_author_name
_audit_author_address
'Seth Brown' 'University of Notre Dame'
_audit_update_record             
;
2020-05-11 deposited with the CCDC.	2020-06-05 downloaded from the CCDC.
;

_vrf_PLAT094_ospin               
;
PROBLEM: Ratio of Maximum / Minimum Residual Density ....       4.55 Report
RESPONSE: There is a large peak of residual density near the Os atom,
possibly due to a small amount of whole-molecule disorder where the Os=O
unit is oriented 180 degrees from the major component.  Attempting to 
model this disorder resulted in less than 1% occupancy, so it was 
ignored in the final model.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
Oxo(pinacolato)(2-(phenylimido)-4,6-di-tert-butylphenoxo)-osmium(VI)
_chemical_name_common            (Hap)OsO(pin)
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H37 N O4 Os'
_chemical_formula_sum            'C26 H37 N O4 Os'
_chemical_formula_weight         617.76

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'
Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   10.1408(4)
_cell_length_b                   16.5112(6)
_cell_length_c                   15.0329(5)
_cell_angle_alpha                90
_cell_angle_beta                 96.6940(10)
_cell_angle_gamma                90
_cell_volume                     2499.90(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9992
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      30.54

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_F_000             1232
_exptl_transmission_factor_min   0.5578
_exptl_transmission_factor_max   0.7461
_exptl_crystal_size_max          0.322
_exptl_crystal_size_mid          0.295
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    5.132
_shelx_estimated_absorpt_T_min   0.289
_shelx_estimated_absorpt_T_max   0.578
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5578
_exptl_absorpt_correction_T_max  0.7461
_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 vapor diffusion of acetonitrile into a solution of the compound in chloroform.'


_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'
_diffrn_measurement_method       'ω and φ-scans'
_diffrn_detector_area_resol_mean 8.33
_diffrn_reflns_number            35684
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.839
_diffrn_reflns_theta_max         30.613
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             7245
_reflns_number_gt                6459
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_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)+(0.0180P)²+2.4639P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7245
_refine_ls_number_parameters     437
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0242
_refine_ls_R_factor_gt           0.0195
_refine_ls_wR_factor_ref         0.0436
_refine_ls_wR_factor_gt          0.0422
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.040
_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
Os Os 0.79508(2) 0.74225(2) 0.58819(2) 0.01179(3) Uani 1 1 d . . . . .
O O 0.76196(15) 0.77966(10) 0.68731(11) 0.0203(3) Uani 1 1 d . . . . .
O1 O 0.83683(14) 0.62958(9) 0.61678(10) 0.0142(3) Uani 1 1 d . . . . .
O3 O 0.77021(14) 0.82695(9) 0.50287(10) 0.0153(3) Uani 1 1 d . . . . .
O4 O 0.65529(14) 0.69480(9) 0.51169(10) 0.0150(3) Uani 1 1 d . . . . .
N1 N 0.98051(17) 0.74498(10) 0.57967(12) 0.0127(3) Uani 1 1 d . . . . .
C1 C 0.6363(2) 0.82894(13) 0.45563(14) 0.0150(4) Uani 1 1 d . . . . .
C2 C 0.6072(2) 0.74004(13) 0.43169(14) 0.0150(4) Uani 1 1 d . . . . .
C3 C 0.6405(3) 0.88325(16) 0.37514(18) 0.0233(5) Uani 1 1 d . . . . .
C4 C 0.5443(2) 0.86390(15) 0.51854(18) 0.0210(5) Uani 1 1 d . . . . .
C5 C 0.6853(3) 0.71055(16) 0.35786(17) 0.0236(5) Uani 1 1 d . . . . .
C6 C 0.4616(2) 0.71999(16) 0.40940(18) 0.0212(5) Uani 1 1 d . . . . .
C11 C 0.96873(19) 0.61266(12) 0.63067(14) 0.0120(4) Uani 1 1 d . . . . .
C12 C 1.05165(19) 0.67516(12) 0.61116(13) 0.0117(4) Uani 1 1 d . . . . .
C13 C 1.18859(19) 0.66735(12) 0.62383(13) 0.0116(4) Uani 1 1 d . . . . .
C14 C 1.24349(19) 0.59481(12) 0.65585(13) 0.0111(4) Uani 1 1 d . . . . .
C15 C 1.15784(19) 0.53149(12) 0.67188(13) 0.0118(4) Uani 1 1 d . . . . .
C16 C 1.01992(19) 0.53766(12) 0.66077(13) 0.0114(4) Uani 1 1 d . . . . .
C17 C 0.9284(2) 0.46830(12) 0.68037(15) 0.0137(4) Uani 1 1 d . . . . .
C18 C 1.39401(19) 0.58277(13) 0.67017(14) 0.0133(4) Uani 1 1 d . . . . .
C21 C 1.04868(19) 0.80700(12) 0.53642(14) 0.0129(4) Uani 1 1 d . . . . .
C22 C 1.1004(2) 0.79032(14) 0.45757(15) 0.0175(4) Uani 1 1 d . . . . .
C23 C 1.1652(2) 0.85013(15) 0.41576(16) 0.0204(5) Uani 1 1 d . . . . .
C24 C 1.1782(2) 0.92646(15) 0.45273(17) 0.0220(5) Uani 1 1 d . . . . .
C25 C 1.1261(3) 0.94287(15) 0.53110(18) 0.0268(5) Uani 1 1 d . . . . .
C26 C 1.0607(2) 0.88301(14) 0.57317(17) 0.0215(5) Uani 1 1 d . . . . .
C171 C 1.0059(2) 0.39346(14) 0.71562(19) 0.0220(5) Uani 1 1 d . . . . .
C172 C 0.8400(2) 0.49372(15) 0.75139(17) 0.0194(4) Uani 1 1 d . . . . .
C173 C 0.8419(2) 0.44516(15) 0.59384(17) 0.0219(5) Uani 1 1 d . . . . .
C181 C 1.4381(2) 0.54257(17) 0.58749(17) 0.0222(5) Uani 1 1 d . . . . .
C182 C 1.4351(2) 0.52875(16) 0.75088(17) 0.0215(5) Uani 1 1 d . . . . .
C183 C 1.4672(2) 0.66315(15) 0.68637(18) 0.0204(5) Uani 1 1 d . . . . .
H13 H 1.237(2) 0.7105(15) 0.6122(15) 0.009(5) Uiso 1 1 d . . . . .
H15 H 1.193(2) 0.4817(14) 0.6908(15) 0.007(5) Uiso 1 1 d . . . . .
H17A H 0.946(3) 0.3512(17) 0.7273(18) 0.027(7) Uiso 1 1 d . . . . .
H17B H 1.060(3) 0.3717(17) 0.6715(19) 0.026(7) Uiso 1 1 d . . . . .
H17C H 1.061(3) 0.4022(16) 0.7676(18) 0.018(7) Uiso 1 1 d . . . . .
H17D H 0.790(3) 0.5374(16) 0.7317(17) 0.020(7) Uiso 1 1 d . . . . .
H17E H 0.892(2) 0.5075(15) 0.8054(18) 0.017(6) Uiso 1 1 d . . . . .
H17F H 0.782(2) 0.4521(14) 0.7608(15) 0.009(6) Uiso 1 1 d . . . . .
H17G H 0.787(3) 0.4020(18) 0.6039(18) 0.024(7) Uiso 1 1 d . . . . .
H17H H 0.792(3) 0.4910(19) 0.5693(19) 0.029(8) Uiso 1 1 d . . . . .
H17I H 0.897(3) 0.4292(17) 0.5509(19) 0.026(7) Uiso 1 1 d . . . . .
H18A H 1.525(3) 0.5346(18) 0.596(2) 0.034(8) Uiso 1 1 d . . . . .
H18B H 1.419(3) 0.5744(18) 0.539(2) 0.029(8) Uiso 1 1 d . . . . .
H18C H 1.399(3) 0.4902(17) 0.5772(18) 0.022(7) Uiso 1 1 d . . . . .
H18D H 1.408(3) 0.5548(18) 0.807(2) 0.033(8) Uiso 1 1 d . . . . .
H18E H 1.524(3) 0.5266(16) 0.7600(17) 0.021(7) Uiso 1 1 d . . . . .
H18F H 1.398(3) 0.4784(17) 0.7474(18) 0.024(7) Uiso 1 1 d . . . . .
H18G H 1.560(3) 0.6540(15) 0.6988(17) 0.019(6) Uiso 1 1 d . . . . .
H18H H 1.435(3) 0.6916(18) 0.736(2) 0.031(8) Uiso 1 1 d . . . . .
H18I H 1.456(2) 0.6980(17) 0.6341(18) 0.021(7) Uiso 1 1 d . . . . .
H22 H 1.095(3) 0.7398(16) 0.4332(19) 0.023(7) Uiso 1 1 d . . . . .
H23 H 1.195(3) 0.8382(16) 0.3603(18) 0.022(7) Uiso 1 1 d . . . . .
H24 H 1.223(3) 0.9677(18) 0.4273(18) 0.026(7) Uiso 1 1 d . . . . .
H25 H 1.135(3) 0.9946(18) 0.5574(18) 0.027(7) Uiso 1 1 d . . . . .
H26 H 1.026(3) 0.8946(17) 0.6239(19) 0.027(7) Uiso 1 1 d . . . . .
H3A H 0.648(3) 0.9364(17) 0.3945(17) 0.020(7) Uiso 1 1 d . . . . .
H3B H 0.562(3) 0.8814(18) 0.3394(19) 0.032(8) Uiso 1 1 d . . . . .
H3C H 0.712(3) 0.8692(16) 0.3404(18) 0.022(7) Uiso 1 1 d . . . . .
H4A H 0.576(3) 0.9126(18) 0.5431(18) 0.026(7) Uiso 1 1 d . . . . .
H4B H 0.532(3) 0.8286(16) 0.5677(18) 0.021(7) Uiso 1 1 d . . . . .
H4C H 0.466(3) 0.8723(17) 0.4902(19) 0.028(8) Uiso 1 1 d . . . . .
H5A H 0.683(3) 0.6516(19) 0.3549(19) 0.032(8) Uiso 1 1 d . . . . .
H5B H 0.647(3) 0.7334(17) 0.297(2) 0.030(8) Uiso 1 1 d . . . . .
H5C H 0.778(3) 0.7230(19) 0.367(2) 0.034(8) Uiso 1 1 d . . . . .
H6A H 0.454(3) 0.6650(18) 0.3955(18) 0.025(7) Uiso 1 1 d . . . . .
H6B H 0.424(3) 0.7483(17) 0.357(2) 0.033(9) Uiso 1 1 d . . . . .
H6C H 0.415(3) 0.7309(17) 0.457(2) 0.025(7) 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
Os O 1.6825(16) . ?
Os O4 1.8884(14) . ?
Os O3 1.8945(14) . ?
Os N1 1.9002(17) . ?
Os O1 1.9448(14) . ?
O1 C11 1.359(2) . ?
O3 C1 1.457(2) . ?
O4 C2 1.451(2) . ?
N1 C12 1.412(2) . ?
N1 C21 1.433(3) . ?
C1 C3 1.511(3) . ?
C1 C4 1.518(3) . ?
C1 C2 1.532(3) . ?
C2 C6 1.513(3) . ?
C2 C5 1.517(3) . ?
C3 H3A 0.92(3) . ?
C3 H3B 0.91(3) . ?
C3 H3C 0.97(3) . ?
C4 H4A 0.93(3) . ?
C4 H4B 0.96(3) . ?
C4 H4C 0.87(3) . ?
C5 H5A 0.97(3) . ?
C5 H5B 1.02(3) . ?
C5 H5C 0.96(3) . ?
C6 H6A 0.93(3) . ?
C6 H6B 0.95(3) . ?
C6 H6C 0.92(3) . ?
C11 C12 1.384(3) . ?
C11 C16 1.397(3) . ?
C12 C13 1.386(3) . ?
C13 C14 1.383(3) . ?
C13 H13 0.90(2) . ?
C14 C15 1.398(3) . ?
C14 C18 1.529(3) . ?
C15 C16 1.393(3) . ?
C15 H15 0.93(2) . ?
C16 C17 1.524(3) . ?
C17 C171 1.526(3) . ?
C17 C173 1.530(3) . ?
C17 C172 1.530(3) . ?
C18 C181 1.522(3) . ?
C18 C182 1.524(3) . ?
C18 C183 1.526(3) . ?
C21 C26 1.371(3) . ?
C21 C22 1.379(3) . ?
C22 C23 1.378(3) . ?
C22 H22 0.91(3) . ?
C23 C24 1.377(3) . ?
C23 H23 0.94(3) . ?
C24 C25 1.374(4) . ?
C24 H24 0.92(3) . ?
C25 C26 1.383(3) . ?
C25 H25 0.94(3) . ?
C26 H26 0.90(3) . ?
C171 H17A 0.95(3) . ?
C171 H17B 0.97(3) . ?
C171 H17C 0.92(3) . ?
C172 H17D 0.91(3) . ?
C172 H17E 0.94(3) . ?
C172 H17F 0.93(2) . ?
C173 H17G 0.93(3) . ?
C173 H17H 0.96(3) . ?
C173 H17I 0.94(3) . ?
C181 H18A 0.89(3) . ?
C181 H18B 0.90(3) . ?
C181 H18C 0.95(3) . ?
C182 H18D 1.02(3) . ?
C182 H18E 0.90(3) . ?
C182 H18F 0.91(3) . ?
C183 H18G 0.95(3) . ?
C183 H18H 0.97(3) . ?
C183 H18I 0.97(3) . ?

