# 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_cliposcl2
_database_code_depnum_ccdc_archive 'CCDC 1994511'
loop_
_audit_author_name
_audit_author_address
'Seth Brown'
;University of Notre Dame
United States of America
;
_audit_update_record             
;
2020-04-02 deposited with the CCDC.	2020-04-29 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT391_cliposcl2           
;
PROBLEM: Deviating Methyl C181      H-C-H Bond Angle ....        119 Degree
RESPONSE: Hydrogens are observed on a methyl group of a 
tert-butyl group with only moderate precision.
;
# end Validation Reply Form



_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
"2,2'-biphenylenediamido-N,N'-bis(2-oxy-3,5-di-tertbutylphenyl)-dichloroosmium(VI) ethyl acetate solvate"
_chemical_name_common            '(Clip)OsCl2 . EtOAc'
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H48 Cl2 N2 O2 Os, C4 H8 O2'
_chemical_formula_sum            'C44 H56 Cl2 N2 O4 Os'
_chemical_formula_weight         938.00

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'

_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                   11.5267(6)
_cell_length_b                   10.3290(5)
_cell_length_c                   36.2615(19)
_cell_angle_alpha                90
_cell_angle_beta                 98.4471(18)
_cell_angle_gamma                90
_cell_volume                     4270.4(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9897
_cell_measurement_theta_min      2.27
_cell_measurement_theta_max      25.33

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_F_000             1904
_exptl_transmission_factor_min   0.6783
_exptl_transmission_factor_max   0.8620
_exptl_crystal_size_max          0.345
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.084
_exptl_absorpt_coefficient_mu    3.153
_shelx_estimated_absorpt_T_min   0.6783
_shelx_estimated_absorpt_T_max   0.8620
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6783
_exptl_absorpt_correction_T_max  0.8620
_exptl_absorpt_process_details   
;
Blessing, R. H. (1995) Acta Cryst. A51, 33-38.

Sheldrick, G.M. (2008) SADABS v2008/1. Bruker AXS Inc.
Madison, WI USA.
;

_exptl_crystal_recrystallization_method 
'Slow evaporation of a solution of the compound in a hexane/ethyl acetate mixture.'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus 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            58745
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_av_R_equivalents  0.0649
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_theta_min         1.793
_diffrn_reflns_theta_max         26.596
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8851
_reflns_number_gt                7202
_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 carbonyl oxygen of the lattice ethyl acetate was disordered in
two positions.  The two orientations were constratined to have equal 
thermal parameters and the relative occupancies were allowed to 
refine (the major occupancy refined to 0.605(8)).

 Hydrogen atoms on the ethyl acetate were placed in calculated positions,
with thermal parameters 1.5x (CH3) and 1.2x (CH2) the equivalent isotropic 
thermal parameters of the carbon atoms to which they are bonded.  All other
hydrogens were found on difference Fourier maps and refined isotropically.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0202P)²+6.5746P] 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_number_reflns         8851
_refine_ls_number_parameters     674
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0280
_refine_ls_wR_factor_ref         0.0605
_refine_ls_wR_factor_gt          0.0557
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_restrained_S_all      1.009
_refine_ls_shift/su_max          0.005
_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 0.94602(2) 0.95337(2) 0.85868(2) 0.00958(4) Uani 1 1 d . . . . .
O1 O 1.11963(19) 0.9618(2) 0.87332(6) 0.0127(5) Uani 1 1 d . . . . .
Cl1 Cl 0.97085(8) 1.14593(8) 0.82674(2) 0.01667(18) Uani 1 1 d . . . . .
N1 N 0.9994(2) 0.8471(3) 0.82056(7) 0.0112(6) Uani 1 1 d . . . . .
Cl2 Cl 0.74837(7) 0.96302(9) 0.83478(2) 0.01802(19) Uani 1 1 d . . . . .
O2 O 0.91156(19) 1.0467(2) 0.90482(6) 0.0130(5) Uani 1 1 d . . . . .
N2 N 0.9080(2) 0.8084(3) 0.88895(8) 0.0112(6) Uani 1 1 d . . . . .
C11 C 1.1794(3) 0.9252(3) 0.84707(9) 0.0130(7) Uani 1 1 d . . . . .