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
O Os O4 118.59(7) . . ?
O Os O3 107.70(7) . . ?
O4 Os O3 82.11(6) . . ?
O Os N1 110.63(8) . . ?
O4 Os N1 130.34(7) . . ?
O3 Os N1 89.51(7) . . ?
O Os O1 102.49(7) . . ?
O4 Os O1 82.32(6) . . ?
O3 Os O1 149.78(7) . . ?
N1 Os O1 81.14(6) . . ?
C11 O1 Os 114.56(12) . . ?
C1 O3 Os 112.92(12) . . ?
C2 O4 Os 116.56(12) . . ?
C12 N1 C21 118.74(16) . . ?
C12 N1 Os 115.40(13) . . ?
C21 N1 Os 125.52(13) . . ?
O3 C1 C3 106.98(17) . . ?
O3 C1 C4 108.10(18) . . ?
C3 C1 C4 110.49(19) . . ?
O3 C1 C2 103.65(16) . . ?
C3 C1 C2 113.78(19) . . ?
C4 C1 C2 113.26(18) . . ?
O4 C2 C6 107.22(17) . . ?
O4 C2 C5 106.71(18) . . ?
C6 C2 C5 110.3(2) . . ?
O4 C2 C1 105.16(16) . . ?
C6 C2 C1 114.73(18) . . ?
C5 C2 C1 112.12(18) . . ?
C1 C3 H3A 108.7(16) . . ?
C1 C3 H3B 110.5(18) . . ?
H3A C3 H3B 105(2) . . ?
C1 C3 H3C 112.5(16) . . ?
H3A C3 H3C 111(2) . . ?
H3B C3 H3C 109(2) . . ?
C1 C4 H4A 111.4(17) . . ?
C1 C4 H4B 113.1(16) . . ?
H4A C4 H4B 107(2) . . ?
C1 C4 H4C 110.4(19) . . ?
H4A C4 H4C 108(2) . . ?
H4B C4 H4C 106(2) . . ?
C2 C5 H5A 109.9(17) . . ?
C2 C5 H5B 111.2(17) . . ?
H5A C5 H5B 109(2) . . ?
C2 C5 H5C 114.8(18) . . ?
H5A C5 H5C 104(2) . . ?
H5B C5 H5C 108(2) . . ?
C2 C6 H6A 108.2(17) . . ?
C2 C6 H6B 111.0(19) . . ?
H6A C6 H6B 106(2) . . ?
C2 C6 H6C 111.3(18) . . ?
H6A C6 H6C 109(2) . . ?
H6B C6 H6C 111(3) . . ?
O1 C11 C12 115.20(18) . . ?
O1 C11 C16 123.63(18) . . ?
C12 C11 C16 121.16(18) . . ?
C11 C12 C13 121.71(18) . . ?
C11 C12 N1 112.36(17) . . ?
C13 C12 N1 125.92(18) . . ?
C14 C13 C12 118.99(18) . . ?
C14 C13 H13 123.3(15) . . ?
C12 C13 H13 117.6(15) . . ?
C13 C14 C15 118.33(18) . . ?
C13 C14 C18 121.07(18) . . ?
C15 C14 C18 120.56(18) . . ?
C16 C15 C14 124.06(19) . . ?
C16 C15 H15 116.4(14) . . ?
C14 C15 H15 119.5(14) . . ?
C15 C16 C11 115.69(18) . . ?
C15 C16 C17 123.19(18) . . ?
C11 C16 C17 121.12(17) . . ?
C16 C17 C171 112.03(17) . . ?
C16 C17 C173 108.96(18) . . ?
C171 C17 C173 108.30(19) . . ?
C16 C17 C172 110.38(17) . . ?
C171 C17 C172 107.43(19) . . ?
C173 C17 C172 109.71(18) . . ?
C181 C18 C182 108.4(2) . . ?
C181 C18 C183 109.02(19) . . ?
C182 C18 C183 107.40(19) . . ?
C181 C18 C14 108.98(17) . . ?
C182 C18 C14 111.33(17) . . ?
C183 C18 C14 111.61(17) . . ?
C26 C21 C22 120.3(2) . . ?
C26 C21 N1 119.75(19) . . ?
C22 C21 N1 119.95(19) . . ?
C23 C22 C21 119.9(2) . . ?
C23 C22 H22 119.0(18) . . ?
C21 C22 H22 121.1(18) . . ?
C22 C23 C24 120.0(2) . . ?
C22 C23 H23 118.3(16) . . ?
C24 C23 H23 121.6(16) . . ?
C25 C24 C23 119.9(2) . . ?
C25 C24 H24 117.7(18) . . ?
C23 C24 H24 122.4(18) . . ?
C24 C25 C26 120.3(2) . . ?
C24 C25 H25 120.9(17) . . ?
C26 C25 H25 118.8(17) . . ?
C21 C26 C25 119.6(2) . . ?
C21 C26 H26 120.8(18) . . ?
C25 C26 H26 119.5(18) . . ?
C17 C171 H17A 110.0(17) . . ?
C17 C171 H17B 111.6(16) . . ?
H17A C171 H17B 106(2) . . ?
C17 C171 H17C 114.1(16) . . ?
H17A C171 H17C 107(2) . . ?
H17B C171 H17C 108(2) . . ?
C17 C172 H17D 110.0(16) . . ?
C17 C172 H17E 110.5(15) . . ?
H17D C172 H17E 109(2) . . ?
C17 C172 H17F 109.7(15) . . ?
H17D C172 H17F 107(2) . . ?
H17E C172 H17F 111(2) . . ?
C17 C173 H17G 110.5(17) . . ?
C17 C173 H17H 110.8(17) . . ?
H17G C173 H17H 111(2) . . ?
C17 C173 H17I 109.2(17) . . ?
H17G C173 H17I 108(2) . . ?
H17H C173 H17I 107(2) . . ?
C18 C181 H18A 109.1(19) . . ?
C18 C181 H18B 110.3(19) . . ?
H18A C181 H18B 109(3) . . ?
C18 C181 H18C 112.0(16) . . ?
H18A C181 H18C 106(2) . . ?
H18B C181 H18C 111(2) . . ?
C18 C182 H18D 109.9(17) . . ?
C18 C182 H18E 108.7(17) . . ?
H18D C182 H18E 105(2) . . ?
C18 C182 H18F 114.5(17) . . ?
H18D C182 H18F 106(2) . . ?
H18E C182 H18F 112(2) . . ?
C18 C183 H18G 110.2(15) . . ?
C18 C183 H18H 110.2(17) . . ?
H18G C183 H18H 110(2) . . ?
C18 C183 H18I 112.1(16) . . ?
H18G C183 H18I 106(2) . . ?
H18H C183 H18I 108(2) . . ?

_refine_diff_density_max         2.848
_refine_diff_density_min         -0.626
_refine_diff_density_rms         0.097

_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_an2eg
_database_code_depnum_ccdc_archive 'CCDC 2003367'
loop_
_audit_author_name
_audit_author_address
'Seth Brown' 'University of Notre Dame'
_audit_update_record             
;
2020-05-11 deposited with the CCDC.	2020-06-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
; 
 1,2-Ethanediyldi-2-aminobenzoate 
;
_chemical_name_common            'Ethylene glycol dianthranilate'
_chemical_melting_point          375
_chemical_formula_moiety         'C16 H16 N2 O4'
_chemical_formula_sum            'C16 H16 N2 O4'
_chemical_formula_weight         300.31

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           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   13.142(3)
_cell_length_b                   11.273(3)
_cell_length_c                   9.569(2)
_cell_angle_alpha                90
_cell_angle_beta                 102.307(5)
_cell_angle_gamma                90
_cell_volume                     1385.1(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    1894
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      26.94

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_F_000             632
_exptl_transmission_factor_min   0.8830
_exptl_transmission_factor_max   1.0000
_exptl_crystal_size_max          0.223
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.116
_exptl_absorpt_coefficient_mu    0.105
_shelx_estimated_absorpt_T_min   0.977
_shelx_estimated_absorpt_T_max   0.988
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.8830
_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_special_details           
; 
 ? 
;

_exptl_crystal_recrystallization_method 
;
Crystals were deposited from methanol.
;


_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            10143
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.404
_diffrn_reflns_theta_max         28.308
_diffrn_reflns_theta_full        25.242
_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             1736
_reflns_number_gt                1266
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker 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)+(0.0548P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   direct
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1736
_refine_ls_number_parameters     132
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0385
_refine_ls_wR_factor_ref         0.1035
_refine_ls_wR_factor_gt          0.0951
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_restrained_S_all      1.074
_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 0.06421(7) 0.62549(8) 0.08420(10) 0.0250(3) Uani 1 1 d . . . . .
O2 O 0.08504(7) 0.82098(8) 0.12143(9) 0.0235(3) Uani 1 1 d . . . . .
N1 N 0.11986(10) 0.53484(10) -0.15132(14) 0.0273(3) Uani 1 1 d . . . . .
H1A H 0.0843(11) 0.5209(14) -0.0835(17) 0.038(5) Uiso 1 1 d . . . . .
H1B H 0.1126(13) 0.4859(16) -0.2233(19) 0.042(5) Uiso 1 1 d . . . . .
C10 C 0.05819(11) 0.80609(13) 0.25892(14) 0.0234(3) Uani 1 1 d . . . . .
H10A H 0.0893(11) 0.7318(14) 0.3042(15) 0.023(4) Uiso 1 1 d . . . . .
H10B H 0.0880(10) 0.8738(13) 0.3151(15) 0.022(4) Uiso 1 1 d . . . . .
C11 C 0.11926(10) 0.74599(11) -0.09219(13) 0.0186(3) Uani 1 1 d . . . . .
C12 C 0.13167(9) 0.65124(12) -0.18428(14) 0.0202(3) Uani 1 1 d . . . . .
C13 C 0.16136(10) 0.67990(12) -0.31350(14) 0.0229(3) Uani 1 1 d . . . . .
H13 H 0.1685(10) 0.6175(13) -0.3778(15) 0.026(4) Uiso 1 1 d . . . . .
C14 C 0.17758(10) 0.79536(12) -0.34833(14) 0.0239(3) Uani 1 1 d . . . . .
H14 H 0.1984(11) 0.8121(12) -0.4385(17) 0.029(4) Uiso 1 1 d . . . . .
C15 C 0.16553(11) 0.88840(12) -0.25769(15) 0.0249(3) Uani 1 1 d . . . . .
H15 H 0.1780(11) 0.9684(14) -0.2807(16) 0.033(4) Uiso 1 1 d . . . . .
C16 C 0.13675(10) 0.86262(12) -0.13109(14) 0.0226(3) Uani 1 1 d . . . . .
H16 H 0.1296(11) 0.9270(13) -0.0653(15) 0.026(4) Uiso 1 1 d . . . . .
C17 C 0.08733(10) 0.72197(11) 0.04320(14) 0.0190(3) Uani 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 C17 1.2165(15) . ?
O2 C17 1.3479(15) . ?
O2 C10 1.4428(15) . ?
N1 C12 1.3661(18) . ?
N1 H1A 0.891(15) . ?
N1 H1B 0.871(19) . ?
C10 C10 1.502(3) 2 ?
C10 H10A 0.990(15) . ?
C10 H10B 0.967(15) . ?
C11 C16 1.3987(18) . ?
C11 C12 1.4161(18) . ?
C11 C17 1.4696(18) . ?
C12 C13 1.4112(19) . ?
C13 C14 1.3714(19) . ?
C13 H13 0.952(15) . ?
C14 C15 1.3914(19) . ?
C14 H14 0.978(15) . ?
C15 C16 1.3749(18) . ?
C15 H15 0.950(16) . ?
C16 H16 0.979(15) . ?

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
C17 O2 C10 116.67(10) . . ?
C12 N1 H1A 116.1(11) . . ?
C12 N1 H1B 115.1(11) . . ?
H1A N1 H1B 118.6(15) . . ?
O2 C10 C10 109.72(14) . 2 ?
O2 C10 H10A 109.8(8) . . ?
C10 C10 H10A 111.4(8) 2 . ?
O2 C10 H10B 105.5(8) . . ?
C10 C10 H10B 110.2(8) 2 . ?
H10A C10 H10B 110.1(12) . . ?
C16 C11 C12 119.74(12) . . ?
C16 C11 C17 120.12(11) . . ?
C12 C11 C17 120.14(11) . . ?
N1 C12 C13 119.24(12) . . ?
N1 C12 C11 123.16(13) . . ?
C13 C12 C11 117.56(12) . . ?
C14 C13 C12 121.11(12) . . ?
C14 C13 H13 120.2(9) . . ?
C12 C13 H13 118.7(9) . . ?
C13 C14 C15 121.30(13) . . ?
C13 C14 H14 119.0(8) . . ?
C15 C14 H14 119.7(8) . . ?
C16 C15 C14 118.63(13) . . ?
C16 C15 H15 119.9(9) . . ?
C14 C15 H15 121.5(9) . . ?
C15 C16 C11 121.66(12) . . ?
C15 C16 H16 119.5(8) . . ?
C11 C16 H16 118.8(8) . . ?
O1 C17 O2 121.63(11) . . ?
O1 C17 C11 125.94(11) . . ?
O2 C17 C11 112.42(10) . . ?

_refine_diff_density_max         0.267
_refine_diff_density_min         -0.219
_refine_diff_density_rms         0.045

_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_Final
_database_code_depnum_ccdc_archive 'CCDC 2003365'
loop_
_audit_author_name
_audit_author_address
'Seth Brown' 'University of Notre Dame'
_audit_update_record             
;
2020-05-11 deposited with the CCDC.	2020-06-05 downloaded from the CCDC.
;

_vrf_PLAT213_Final               
;
RESPONSE:C23 and C24 show elongated thermal ellipsoids, possibly due to 
unresolved disorder in the phenyl group.
;
_vrf_PLAT391_Final               
;
RESPONSE:C171 C173 C181 and C182 belong to tert butyl groups in which the 
hydrogen atoms have been allowed to refine freely.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        
'Cis-bis-(2-(phenylimido)-4,6-di-tert-butylphenoxo)dichloroosmium(VI) chloroform solvate'
_chemical_name_common            
;
Os(Phap)₂Cl₂ . CDCl₃
;
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H50 Cl2 N2 O2 Os, C D Cl3'
_chemical_formula_sum            'C41 H50 D Cl5 N2 O2 Os'
_chemical_formula_weight         972.29

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
D D 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_H-M_alt        'F d d 2'
_space_group_name_Hall           'F 2 -2d'

_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+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'

_cell_length_a                   16.8082(7)
_cell_length_b                   40.829(2)
_cell_length_c                   12.5096(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8584.8(8)
_cell_formula_units_Z            8
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9955
_cell_measurement_theta_min      2.521
_cell_measurement_theta_max      28.2465