C12 C 1.1143(3) 0.8581(3) 0.81649(9) 0.0129(7) Uani 1 1 d . . . . .
C13 C 1.1693(3) 0.8041(4) 0.78775(10) 0.0157(8) Uani 1 1 d . . . . .
C14 C 1.2869(3) 0.8218(4) 0.78883(10) 0.0183(8) Uani 1 1 d . . . . .
C15 C 1.3499(3) 0.8894(4) 0.81994(11) 0.0212(9) Uani 1 1 d . . . . .
C16 C 1.3021(3) 0.9403(4) 0.84909(10) 0.0188(8) Uani 1 1 d . . . . .
C17 C 1.3732(3) 1.0128(4) 0.88135(11) 0.0246(9) Uani 1 1 d . . . . .
C18 C 1.3545(3) 0.7730(4) 0.75816(11) 0.0250(9) Uani 1 1 d . . . . .
C21 C 0.8530(3) 0.9758(3) 0.92542(9) 0.0104(7) Uani 1 1 d . . . . .
C22 C 0.8468(3) 0.8412(3) 0.91714(9) 0.0120(7) Uani 1 1 d . . . . .
C23 C 0.7874(3) 0.7557(4) 0.93812(10) 0.0140(8) Uani 1 1 d . . . . .
C24 C 0.7385(3) 0.8008(3) 0.96764(10) 0.0124(7) Uani 1 1 d . . . . .
C25 C 0.7497(3) 0.9353(3) 0.97634(9) 0.0128(7) Uani 1 1 d . . . . .
C26 C 0.8063(3) 1.0229(3) 0.95690(9) 0.0103(7) Uani 1 1 d . . . . .
C27 C 0.8206(3) 1.1660(3) 0.96789(9) 0.0128(7) Uani 1 1 d . . . . .
C28 C 0.6771(3) 0.7136(4) 0.99282(10) 0.0161(8) Uani 1 1 d . . . . .
C31 C 0.9230(3) 0.7603(3) 0.79819(10) 0.0134(7) Uani 1 1 d . . . . .
C32 C 0.8806(3) 0.6524(3) 0.81479(10) 0.0155(8) Uani 1 1 d . . . . .
C33 C 0.7992(4) 0.5754(4) 0.79217(11) 0.0241(9) Uani 1 1 d . . . . .
C34 C 0.7631(4) 0.6043(4) 0.75533(11) 0.0265(10) Uani 1 1 d . . . . .
C35 C 0.8068(4) 0.7116(4) 0.73954(11) 0.0245(9) Uani 1 1 d . . . . .
C36 C 0.8868(3) 0.7897(4) 0.76094(10) 0.0174(8) Uani 1 1 d . . . . .
C41 C 0.9440(3) 0.6763(3) 0.88628(10) 0.0141(8) Uani 1 1 d . . . . .
C42 C 0.9287(3) 0.6057(3) 0.85290(10) 0.0164(8) Uani 1 1 d . . . . .
C43 C 0.9621(4) 0.4752(4) 0.85575(12) 0.0243(9) Uani 1 1 d . . . . .
C44 C 1.0096(4) 0.4182(4) 0.88886(12) 0.0285(10) Uani 1 1 d . . . . .
C45 C 1.0297(4) 0.4924(4) 0.92074(12) 0.0256(10) Uani 1 1 d . . . . .
C46 C 0.9966(3) 0.6195(4) 0.91923(10) 0.0160(8) Uani 1 1 d . . . . .
C171 C 1.5044(4) 1.0050(6) 0.87923(16) 0.0441(14) Uani 1 1 d . . . . .
C172 C 1.3347(4) 1.1537(5) 0.87964(13) 0.0297(10) Uani 1 1 d . . . . .
C173 C 1.3543(4) 0.9531(5) 0.91867(11) 0.0281(9) Uani 1 1 d . . . . .
C181 C 1.2724(5) 0.7126(6) 0.72617(14) 0.0416(13) Uani 1 1 d . . . . .
C182 C 1.4192(6) 0.8855(6) 0.74349(17) 0.0531(17) Uani 1 1 d . . . . .
C183 C 1.4424(5) 0.6706(6) 0.77478(16) 0.0516(16) Uani 1 1 d . . . . .