_exptl_crystal_description       Square
_exptl_crystal_colour            Black
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_F_000             3904
_exptl_transmission_factor_min   0.664400
_exptl_transmission_factor_max   0.745700
_exptl_crystal_size_max          0.229
_exptl_crystal_size_mid          0.202
_exptl_crystal_size_min          0.186
_exptl_absorpt_coefficient_mu    3.317
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.664400
_exptl_absorpt_correction_T_max  0.745700
_exptl_absorpt_process_details   
;
L. Krause, R. Herbst-Irmer, G. M. Sheldrick & D. Stalke. J. Appl.
Cryst., 2015, 48, 3.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_recrystallization_method 
'Crystals were deposited from a solution of the material dissolvedin CDCl3.'
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Kappa X8-APEX-II'
_diffrn_measurement_method       'combination of ω and φ-scans '
_diffrn_detector_area_resol_mean 8.33
_diffrn_reflns_number            33267
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -54
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.995
_diffrn_reflns_theta_max         28.244
_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 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             5294
_reflns_number_gt                5033
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.910
_reflns_Friedel_fraction_max     0.995
_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 APEX-3 (Bruker, 2015)'
_computing_cell_refinement       'Bruker SAINT (Bruker, 2015)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2015)'
_computing_structure_solution    'SHELXT-2014/2 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_molecular_graphics    'Bruker XP (Bruker, 2015)'
_computing_publication_material  'CIFTAB (Sheldrick, 2008)'
_refine_special_details          
;
Hydrogen atoms were found on the main molecule and solvent molecule
except for on the N-Phenyl ring (H23,H24 and H25). This was due to 
slight disorder in the phenyl ring that was not modeled. Hydrogens 
on C172 (H17D, H17E, H17F) were placed in 
calculated positions. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0066P)²+7.1970P] 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 2331 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.007(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5294
_refine_ls_number_parameters     329
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0156
_refine_ls_R_factor_gt           0.0140
_refine_ls_wR_factor_ref         0.0327
_refine_ls_wR_factor_gt          0.0322
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.047
_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
Os Os 0.500000 0.500000 0.85075(2) 0.01625(4) Uani 1 2 d S T P . .
O1 O 0.57666(10) 0.46229(4) 0.85050(17) 0.0198(4) Uani 1 1 d . . . . .
N1 N 0.45027(13) 0.47078(6) 0.74592(18) 0.0181(4) Uani 1 1 d . . . . .
Cl1 Cl 0.43031(4) 0.47096(2) 0.98462(6) 0.02747(15) Uani 1 1 d . . . . .
C11 C 0.54629(16) 0.43531(7) 0.8129(2) 0.0201(5) Uani 1 1 d . . . . .
C12 C 0.47508(16) 0.43923(7) 0.7505(2) 0.0205(5) Uani 1 1 d . . . . .
C13 C 0.43838(17) 0.41183(7) 0.7011(2) 0.0232(6) Uani 1 1 d . . . . .
H13 H 0.392(2) 0.4152(8) 0.658(3) 0.014(8) Uiso 1 1 d . . . . .
C14 C 0.47012(18) 0.38161(8) 0.7147(3) 0.0266(6) Uani 1 1 d . . . . .
C15 C 0.54157(18) 0.37825(8) 0.7776(3) 0.0284(7) Uani 1 1 d . . . . .
H15 H 0.5616(19) 0.3569(8) 0.784(3) 0.022(8) Uiso 1 1 d . . . . .
C16 C 0.58082(17) 0.40358(7) 0.8259(2) 0.0243(6) Uani 1 1 d . . . . .
C17 C 0.65755(18) 0.39917(8) 0.8908(3) 0.0297(7) Uani 1 1 d . . . . .
C171 C 0.7257(3) 0.41748(11) 0.8345(4) 0.0374(10) Uani 1 1 d . . . . .
H17A H 0.715(3) 0.4413(11) 0.824(4) 0.047(12) Uiso 1 1 d . . . . .
H17B H 0.734(3) 0.4116(13) 0.766(4) 0.059(15) Uiso 1 1 d . . . . .
H17C H 0.773(3) 0.4139(13) 0.878(5) 0.051(16) Uiso 1 1 d . . . . .
C172 C 0.6461(2) 0.41251(9) 1.0048(3) 0.0344(8) Uani 1 1 d . . . . .
H17D H 0.695415 0.409578 1.045523 0.052 Uiso 1 1 calc R U . . .
H17E H 0.632844 0.435858 1.001470 0.052 Uiso 1 1 calc R U . . .
H17F H 0.602838 0.400581 1.039989 0.052 Uiso 1 1 calc R U . . .
C173 C 0.6796(3) 0.36276(10) 0.8994(4) 0.0433(10) Uani 1 1 d . . . . .
H17G H 0.723(3) 0.3613(11) 0.938(3) 0.043(11) Uiso 1 1 d . . . . .
H17H H 0.690(2) 0.3539(10) 0.833(3) 0.037(11) Uiso 1 1 d . . . . .
H17I H 0.642(3) 0.3506(11) 0.946(4) 0.043(12) Uiso 1 1 d . . . . .
C18 C 0.4313(2) 0.35054(8) 0.6697(3) 0.0339(8) Uani 1 1 d . . . . .
C181 C 0.3986(3) 0.33025(10) 0.7625(4) 0.0474(10) Uani 1 1 d . . . . .
H18A H 0.374(2) 0.3093(11) 0.732(3) 0.050(11) Uiso 1 1 d . . . . .
H18B H 0.361(3) 0.3427(11) 0.804(3) 0.042(12) Uiso 1 1 d . . . . .
H18C H 0.436(3) 0.3232(11) 0.813(4) 0.052(13) Uiso 1 1 d . . . . .
C182 C 0.3626(3) 0.35913(9) 0.5943(5) 0.0495(11) Uani 1 1 d . . . . .
H18D H 0.318(3) 0.3683(10) 0.640(3) 0.038(11) Uiso 1 1 d . . . . .
H18E H 0.334(3) 0.3403(12) 0.571(4) 0.057(13) Uiso 1 1 d . . . . .
H18F H 0.385(3) 0.3722(12) 0.542(4) 0.059(15) Uiso 1 1 d . . . . .
C183 C 0.4921(3) 0.33069(14) 0.6066(6) 0.0491(14) Uani 1 1 d . . . . .
H18G H 0.467(3) 0.3122(12) 0.574(4) 0.052(13) Uiso 1 1 d . . . . .
H18H H 0.512(3) 0.3420(14) 0.552(5) 0.053(17) Uiso 1 1 d . . . . .
H18I H 0.535(3) 0.3229(13) 0.647(4) 0.057(17) Uiso 1 1 d . . . . .
C21 C 0.38914(18) 0.47964(7) 0.6713(2) 0.0241(6) Uani 1 1 d . . . . .
C22 C 0.3203(2) 0.49395(9) 0.7102(4) 0.0403(9) Uani 1 1 d . . . . .
H22 H 0.315(3) 0.4997(9) 0.784(4) 0.048(13) Uiso 1 1 d . . . . .
C23 C 0.2594(4) 0.50191(16) 0.6416(10) 0.074(3) Uani 1 1 d . . . . .
H23 H 0.211775 0.511331 0.668517 0.089 Uiso 1 1 calc R U . . .
C24 C 0.2677(5) 0.49620(17) 0.5344(9) 0.083(3) Uani 1 1 d . . . . .
H24 H 0.225464 0.501426 0.486944 0.100 Uiso 1 1 calc R U . . .
C25 C 0.3371(3) 0.48290(13) 0.4948(4) 0.0685(16) Uani 1 1 d . . . . .
H25 H 0.342856 0.479528 0.420102 0.082 Uiso 1 1 calc R U . . .
C26 C 0.3988(2) 0.47437(11) 0.5638(3) 0.0415(9) Uani 1 1 d . . . . .
H26 H 0.440(2) 0.4672(10) 0.529(3) 0.042(12) Uiso 1 1 d . . . . .
C91 C 0.4979(5) 0.49032(16) 0.2241(5) 0.0346(17) Uani 0.5 1 d . . P A -1
D91 D 0.483(4) 0.4901(17) 0.149(6) 0.026(19) Uiso 0.5 1 d . . P B -1
Cl91 Cl 0.43942(13) 0.45905(5) 0.27800(17) 0.0497(5) Uani 0.5 1 d . . P A -1
Cl92 Cl 0.59823(12) 0.47982(5) 0.23672(18) 0.0506(5) Uani 0.5 1 d . . P A -1
Cl93 Cl 0.47770(16) 0.52787(5) 0.2865(2) 0.0602(6) Uani 0.5 1 d . . P A -1


_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
Os N1 1.960(2) . ?
Os N1 1.960(2) 2_665 ?
Os O1 2.0076(17) . ?
Os O1 2.0077(17) 2_665 ?
Os Cl1 2.3626(7) . ?
Os Cl1 2.3626(7) 2_665 ?
O1 C11 1.302(3) . ?
N1 C12 1.355(4) . ?
N1 C21 1.434(4) . ?
C11 C16 1.429(4) . ?
C11 C12 1.438(4) . ?
C12 C13 1.419(4) . ?
C13 C14 1.355(4) . ?
C14 C15 1.442(4) . ?
C14 C18 1.534(4) . ?
C15 C16 1.367(4) . ?
C16 C17 1.534(4) . ?
C17 C173 1.536(5) . ?
C17 C171 1.538(6) . ?
C17 C172 1.539(5) . ?
C18 C183 1.524(6) . ?
C18 C181 1.529(6) . ?
C18 C182 1.531(5) . ?
C21 C26 1.371(5) . ?
C21 C22 1.384(5) . ?
C22 C23 1.374(9) . ?
C23 C24 1.369(11) . ?
C24 C25 1.377(11) . ?
C25 C26 1.394(6) . ?
C91 Cl91 1.746(8) . ?
C91 Cl92 1.747(8) . ?
C91 Cl93 1.753(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Os N1 96.01(13) . 2_665 ?
N1 Os O1 78.81(9) . . ?
N1 Os O1 101.07(9) 2_665 . ?
N1 Os O1 101.07(9) . 2_665 ?
N1 Os O1 78.80(9) 2_665 2_665 ?
O1 Os O1 179.82(12) . 2_665 ?
N1 Os Cl1 87.56(7) . . ?
N1 Os Cl1 172.34(7) 2_665 . ?
O1 Os Cl1 86.24(6) . . ?
O1 Os Cl1 93.88(6) 2_665 . ?
N1 Os Cl1 172.35(7) . 2_665 ?
N1 Os Cl1 87.56(7) 2_665 2_665 ?
O1 Os Cl1 93.88(6) . 2_665 ?
O1 Os Cl1 86.24(6) 2_665 2_665 ?
Cl1 Os Cl1 89.72(4) . 2_665 ?
C11 O1 Os 113.45(16) . . ?
C12 N1 C21 119.2(2) . . ?
C12 N1 Os 114.77(18) . . ?
C21 N1 Os 125.97(19) . . ?
O1 C11 C16 124.5(2) . . ?
O1 C11 C12 115.3(2) . . ?
C16 C11 C12 120.0(2) . . ?
N1 C12 C13 126.7(3) . . ?
N1 C12 C11 112.6(2) . . ?
C13 C12 C11 120.7(3) . . ?
C14 C13 C12 119.5(3) . . ?
C13 C14 C15 118.9(3) . . ?
C13 C14 C18 122.7(3) . . ?
C15 C14 C18 118.4(3) . . ?
C16 C15 C14 124.8(3) . . ?
C15 C16 C11 116.1(3) . . ?
C15 C16 C17 123.4(3) . . ?
C11 C16 C17 120.5(3) . . ?
C16 C17 C173 110.7(3) . . ?
C16 C17 C171 109.0(3) . . ?
C173 C17 C171 108.8(3) . . ?
C16 C17 C172 110.1(3) . . ?
C173 C17 C172 107.9(3) . . ?
C171 C17 C172 110.2(3) . . ?
C183 C18 C181 110.3(4) . . ?
C183 C18 C182 108.0(4) . . ?
C181 C18 C182 108.7(3) . . ?
C183 C18 C14 110.2(3) . . ?
C181 C18 C14 108.8(3) . . ?
C182 C18 C14 110.9(3) . . ?
C26 C21 C22 120.6(3) . . ?
C26 C21 N1 120.9(3) . . ?
C22 C21 N1 118.5(3) . . ?
C23 C22 C21 120.2(6) . . ?
C24 C23 C22 119.7(7) . . ?
C23 C24 C25 120.4(5) . . ?
C24 C25 C26 120.4(5) . . ?
C21 C26 C25 118.6(5) . . ?
Cl91 C91 Cl92 109.2(4) . . ?
Cl91 C91 Cl93 111.0(4) . . ?
Cl92 C91 Cl93 111.2(4) . . ?

_refine_diff_density_max         0.482
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.052

####################################################################### 
# 
# 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_Final_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2003364'
loop_
_audit_author_name
_audit_author_address
'Seth Brown' 'University of Notre Dame'
_audit_update_record             
;
2020-05-11 deposited with the CCDC.	2020-06-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        
'Cis-bis-(2-(phenylimido)-4,6-di-tert-butylphenoxo)dichloroosmium(VI) deuterodichloromethane solvate'
_chemical_name_common            
;
Os(Phap)₂Cl₂ . CD₂Cl₂
;
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H50 Cl2 N2 O2 Os, C D2 Cl2'
_chemical_formula_sum            'C41 H50 D2 Cl4 N2 O2 Os'
_chemical_formula_weight         938.86

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
D D 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_H-M_alt        'F d d 2'
_space_group_name_Hall           'F 2 -2d'

_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+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'

_cell_length_a                   16.7630(14)
_cell_length_b                   40.360(4)
_cell_length_c                   12.3474(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8353.7(15)
_cell_formula_units_Z            8
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9631
_cell_measurement_theta_min      2.5465
_cell_measurement_theta_max      28.178

_exptl_crystal_description       Block
_exptl_crystal_colour            Black
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_F_000             3776
_exptl_transmission_factor_min   0.6822
_exptl_transmission_factor_max   0.7457
_exptl_crystal_size_max          0.094
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.089
_exptl_absorpt_coefficient_mu    3.344
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6822
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   
;
L. Krause, R. Herbst-Irmer, G. M. Sheldrick & D. Stalke. J. Appl.
Cryst., 2015, 48, 3.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_recrystallization_method 
'Crystals were deposited from a solution of the material dissolvedin CD2Cl2 layered with pentane.'
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_monochromator     'Bruker TRIUMPH curved-graphite'
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       'combination of ω and φ-scans '
_diffrn_detector_area_resol_mean 8.33
_diffrn_reflns_number            47083
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -53
_diffrn_reflns_limit_k_max       53
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.018
_diffrn_reflns_theta_max         28.338
_diffrn_reflns_theta_full        25.242
_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 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5202
_reflns_number_gt                4719
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.911
_reflns_Friedel_fraction_max     0.996
_reflns_Friedel_fraction_full    0.998

_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 APEX-3 (Bruker, 2015)'
_computing_cell_refinement       'Bruker SAINT (Bruker, 2015)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2015)'
_computing_structure_solution    'SHELXT-2014/2 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_molecular_graphics    'Bruker XP (Bruker, 2015)'
_computing_publication_material  'CIFTAB (Sheldrick, 2008)'
_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)+(0.0161P)²+23.4062P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_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 2123 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.005(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5202
_refine_ls_number_parameters     235
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0256
_refine_ls_wR_factor_ref         0.0488
_refine_ls_wR_factor_gt          0.0472
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.057
_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
Os Os 0.500000 0.500000 0.95268(3) 0.01426(6) Uani 1 2 d S T P . .
O1 O 0.57661(16) 0.46174(7) 0.9517(3) 0.0162(6) Uani 1 1 d . . . . .
N1 N 0.4493(2) 0.47050(9) 0.8476(3) 0.0160(8) Uani 1 1 d . . . . .
Cl1 Cl 0.43066(7) 0.47062(3) 1.08879(9) 0.0227(2) Uani 1 1 d . . . . .
C11 C 0.5453(3) 0.43453(11) 0.9139(4) 0.0163(9) Uani 1 1 d . . . . .
C12 C 0.4736(3) 0.43859(11) 0.8515(4) 0.0178(9) Uani 1 1 d . . . . .
C13 C 0.4360(3) 0.41103(11) 0.8023(4) 0.0195(10) Uani 1 1 d . . . . .
H13 H 0.389340 0.413965 0.759752 0.023 Uiso 1 1 calc R U . . .
C14 C 0.4675(3) 0.38025(11) 0.8167(4) 0.0208(10) Uani 1 1 d . . . . .
C15 C 0.5394(3) 0.37690(11) 0.8797(4) 0.0207(10) Uani 1 1 d . . . . .
H15 H 0.560529 0.355227 0.888579 0.025 Uiso 1 1 calc R U . . .
C16 C 0.5797(3) 0.40243(11) 0.9276(4) 0.0183(10) Uani 1 1 d . . . . .
C17 C 0.6567(3) 0.39791(11) 0.9926(4) 0.0220(10) Uani 1 1 d . . . . .
C171 C 0.7248(3) 0.41614(14) 0.9354(5) 0.0274(13) Uani 1 1 d . . . . .
H17A H 0.774192 0.413312 0.976727 0.041 Uiso 1 1 calc R U . . .
H17B H 0.731795 0.406998 0.862449 0.041 Uiso 1 1 calc R U . . .
H17C H 0.711874 0.439768 0.930223 0.041 Uiso 1 1 calc R U . . .
C172 C 0.6454(3) 0.41149(13) 1.1084(4) 0.0277(11) Uani 1 1 d . . . . .
H17D H 0.601692 0.399594 1.143952 0.042 Uiso 1 1 calc R U . . .
H17E H 0.694708 0.408345 1.149752 0.042 Uiso 1 1 calc R U . . .
H17F H 0.632606 0.435159 1.104939 0.042 Uiso 1 1 calc R U . . .
C173 C 0.6791(3) 0.36099(13) 1.0014(5) 0.0328(13) Uani 1 1 d . . . . .
H17G H 0.636149 0.348922 1.037936 0.049 Uiso 1 1 calc R U . . .
H17H H 0.686990 0.351829 0.928647 0.049 Uiso 1 1 calc R U . . .
H17I H 0.728576 0.358721 1.043118 0.049 Uiso 1 1 calc R U . . .
C18 C 0.4272(3) 0.34894(12) 0.7722(4) 0.0266(11) Uani 1 1 d . . . . .
C181 C 0.3579(4) 0.35763(13) 0.6966(6) 0.0446(16) Uani 1 1 d . . . . .
H18A H 0.318556 0.370934 0.736098 0.067 Uiso 1 1 calc R U . . .
H18B H 0.378043 0.370316 0.634746 0.067 Uiso 1 1 calc R U . . .
H18C H 0.332712 0.337202 0.670736 0.067 Uiso 1 1 calc R U . . .
C182 C 0.4874(4) 0.32820(16) 0.7079(7) 0.0382(15) Uani 1 1 d . . . . .
H18D H 0.532426 0.322318 0.754667 0.057 Uiso 1 1 calc R U . . .
H18E H 0.461417 0.307943 0.681885 0.057 Uiso 1 1 calc R U . . .
H18F H 0.506748 0.341057 0.645895 0.057 Uiso 1 1 calc R U . . .
C183 C 0.3943(4) 0.32888(13) 0.8681(5) 0.0372(14) Uani 1 1 d . . . . .
H18G H 0.438041 0.323123 0.917251 0.056 Uiso 1 1 calc R U . . .
H18H H 0.354635 0.342159 0.906999 0.056 Uiso 1 1 calc R U . . .
H18I H 0.369217 0.308560 0.841081 0.056 Uiso 1 1 calc R U . . .
C26 C 0.3950(3) 0.47467(13) 0.6639(4) 0.0266(11) Uani 1 1 d . . . . .
H26 H 0.443252 0.465861 0.635571 0.032 Uiso 1 1 calc R U . . .
C25 C 0.3320(4) 0.48283(14) 0.5952(5) 0.0342(13) Uani 1 1 d . . . . .
H25 H 0.337293 0.479782 0.519239 0.041 Uiso 1 1 calc R U . . .
C24 C 0.2620(5) 0.4953(2) 0.6373(8) 0.036(2) Uani 1 1 d . . . . .
H24 H 0.218758 0.500134 0.590115 0.043 Uiso 1 1 calc R U . . .
C23 C 0.2538(5) 0.5009(2) 0.7474(9) 0.035(2) Uani 1 1 d . . . . .
H23 H 0.205861 0.510054 0.775536 0.042 Uiso 1 1 calc R U . . .
C22 C 0.3167(3) 0.49309(11) 0.8161(4) 0.0243(11) Uani 1 1 d . . . . .
H22 H 0.312168 0.496958 0.891722 0.029 Uiso 1 1 calc R U . . .
C21 C 0.3859(3) 0.47963(11) 0.7739(4) 0.0199(10) Uani 1 1 d . . . . .
C9S C 0.5289(9) 0.4905(3) 0.3322(11) 0.055(4) Uani 0.5 1 d . . P A -1
D9S1 D 0.524021 0.490554 0.252317 0.066 Uiso 0.5 1 calc R U P A -1
D9S2 D 0.584144 0.484200 0.351729 0.066 Uiso 0.5 1 calc R U P A -1
Cl9S Cl 0.4615(2) 0.46326(9) 0.3887(3) 0.0412(8) Uani 0.5 1 d . . P A -1
Cl10 Cl 0.5043(3) 0.53149(16) 0.3876(5) 0.0774(19) Uiso 0.5 1 d . . P A -1


_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
Os N1 1.956(4) . ?
Os N1 1.956(4) 2_665 ?
Os O1 2.008(3) . ?
Os O1 2.009(3) 2_665 ?
Os Cl1 2.3626(12) . ?
Os Cl1 2.3626(12) 2_665 ?
O1 C11 1.304(5) . ?
N1 C12 1.351(6) . ?
N1 C21 1.447(6) . ?
C11 C16 1.428(6) . ?
C11 C12 1.437(6) . ?
C12 C13 1.415(6) . ?
C13 C14 1.361(6) . ?
C13 H13 0.9500 . ?
C14 C15 1.441(7) . ?
C14 C18 1.534(6) . ?
C15 C16 1.366(6) . ?
C15 H15 0.9500 . ?
C16 C17 1.532(6) . ?
C17 C171 1.530(8) . ?
C17 C173 1.541(7) . ?
C17 C172 1.542(7) . ?
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 . ?
C18 C181 1.531(7) . ?
C18 C182 1.533(8) . ?
C18 C183 1.537(8) . ?
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 . ?
C26 C21 1.382(7) . ?
C26 C25 1.394(7) . ?
C26 H26 0.9500 . ?
C25 C24 1.379(11) . ?
C25 H25 0.9500 . ?
C24 C23 1.385(10) . ?
C24 H24 0.9500 . ?
C23 C22 1.390(11) . ?
C23 H23 0.9500 . ?
C22 C21 1.382(7) . ?
C22 H22 0.9500 . ?
C9S Cl9S 1.723(13) . ?
C9S Cl10 1.837(14) . ?
C9S D9S1 0.9900 . ?
C9S D9S2 0.9900 . ?

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 Os N1 96.8(2) . 2_665 ?
N1 Os O1 78.79(14) . . ?
N1 Os O1 100.73(14) 2_665 . ?
N1 Os O1 100.73(14) . 2_665 ?
N1 Os O1 78.79(14) 2_665 2_665 ?
O1 Os O1 179.3(2) . 2_665 ?
N1 Os Cl1 87.29(11) . . ?
N1 Os Cl1 172.52(11) 2_665 . ?
O1 Os Cl1 86.16(10) . . ?
O1 Os Cl1 94.34(9) 2_665 . ?
N1 Os Cl1 172.52(11) . 2_665 ?
N1 Os Cl1 87.29(11) 2_665 2_665 ?
O1 Os Cl1 94.34(9) . 2_665 ?
O1 Os Cl1 86.16(10) 2_665 2_665 ?
Cl1 Os Cl1 89.31(6) . 2_665 ?
C11 O1 Os 113.1(3) . . ?
C12 N1 C21 119.1(4) . . ?
C12 N1 Os 115.2(3) . . ?
C21 N1 Os 125.5(3) . . ?
O1 C11 C16 124.0(4) . . ?
O1 C11 C12 115.7(4) . . ?
C16 C11 C12 120.3(4) . . ?
N1 C12 C13 126.9(4) . . ?
N1 C12 C11 112.3(4) . . ?
C13 C12 C11 120.8(4) . . ?
C14 C13 C12 119.3(4) . . ?
C14 C13 H13 120.4 . . ?
C12 C13 H13 120.4 . . ?
C13 C14 C15 118.7(4) . . ?
C13 C14 C18 122.3(4) . . ?
C15 C14 C18 119.0(4) . . ?
C16 C15 C14 125.2(4) . . ?
C16 C15 H15 117.4 . . ?
C14 C15 H15 117.4 . . ?
C15 C16 C11 115.7(4) . . ?
C15 C16 C17 123.6(4) . . ?
C11 C16 C17 120.7(4) . . ?
C171 C17 C16 109.2(4) . . ?
C171 C17 C173 108.4(4) . . ?
C16 C17 C173 110.9(4) . . ?
C171 C17 C172 110.4(4) . . ?
C16 C17 C172 109.9(4) . . ?
C173 C17 C172 108.0(4) . . ?
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 . . ?
C181 C18 C182 108.0(5) . . ?
C181 C18 C14 111.3(4) . . ?
C182 C18 C14 110.3(5) . . ?
C181 C18 C183 108.5(5) . . ?
C182 C18 C183 110.3(5) . . ?
C14 C18 C183 108.4(4) . . ?
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 . . ?
C21 C26 C25 118.7(6) . . ?
C21 C26 H26 120.7 . . ?
C25 C26 H26 120.7 . . ?
C24 C25 C26 120.1(6) . . ?
C24 C25 H25 119.9 . . ?
C26 C25 H25 119.9 . . ?
C25 C24 C23 120.9(6) . . ?
C25 C24 H24 119.5 . . ?
C23 C24 H24 119.5 . . ?
C24 C23 C22 119.1(7) . . ?
C24 C23 H23 120.4 . . ?
C22 C23 H23 120.4 . . ?
C21 C22 C23 119.7(6) . . ?
C21 C22 H22 120.1 . . ?
C23 C22 H22 120.1 . . ?
C26 C21 C22 121.3(5) . . ?
C26 C21 N1 120.0(5) . . ?
C22 C21 N1 118.7(4) . . ?
Cl9S C9S Cl10 106.1(7) . . ?
Cl9S C9S D9S1 110.5 . . ?
Cl10 C9S D9S1 110.5 . . ?
Cl9S C9S D9S2 110.5 . . ?
Cl10 C9S D9S2 110.5 . . ?
D9S1 C9S D9S2 108.7 . . ?