C271 C 0.7605(4) 1.2508(4) 0.93621(12) 0.0206(8) Uani 1 1 d . . . . .
C272 C 0.9512(3) 1.1987(4) 0.97611(12) 0.0194(8) Uani 1 1 d . . . . .
C273 C 0.7678(4) 1.1959(4) 1.00333(12) 0.0209(9) Uani 1 1 d . . . . .
C281 C 0.6827(4) 0.5719(4) 0.98211(12) 0.0249(9) Uani 1 1 d . . . . .
C282 C 0.5486(3) 0.7532(5) 0.99073(13) 0.0258(10) Uani 1 1 d . . . . .
C283 C 0.7376(4) 0.7292(4) 1.03280(11) 0.0226(9) Uani 1 1 d . . . . .
O41 O 0.4259(8) 0.5347(13) 0.9142(3) 0.125(4) Uani 0.605(8) 1 d . . P A 1
O42 O 0.4700(12) 0.641(2) 0.8988(4) 0.125(4) Uani 0.395(8) 1 d . . P A 2
O32 O 0.4488(4) 0.4831(5) 0.85885(12) 0.0899(15) Uani 1 1 d . . . . .
C51 C 0.2728(5) 0.5740(6) 0.86924(19) 0.078(2) Uani 1 1 d . . . . .
H51A H 0.2588 0.5893 0.8423 0.117 Uiso 1 1 calc R U . . .
H51B H 0.2458 0.6491 0.8822 0.117 Uiso 1 1 calc R U . . .
H51C H 0.2296 0.4968 0.8751 0.117 Uiso 1 1 calc R U . . .
C52 C 0.3965(7) 0.5547(8) 0.8813(2) 0.089(2) Uani 1 1 d . . . . .
C53 C 0.5833(8) 0.4732(10) 0.86799(19) 0.127(4) Uani 1 1 d . . . . .
H53A H 0.6219 0.5531 0.8609 0.153 Uiso 1 1 calc R U . . .
H53B H 0.6086 0.4554 0.8948 0.153 Uiso 1 1 calc R U . . .
C54 C 0.6070(6) 0.3663(7) 0.84545(19) 0.086(2) Uani 1 1 d . . . . .
H54A H 0.6917 0.3501 0.8488 0.129 Uiso 1 1 calc R U . . .
H54B H 0.5792 0.3860 0.8192 0.129 Uiso 1 1 calc R U . . .
H54C H 0.5665 0.2892 0.8528 0.129 Uiso 1 1 calc R U . . .
H25 H 0.717(3) 0.965(3) 0.9986(9) 0.007(9) Uiso 1 1 d . . . . .
H28C H 0.641(3) 0.553(3) 0.9571(10) 0.011(9) Uiso 1 1 d . . . . .
H28I H 0.821(3) 0.707(4) 1.0348(10) 0.020(10) Uiso 1 1 d . . . . .
H28B H 0.767(4) 0.544(4) 0.9846(11) 0.031(12) Uiso 1 1 d . . . . .
H27C H 0.790(3) 1.232(4) 0.9122(11) 0.023(11) Uiso 1 1 d . . . . .
H46 H 1.009(3) 0.676(3) 0.9397(10) 0.008(9) Uiso 1 1 d . . . . .
H28A H 0.651(3) 0.520(3) 0.9995(10) 0.011(9) Uiso 1 1 d . . . . .
H27I H 0.683(3) 1.178(4) 0.9986(10) 0.021(10) Uiso 1 1 d . . . . .
H23 H 0.781(3) 0.676(4) 0.9316(10) 0.009(10) Uiso 1 1 d . . . . .
H17I H 1.277(3) 0.962(4) 0.9232(10) 0.016(10) Uiso 1 1 d . . . . .
H27B H 0.773(3) 1.340(4) 0.9415(10) 0.015(10) Uiso 1 1 d . . . . .
H17H H 1.403(4) 0.997(4) 0.9392(12) 0.028(11) Uiso 1 1 d . . . . .
H28H H 0.707(3) 0.668(4) 1.0492(10) 0.019(10) Uiso 1 1 d . . . . .
H27F H 0.988(3) 1.146(4) 0.9955(11) 0.023(11) Uiso 1 1 d . . . . .