_refine_diff_density_max         1.768
_refine_diff_density_min         -1.241
_refine_diff_density_rms         0.118

####################################################################### 
# 
# 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_eganoso
_database_code_depnum_ccdc_archive 'CCDC 2003368'
loop_
_audit_author_name
_audit_author_address
'Seth Brown' 'University of Notre Dame'
_audit_update_record             
;
2020-05-11 deposited with the CCDC.	2020-06-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
(Oxo)(1,2-ethanedi-(2-(3,5-di-tert-butyl-2-oxyphenyl)amido)-benzoate)osmium(VI)
_chemical_name_common            (Egan)OsO
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H52 N2 O7 Os'
_chemical_formula_sum            'C44 H52 N2 O7 Os'
_chemical_formula_weight         911.07

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'
Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

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

_cell_length_a                   13.0153(6)
_cell_length_b                   13.1218(7)
_cell_length_c                   14.0466(6)
_cell_angle_alpha                105.229(2)
_cell_angle_beta                 104.4965(19)
_cell_angle_gamma                108.180(2)
_cell_volume                     2049.60(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9775
_cell_measurement_theta_min      2.50
_cell_measurement_theta_max      30.64

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_F_000             924
_exptl_transmission_factor_min   0.6140
_exptl_transmission_factor_max   0.7802
_exptl_crystal_size_max          0.214
_exptl_crystal_size_mid          0.129
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    3.162
_shelx_estimated_absorpt_T_min   0.551
_shelx_estimated_absorpt_T_max   0.703
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.6140
_exptl_absorpt_correction_T_max  0.7802
_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 vapor diffusion of methanol intoa benzene solution of the complex.'

_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            66041
_diffrn_reflns_av_unetI/netI     0.0166
_diffrn_reflns_av_R_equivalents  0.0210
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.612
_diffrn_reflns_theta_max         30.659
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             12637
_reflns_number_gt                11999
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker 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)+(0.0160P)²+0.7482P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12637
_refine_ls_number_parameters     88
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0156
_refine_ls_R_factor_gt           0.0140
_refine_ls_wR_factor_ref         0.0336
_refine_ls_wR_factor_gt          0.0332
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.007
_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
Os Os 0.97083(2) 0.91603(2) 0.71251(2) 0.01122(2) Uani 1 1 d . . . . .
O O 1.00751(8) 1.06044(8) 0.75597(8) 0.01992(19) Uani 1 1 d . . . . .
O1 O 1.11099(7) 0.88958(8) 0.73876(7) 0.01379(16) Uani 1 1 d . . . . .
N1 N 0.96508(9) 0.86012(9) 0.82583(8) 0.01312(19) Uani 1 1 d . . . . .
C1 C 0.87670(12) 0.53281(12) 0.64354(11) 0.0189(2) Uani 1 1 d . . . . .
H1B H 0.9546(15) 0.5472(15) 0.6793(13) 0.021(4) Uiso 1 1 d . . . . .
H1A H 0.8269(15) 0.4630(16) 0.6416(13) 0.024(4) Uiso 1 1 d . . . . .
O2 O 0.80360(7) 0.83717(8) 0.65392(7) 0.01348(16) Uani 1 1 d . . . . .
N2 N 0.94865(9) 0.85627(9) 0.56449(8) 0.01241(18) Uani 1 1 d . . . . .
C2 C 0.85566(12) 0.52989(12) 0.53326(11) 0.0196(3) Uani 1 1 d . . . . .
H2B H 0.7805(15) 0.5257(14) 0.5021(13) 0.020(4) Uiso 1 1 d . . . . .
H2A H 0.8627(16) 0.4648(17) 0.4904(15) 0.030(5) Uiso 1 1 d . . . . .
O10 O 0.80367(13) 0.52519(10) 0.80151(10) 0.0400(3) Uani 1 1 d . . . . .
O11 O 0.85303(8) 0.62551(8) 0.70182(7) 0.01702(17) Uani 1 1 d . . . . .
C11 C 1.14152(10) 0.85721(10) 0.82294(9) 0.0133(2) Uani 1 1 d . . . . .
C12 C 1.06022(10) 0.83637(11) 0.87072(9) 0.0135(2) Uani 1 1 d . . . . .
C13 C 1.07579(11) 0.79507(11) 0.95252(10) 0.0161(2) Uani 1 1 d . . . . .
H13 H 1.0183(15) 0.7820(15) 0.9850(14) 0.024(4) Uiso 1 1 d . . . . .
C14 C 1.17535(11) 0.77608(11) 0.98702(10) 0.0172(2) Uani 1 1 d . . . . .
C15 C 1.25812(11) 0.80228(12) 0.93976(10) 0.0171(2) Uani 1 1 d . . . . .
H15 H 1.3272(14) 0.7910(14) 0.9651(12) 0.015(4) Uiso 1 1 d . . . . .
C16 C 1.24418(10) 0.84207(11) 0.85662(9) 0.0144(2) Uani 1 1 d . . . . .
C17 C 1.33182(11) 0.86308(12) 0.80175(10) 0.0173(2) Uani 1 1 d . . . . .
C18 C 1.19465(12) 0.72194(14) 1.07037(11) 0.0238(3) Uani 1 1 d . . . . .
O20 O 0.91334(9) 0.55107(9) 0.36706(8) 0.0252(2) Uani 1 1 d . . . . .
O21 O 0.93952(8) 0.63485(8) 0.53804(7) 0.01728(18) Uani 1 1 d . . . . .
C21 C 0.75430(10) 0.78906(10) 0.54589(9) 0.0130(2) Uani 1 1 d . . . . .
C22 C 0.83286(10) 0.79595(10) 0.49423(9) 0.0128(2) Uani 1 1 d . . . . .
C23 C 0.79540(11) 0.74806(11) 0.38477(10) 0.0151(2) Uani 1 1 d . . . . .
H23 H 0.8521(14) 0.7566(14) 0.3518(13) 0.017(4) Uiso 1 1 d . . . . .
C24 C 0.67732(11) 0.68946(11) 0.32621(10) 0.0169(2) Uani 1 1 d . . . . .
C25 C 0.60002(11) 0.68593(12) 0.38021(10) 0.0177(2) Uani 1 1 d . . . . .
H25 H 0.5173(14) 0.6471(14) 0.3395(13) 0.017(4) Uiso 1 1 d . . . . .
C26 C 0.63451(10) 0.73633(11) 0.48981(10) 0.0151(2) Uani 1 1 d . . . . .
C27 C 0.54803(11) 0.73902(12) 0.54565(10) 0.0177(2) Uani 1 1 d . . . . .
C28 C 0.63268(12) 0.62299(13) 0.20701(10) 0.0223(3) Uani 1 1 d . . . . .
C30 C 0.82131(12) 0.61183(12) 0.78287(10) 0.0192(2) Uani 1 1 d . . . . .
C31 C 0.80422(11) 0.71302(11) 0.84282(10) 0.0162(2) Uani 1 1 d . . . . .
C32 C 0.86664(10) 0.82683(11) 0.85557(9) 0.0145(2) Uani 1 1 d . . . . .
C33 C 0.83640(11) 0.91349(12) 0.90378(10) 0.0193(2) Uani 1 1 d . . . . .
H33 H 0.8736(16) 0.9875(17) 0.9107(14) 0.029(5) Uiso 1 1 d . . . . .
C34 C 0.74686(12) 0.88891(14) 0.94230(11) 0.0236(3) Uani 1 1 d . . . . .
H34 H 0.7285(15) 0.9475(16) 0.9752(14) 0.026(4) Uiso 1 1 d . . . . .
C35 C 0.68913(12) 0.77732(14) 0.93465(11) 0.0245(3) Uani 1 1 d . . . . .
H35 H 0.6289(16) 0.7586(16) 0.9596(15) 0.032(5) Uiso 1 1 d . . . . .
C36 C 0.71777(12) 0.69033(13) 0.88556(11) 0.0213(3) Uani 1 1 d . . . . .
H36 H 0.6794(15) 0.6151(15) 0.8776(13) 0.020(4) Uiso 1 1 d . . . . .
C40 C 0.95559(11) 0.63498(12) 0.44742(10) 0.0175(2) Uani 1 1 d . . . . .
C41 C 1.03804(11) 0.75091(11) 0.46239(10) 0.0166(2) Uani 1 1 d . . . . .
C42 C 1.03882(10) 0.85368(11) 0.52524(10) 0.0142(2) Uani 1 1 d . . . . .
C43 C 1.12768(11) 0.95796(12) 0.54725(11) 0.0184(2) Uani 1 1 d . . . . .
H43 H 1.1319(15) 1.0264(16) 0.5901(14) 0.026(4) Uiso 1 1 d . . . . .
C44 C 1.21337(13) 0.96128(14) 0.50446(13) 0.0252(3) Uani 1 1 d . . . . .
H44 H 1.2725(16) 1.0295(16) 0.5201(14) 0.029(5) Uiso 1 1 d . . . . .
C45 C 1.20814(14) 0.86103(15) 0.43632(13) 0.0279(3) Uani 1 1 d . . . . .
H45 H 1.2649(17) 0.8668(17) 0.4069(15) 0.034(5) Uiso 1 1 d . . . . .
C46 C 1.12039(13) 0.75623(14) 0.41484(12) 0.0234(3) Uani 1 1 d . . . . .
H46 H 1.1171(15) 0.6878(16) 0.3684(14) 0.024(4) Uiso 1 1 d . . . . .
C171 C 1.27406(13) 0.77443(15) 0.68805(11) 0.0249(3) Uani 1 1 d . . . . .
H17C H 1.2050(17) 0.7804(16) 0.6503(15) 0.030(5) Uiso 1 1 d . . . . .
H17B H 1.2545(17) 0.6985(18) 0.6890(15) 0.036(5) Uiso 1 1 d . . . . .
H17A H 1.3272(18) 0.7843(18) 0.6491(16) 0.040(5) Uiso 1 1 d . . . . .
C172 C 1.44056(12) 0.84798(15) 0.85609(12) 0.0243(3) Uani 1 1 d . . . . .
H17F H 1.4793(15) 0.9029(16) 0.9284(14) 0.026(4) Uiso 1 1 d . . . . .
H17E H 1.4227(15) 0.7687(16) 0.8553(14) 0.026(5) Uiso 1 1 d . . . . .
H17D H 1.4947(16) 0.8618(16) 0.8196(14) 0.029(5) Uiso 1 1 d . . . . .
C173 C 1.36968(12) 0.98591(14) 0.80123(12) 0.0240(3) Uani 1 1 d . . . . .
H17I H 1.3056(16) 1.0047(16) 0.7657(14) 0.028(5) Uiso 1 1 d . . . . .
H17H H 1.4100(17) 1.0444(17) 0.8728(16) 0.033(5) Uiso 1 1 d . . . . .
H17G H 1.4243(18) 0.9986(17) 0.7649(16) 0.038(5) Uiso 1 1 d . . . . .
C181 C 1.2060(2) 0.60913(17) 1.02004(17) 0.0400(4) Uani 1 1 d . . . . .
H18C H 1.2141(18) 0.5729(18) 1.0721(16) 0.041(6) Uiso 1 1 d . . . . .
H18B H 1.1354(19) 0.5561(19) 0.9584(18) 0.045(6) Uiso 1 1 d . . . . .
H18A H 1.2720(18) 0.6224(18) 0.9925(16) 0.040(5) Uiso 1 1 d . . . . .
C182 C 1.09422(16) 0.6940(2) 1.10990(16) 0.0386(4) Uani 1 1 d . . . . .
H18F H 1.0225(18) 0.6423(17) 1.0515(16) 0.037(5) Uiso 1 1 d . . . . .
H18E H 1.0878(18) 0.7642(19) 1.1461(16) 0.041(6) Uiso 1 1 d . . . . .
H18D H 1.1068(18) 0.6576(18) 1.1596(16) 0.041(6) Uiso 1 1 d . . . . .
C183 C 1.30623(16) 0.80338(19) 1.16481(14) 0.0379(4) Uani 1 1 d . . . . .
H18I H 1.3176(19) 0.768(2) 1.2150(18) 0.051(6) Uiso 1 1 d . . . . .
H18H H 1.3748(19) 0.8234(19) 1.1439(17) 0.046(6) Uiso 1 1 d . . . . .
H18G H 1.2992(17) 0.8728(19) 1.1969(16) 0.037(6) Uiso 1 1 d . . . . .
C271 C 0.42294(12) 0.68014(15) 0.46714(12) 0.0260(3) Uani 1 1 d . . . . .
H27C H 0.4103(16) 0.7156(16) 0.4184(15) 0.027(5) Uiso 1 1 d . . . . .
H27B H 0.3712(17) 0.6858(16) 0.5048(15) 0.032(5) Uiso 1 1 d . . . . .
H27A H 0.4018(16) 0.6000(18) 0.4309(15) 0.033(5) Uiso 1 1 d . . . . .
C272 C 0.57279(13) 0.86516(14) 0.60498(13) 0.0253(3) Uani 1 1 d . . . . .
H27F H 0.6503(16) 0.9075(15) 0.6569(14) 0.026(4) Uiso 1 1 d . . . . .
H27E H 0.5206(16) 0.8698(16) 0.6399(15) 0.029(5) Uiso 1 1 d . . . . .
H27D H 0.5626(16) 0.9020(17) 0.5575(15) 0.031(5) Uiso 1 1 d . . . . .
C273 C 0.55903(13) 0.67703(15) 0.62369(12) 0.0255(3) Uani 1 1 d . . . . .
H27I H 0.6347(17) 0.7136(16) 0.6779(15) 0.031(5) Uiso 1 1 d . . . . .
H27H H 0.5478(17) 0.5995(18) 0.5904(15) 0.034(5) Uiso 1 1 d . . . . .
H27G H 0.5037(17) 0.6796(17) 0.6591(15) 0.035(5) Uiso 1 1 d . . . . .
C281 C 0.52660(18) 0.6404(2) 0.15008(13) 0.0397(4) Uani 1 1 d . . . . .
H28C H 0.5464(17) 0.7197(19) 0.1638(15) 0.034(5) Uiso 1 1 d . . . . .
H28B H 0.4999(18) 0.6015(19) 0.0765(18) 0.045(6) Uiso 1 1 d . . . . .
H28A H 0.462(2) 0.6167(19) 0.1742(17) 0.049(6) Uiso 1 1 d . . . . .
C282 C 0.72487(16) 0.65865(18) 0.15926(12) 0.0370(4) Uani 1 1 d . . . . .
H28F H 0.7508(17) 0.7404(18) 0.1723(15) 0.035(5) Uiso 1 1 d . . . . .
H28E H 0.792(2) 0.6449(19) 0.1876(17) 0.047(6) Uiso 1 1 d . . . . .
H28D H 0.6893(18) 0.6140(18) 0.0796(17) 0.043(6) Uiso 1 1 d . . . . .
C283 C 0.59902(16) 0.49477(15) 0.18960(13) 0.0321(3) Uani 1 1 d . . . . .
H28I H 0.6684(18) 0.4799(18) 0.2229(16) 0.039(5) Uiso 1 1 d . . . . .
H28H H 0.5687(17) 0.4466(17) 0.1151(16) 0.038(5) Uiso 1 1 d . . . . .
H28G H 0.5381(17) 0.4657(17) 0.2195(15) 0.035(5) 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
Os O 1.6951(9) . ?
Os O1 1.9260(9) . ?
Os N1 1.9277(10) . ?
Os N2 1.9295(10) . ?
Os O2 1.9328(9) . ?
O1 C11 1.3676(14) . ?