H28G H 0.731(3) 0.811(4) 1.0426(11) 0.025(12) Uiso 1 1 d . . . . .
H27A H 0.669(4) 1.234(4) 0.9330(11) 0.025(11) Uiso 1 1 d . . . . .
H27E H 0.988(3) 1.189(4) 0.9554(11) 0.019(10) Uiso 1 1 d . . . . .
H45 H 1.068(3) 0.458(4) 0.9434(12) 0.029(11) Uiso 1 1 d . . . . .
H27H H 0.807(3) 1.147(4) 1.0255(11) 0.026(11) Uiso 1 1 d . . . . .
H27G H 0.777(3) 1.285(4) 1.0090(11) 0.023(11) Uiso 1 1 d . . . . .
H27D H 0.966(4) 1.286(5) 0.9844(12) 0.039(13) Uiso 1 1 d . . . . .
H15 H 1.429(3) 0.899(3) 0.8193(9) 0.009(9) Uiso 1 1 d . . . . .
H44 H 1.028(3) 0.336(4) 0.8872(11) 0.021(11) Uiso 1 1 d . . . . .
H28F H 0.539(4) 0.845(5) 0.9962(12) 0.035(13) Uiso 1 1 d . . . . .
H17F H 1.382(4) 1.203(4) 0.8997(12) 0.029(12) Uiso 1 1 d . . . . .
H17C H 1.519(4) 1.054(4) 0.8579(12) 0.029(12) Uiso 1 1 d . . . . .
H36 H 0.916(3) 0.863(3) 0.7517(9) 0.008(9) Uiso 1 1 d . . . . .
H28E H 0.513(4) 0.707(4) 1.0089(13) 0.040(13) Uiso 1 1 d . . . . .
H17E H 1.252(4) 1.166(4) 0.8827(11) 0.031(12) Uiso 1 1 d . . . . .
H13 H 1.121(3) 0.756(4) 0.7678(10) 0.016(10) Uiso 1 1 d . . . . .
H34 H 0.712(4) 0.555(4) 0.7410(12) 0.032(12) Uiso 1 1 d . . . . .
H17G H 1.377(4) 0.862(5) 0.9188(12) 0.036(12) Uiso 1 1 d . . . . .
H28D H 0.504(4) 0.737(5) 0.9671(15) 0.056(16) Uiso 1 1 d . . . . .
H17B H 1.541(4) 0.907(4) 0.8799(12) 0.039(13) Uiso 1 1 d . . . . .
H43 H 0.953(3) 0.425(4) 0.8340(11) 0.022(11) Uiso 1 1 d . . . . .
H17D H 1.347(3) 1.194(4) 0.8594(12) 0.026(12) Uiso 1 1 d . . . . .
H33 H 0.776(3) 0.499(4) 0.8026(11) 0.021(11) Uiso 1 1 d . . . . .
H17A H 1.546(4) 1.056(5) 0.9001(15) 0.061(16) Uiso 1 1 d . . . . .
H18D H 1.456(4) 0.859(4) 0.7239(13) 0.042(13) Uiso 1 1 d . . . . .
H35 H 0.784(3) 0.730(4) 0.7150(11) 0.021(11) Uiso 1 1 d . . . . .
H18G H 1.505(4) 0.703(5) 0.7971(14) 0.052(15) Uiso 1 1 d . . . . .
H18A H 1.236(4) 0.634(5) 0.7350(13) 0.047(15) Uiso 1 1 d . . . . .
H18E H 1.475(5) 0.926(5) 0.7630(15) 0.059(17) Uiso 1 1 d . . . . .
H18H H 1.482(5) 0.641(5) 0.7556(15) 0.067(17) Uiso 1 1 d . . . . .
H18B H 1.318(4) 0.687(5) 0.7069(14) 0.051(14) Uiso 1 1 d . . . . .
H18C H 1.218(5) 0.787(6) 0.7139(16) 0.07(2) Uiso 1 1 d . . . . .
H18I H 1.400(5) 0.590(6) 0.7846(16) 0.07(2) Uiso 1 1 d . . . . .
H18F H 1.353(5) 0.951(6) 0.7284(16) 0.073(19) 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 N1 1.935(3) . ?
Os N2 1.944(3) . ?
Os O1 1.996(2) . ?
Os O2 2.021(2) . ?