N1 C12 1.4076(15) . ?
N1 C32 1.4217(15) . ?
C1 O11 1.4428(16) . ?
C1 C2 1.4918(19) . ?
C1 H1B 0.945(17) . ?
C1 H1A 0.932(18) . ?
O2 C21 1.3673(14) . ?
N2 C22 1.4044(15) . ?
N2 C42 1.4218(15) . ?
C2 O21 1.4385(16) . ?
C2 H2B 0.944(17) . ?
C2 H2A 0.953(19) . ?
O10 C30 1.1988(17) . ?
O11 C30 1.3399(15) . ?
C11 C12 1.3843(17) . ?
C11 C16 1.3954(17) . ?
C12 C13 1.3908(17) . ?
C13 C14 1.3880(18) . ?
C13 H13 0.963(18) . ?
C14 C15 1.4022(18) . ?
C14 C18 1.5296(18) . ?
C15 C16 1.3937(17) . ?
C15 H15 0.953(16) . ?
C16 C17 1.5254(17) . ?
C17 C172 1.5292(18) . ?
C17 C171 1.5317(19) . ?
C17 C173 1.534(2) . ?
C18 C182 1.524(2) . ?
C18 C183 1.527(2) . ?
C18 C181 1.533(3) . ?
O20 C40 1.2030(16) . ?
O21 C40 1.3411(15) . ?
C21 C22 1.3885(16) . ?
C21 C26 1.3985(16) . ?
C22 C23 1.3866(17) . ?
C23 C24 1.3882(18) . ?
C23 H23 0.958(17) . ?
C24 C25 1.4004(18) . ?
C24 C28 1.5269(18) . ?
C25 C26 1.3939(17) . ?
C25 H25 0.971(16) . ?
C26 C27 1.5282(17) . ?
C27 C271 1.5272(18) . ?
C27 C272 1.532(2) . ?
C27 C273 1.532(2) . ?
C28 C282 1.525(2) . ?
C28 C281 1.529(2) . ?
C28 C283 1.534(2) . ?
C30 C31 1.4875(19) . ?
C31 C36 1.3921(18) . ?
C31 C32 1.3971(18) . ?
C32 C33 1.3838(19) . ?
C33 C34 1.3885(19) . ?
C33 H33 0.906(19) . ?
C34 C35 1.382(2) . ?
C34 H34 0.920(19) . ?
C35 C36 1.378(2) . ?
C35 H35 0.927(19) . ?
C36 H36 0.919(17) . ?
C40 C41 1.4867(18) . ?
C41 C46 1.3914(18) . ?
C41 C42 1.3998(18) . ?
C42 C43 1.3845(18) . ?
C43 C44 1.3879(19) . ?
C43 H43 0.917(19) . ?
C44 C45 1.379(2) . ?
C44 H44 0.907(19) . ?
C45 C46 1.384(2) . ?
C45 H45 0.93(2) . ?
C46 H46 0.943(18) . ?
C171 H17C 0.961(19) . ?
C171 H17B 0.95(2) . ?
C171 H17A 0.98(2) . ?
C172 H17F 0.968(18) . ?
C172 H17E 0.989(19) . ?
C172 H17D 0.970(19) . ?
C173 H17I 0.995(19) . ?
C173 H17H 0.98(2) . ?
C173 H17G 0.97(2) . ?
C181 H18C 0.97(2) . ?
C181 H18B 0.98(2) . ?
C181 H18A 1.01(2) . ?
C182 H18F 0.97(2) . ?
C182 H18E 0.97(2) . ?
C182 H18D 0.95(2) . ?
C183 H18I 0.95(2) . ?
C183 H18H 0.99(2) . ?
C183 H18G 0.95(2) . ?
C271 H27C 0.933(19) . ?
C271 H27B 0.96(2) . ?
C271 H27A 0.95(2) . ?
C272 H27F 0.963(18) . ?
C272 H27E 0.940(19) . ?
C272 H27D 0.928(19) . ?
C273 H27I 0.958(19) . ?
C273 H27H 0.95(2) . ?
C273 H27G 0.98(2) . ?
C281 H28C 0.94(2) . ?
C281 H28B 0.94(2) . ?
C281 H28A 0.98(2) . ?
C282 H28F 0.97(2) . ?
C282 H28E 0.95(2) . ?
C282 H28D 1.02(2) . ?
C283 H28I 1.01(2) . ?
C283 H28H 0.97(2) . ?
C283 H28G 1.01(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
O Os O1 108.56(4) . . ?
O Os N1 110.68(5) . . ?
O1 Os N1 80.54(4) . . ?
O Os N2 110.63(5) . . ?
O1 Os N2 86.04(4) . . ?
N1 Os N2 138.69(4) . . ?
O Os O2 108.78(4) . . ?
O1 Os O2 142.66(4) . . ?
N1 Os O2 86.68(4) . . ?
N2 Os O2 80.77(4) . . ?
C11 O1 Os 116.26(7) . . ?
C12 N1 C32 118.78(10) . . ?
C12 N1 Os 115.92(8) . . ?
C32 N1 Os 124.68(8) . . ?
O11 C1 C2 108.71(11) . . ?
O11 C1 H1B 107.4(10) . . ?
C2 C1 H1B 111.9(10) . . ?
O11 C1 H1A 109.2(11) . . ?
C2 C1 H1A 109.2(11) . . ?
H1B C1 H1A 110.3(15) . . ?
C21 O2 Os 115.91(7) . . ?
C22 N2 C42 118.91(10) . . ?
C22 N2 Os 115.73(8) . . ?
C42 N2 Os 124.58(8) . . ?
O21 C2 C1 108.02(11) . . ?
O21 C2 H2B 108.8(10) . . ?
C1 C2 H2B 110.6(10) . . ?
O21 C2 H2A 110.0(11) . . ?
C1 C2 H2A 111.0(11) . . ?
H2B C2 H2A 108.3(15) . . ?
C30 O11 C1 115.34(10) . . ?
O1 C11 C12 114.64(10) . . ?
O1 C11 C16 123.32(11) . . ?
C12 C11 C16 122.00(11) . . ?
C11 C12 C13 121.00(11) . . ?
C11 C12 N1 112.32(10) . . ?
C13 C12 N1 126.67(11) . . ?
C14 C13 C12 119.01(12) . . ?
C14 C13 H13 121.5(10) . . ?
C12 C13 H13 119.4(10) . . ?
C13 C14 C15 118.57(12) . . ?
C13 C14 C18 122.27(12) . . ?
C15 C14 C18 119.09(12) . . ?
C16 C15 C14 123.71(12) . . ?
C16 C15 H15 118.1(10) . . ?
C14 C15 H15 118.2(9) . . ?
C15 C16 C11 115.63(11) . . ?
C15 C16 C17 122.93(11) . . ?
C11 C16 C17 121.39(11) . . ?
C16 C17 C172 112.16(11) . . ?
C16 C17 C171 108.01(11) . . ?
C172 C17 C171 108.05(12) . . ?
C16 C17 C173 110.52(11) . . ?
C172 C17 C173 107.98(11) . . ?
C171 C17 C173 110.09(12) . . ?
C182 C18 C183 108.73(14) . . ?
C182 C18 C14 112.33(12) . . ?
C183 C18 C14 110.20(13) . . ?
C182 C18 C181 108.29(15) . . ?
C183 C18 C181 108.97(15) . . ?
C14 C18 C181 108.24(12) . . ?
C40 O21 C2 116.46(10) . . ?
O2 C21 C22 114.75(10) . . ?
O2 C21 C26 123.72(11) . . ?
C22 C21 C26 121.52(11) . . ?
C23 C22 C21 121.16(11) . . ?
C23 C22 N2 126.22(11) . . ?
C21 C22 N2 112.62(10) . . ?
C22 C23 C24 119.26(11) . . ?
C22 C23 H23 118.8(10) . . ?
C24 C23 H23 121.9(10) . . ?
C23 C24 C25 118.31(11) . . ?
C23 C24 C28 121.04(12) . . ?
C25 C24 C28 120.50(12) . . ?
C26 C25 C24 123.92(12) . . ?
C26 C25 H25 117.4(10) . . ?
C24 C25 H25 118.7(9) . . ?
C25 C26 C21 115.70(11) . . ?
C25 C26 C27 122.61(11) . . ?
C21 C26 C27 121.64(11) . . ?
C271 C27 C26 111.76(11) . . ?
C271 C27 C272 108.11(12) . . ?
C26 C27 C272 108.68(11) . . ?
C271 C27 C273 107.90(12) . . ?
C26 C27 C273 110.53(11) . . ?
C272 C27 C273 109.82(12) . . ?
C282 C28 C24 112.38(12) . . ?
C282 C28 C281 108.77(14) . . ?
C24 C28 C281 110.82(13) . . ?
C282 C28 C283 107.97(14) . . ?
C24 C28 C283 107.19(11) . . ?
C281 C28 C283 109.65(14) . . ?
O10 C30 O11 123.32(13) . . ?
O10 C30 C31 124.06(13) . . ?
O11 C30 C31 112.53(11) . . ?
C36 C31 C32 119.07(13) . . ?
C36 C31 C30 116.78(12) . . ?
C32 C31 C30 124.13(11) . . ?
C33 C32 C31 119.62(12) . . ?
C33 C32 N1 117.31(12) . . ?
C31 C32 N1 123.00(11) . . ?
C32 C33 C34 120.63(14) . . ?
C32 C33 H33 121.4(12) . . ?
C34 C33 H33 118.0(12) . . ?
C35 C34 C33 119.71(14) . . ?
C35 C34 H34 120.5(11) . . ?
C33 C34 H34 119.7(12) . . ?
C36 C35 C34 119.96(13) . . ?
C36 C35 H35 118.6(12) . . ?
C34 C35 H35 121.4(12) . . ?
C35 C36 C31 120.86(14) . . ?
C35 C36 H36 121.8(11) . . ?
C31 C36 H36 117.3(11) . . ?
O20 C40 O21 124.26(13) . . ?
O20 C40 C41 125.11(12) . . ?
O21 C40 C41 110.53(11) . . ?
C46 C41 C42 119.21(12) . . ?
C46 C41 C40 117.96(12) . . ?
C42 C41 C40 122.78(11) . . ?
C43 C42 C41 119.55(12) . . ?
C43 C42 N2 117.90(12) . . ?
C41 C42 N2 122.49(11) . . ?
C42 C43 C44 120.38(14) . . ?
C42 C43 H43 121.5(11) . . ?
C44 C43 H43 118.1(11) . . ?
C45 C44 C43 120.14(14) . . ?
C45 C44 H44 119.5(12) . . ?
C43 C44 H44 120.4(12) . . ?
C44 C45 C46 119.81(13) . . ?
C44 C45 H45 117.9(12) . . ?
C46 C45 H45 122.3(12) . . ?
C45 C46 C41 120.57(14) . . ?
C45 C46 H46 119.7(11) . . ?
C41 C46 H46 119.7(11) . . ?
C17 C171 H17C 111.4(11) . . ?
C17 C171 H17B 109.6(12) . . ?
H17C C171 H17B 109.1(16) . . ?
C17 C171 H17A 111.2(12) . . ?
H17C C171 H17A 108.8(16) . . ?
H17B C171 H17A 106.6(17) . . ?
C17 C172 H17F 110.2(11) . . ?
C17 C172 H17E 112.1(10) . . ?
H17F C172 H17E 109.6(14) . . ?
C17 C172 H17D 110.4(11) . . ?
H17F C172 H17D 107.8(15) . . ?
H17E C172 H17D 106.5(15) . . ?
C17 C173 H17I 114.9(11) . . ?
C17 C173 H17H 111.9(11) . . ?
H17I C173 H17H 106.7(15) . . ?
C17 C173 H17G 110.4(12) . . ?
H17I C173 H17G 106.3(15) . . ?
H17H C173 H17G 106.1(16) . . ?
C18 C181 H18C 108.0(13) . . ?
C18 C181 H18B 110.2(13) . . ?
H18C C181 H18B 108.0(18) . . ?
C18 C181 H18A 111.9(12) . . ?
H18C C181 H18A 112.8(17) . . ?
H18B C181 H18A 105.9(17) . . ?
C18 C182 H18F 110.3(12) . . ?
C18 C182 H18E 110.3(13) . . ?
H18F C182 H18E 110.2(17) . . ?
C18 C182 H18D 110.8(13) . . ?
H18F C182 H18D 108.2(17) . . ?
H18E C182 H18D 106.9(17) . . ?
C18 C183 H18I 109.0(14) . . ?
C18 C183 H18H 112.3(13) . . ?
H18I C183 H18H 109.4(19) . . ?
C18 C183 H18G 109.3(13) . . ?
H18I C183 H18G 108.8(18) . . ?
H18H C183 H18G 108.0(18) . . ?
C27 C271 H27C 111.9(11) . . ?
C27 C271 H27B 109.4(11) . . ?
H27C C271 H27B 106.8(16) . . ?
C27 C271 H27A 111.3(11) . . ?
H27C C271 H27A 110.0(16) . . ?
H27B C271 H27A 107.1(16) . . ?
C27 C272 H27F 112.6(11) . . ?
C27 C272 H27E 110.8(12) . . ?
H27F C272 H27E 107.9(15) . . ?
C27 C272 H27D 110.1(12) . . ?
H27F C272 H27D 108.4(16) . . ?
H27E C272 H27D 106.7(16) . . ?
C27 C273 H27I 111.7(11) . . ?
C27 C273 H27H 112.3(12) . . ?
H27I C273 H27H 105.9(16) . . ?
C27 C273 H27G 109.8(11) . . ?
H27I C273 H27G 106.9(16) . . ?
H27H C273 H27G 110.2(16) . . ?
C28 C281 H28C 109.6(12) . . ?
C28 C281 H28B 111.3(13) . . ?
H28C C281 H28B 108.1(17) . . ?
C28 C281 H28A 114.1(13) . . ?
H28C C281 H28A 104.7(18) . . ?
H28B C281 H28A 108.7(18) . . ?
C28 C282 H28F 109.8(12) . . ?
C28 C282 H28E 113.5(13) . . ?
H28F C282 H28E 107.4(18) . . ?
C28 C282 H28D 108.8(12) . . ?
H28F C282 H28D 108.5(16) . . ?
H28E C282 H28D 108.7(17) . . ?
C28 C283 H28I 111.5(12) . . ?
C28 C283 H28H 112.0(12) . . ?
H28I C283 H28H 105.5(16) . . ?
C28 C283 H28G 111.9(11) . . ?
H28I C283 H28G 108.4(16) . . ?
H28H C283 H28G 107.3(16) . . ?

_refine_diff_density_max         0.533
_refine_diff_density_min         -0.593
_refine_diff_density_rms         0.061

_shelxl_version_number           2013-4