Os Cl2 2.3176(8) . ?
Os Cl1 2.3402(9) . ?
O1 C11 1.310(4) . ?
N1 C12 1.360(4) . ?
N1 C31 1.424(4) . ?
O2 C21 1.303(4) . ?
N2 C22 1.367(4) . ?
N2 C41 1.434(4) . ?
C11 C16 1.414(5) . ?
C11 C12 1.424(5) . ?
C12 C13 1.412(5) . ?
C13 C14 1.362(5) . ?
C13 H13 0.98(4) . ?
C14 C15 1.431(5) . ?
C14 C18 1.534(5) . ?
C15 C16 1.367(5) . ?
C15 H15 0.93(3) . ?
C16 C17 1.523(5) . ?
C17 C172 1.519(6) . ?
C17 C171 1.528(5) . ?
C17 C173 1.532(6) . ?
C18 C182 1.519(7) . ?
C18 C181 1.519(6) . ?
C18 C183 1.526(6) . ?
C21 C26 1.418(4) . ?
C21 C22 1.422(5) . ?
C22 C23 1.407(5) . ?
C23 C24 1.363(5) . ?
C23 H23 0.86(4) . ?
C24 C25 1.426(5) . ?
C24 C28 1.528(5) . ?
C25 C26 1.371(5) . ?
C25 H25 0.99(3) . ?
C26 C27 1.533(5) . ?
C27 C271 1.527(5) . ?
C27 C272 1.528(5) . ?
C27 C273 1.531(5) . ?
C28 C281 1.518(5) . ?
C28 C283 1.522(5) . ?
C28 C282 1.528(5) . ?
C31 C36 1.388(5) . ?
C31 C32 1.389(5) . ?
C32 C33 1.400(5) . ?
C32 C42 1.492(5) . ?
C33 C34 1.372(6) . ?
C33 H33 0.93(4) . ?
C34 C35 1.377(6) . ?
C34 H34 0.89(4) . ?
C35 C36 1.376(5) . ?
C35 H35 0.91(4) . ?
C36 H36 0.92(4) . ?
C41 C46 1.388(5) . ?
C41 C42 1.402(5) . ?
C42 C43 1.401(5) . ?
C43 C44 1.377(6) . ?
C43 H43 0.94(4) . ?
C44 C45 1.378(6) . ?
C44 H44 0.88(4) . ?
C45 C46 1.366(5) . ?
C45 H45 0.94(4) . ?
C46 H46 0.94(3) . ?
C171 H17C 0.96(4) . ?
C171 H17B 1.09(5) . ?
C171 H17A 0.99(5) . ?
C172 H17F 0.98(4) . ?
C172 H17E 0.98(4) . ?
C172 H17D 0.87(4) . ?
C173 H17I 0.94(4) . ?
C173 H17H 0.97(4) . ?
C173 H17G 0.98(5) . ?
C181 H18A 0.98(5) . ?
C181 H18B 0.97(5) . ?
C181 H18C 1.04(6) . ?
C182 H18D 0.92(5) . ?
C182 H18E 0.98(5) . ?
C182 H18F 1.10(6) . ?
C183 H18G 1.06(5) . ?
C183 H18H 0.94(6) . ?
C183 H18I 1.06(6) . ?
C271 H27C 1.00(4) . ?
C271 H27B 0.95(4) . ?
C271 H27A 1.06(4) . ?
C272 H27F 0.94(4) . ?
C272 H27E 0.92(4) . ?
C272 H27D 0.95(5) . ?
C273 H27I 0.99(4) . ?
C273 H27H 1.00(4) . ?
C273 H27G 0.94(4) . ?
C281 H28C 0.98(4) . ?
C281 H28B 1.01(4) . ?
C281 H28A 0.95(4) . ?
C282 H28F 0.98(5) . ?
C282 H28E 0.95(5) . ?
C282 H28D 0.95(5) . ?
C283 H28I 0.98(4) . ?
C283 H28H 0.97(4) . ?
C283 H28G 0.93(4) . ?
O41 C52 1.211(11) . ?
O42 C52 1.328(17) . ?
O32 C52 1.309(8) . ?
O32 C53 1.541(9) . ?
C51 C52 1.443(9) . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C53 C54 1.424(10) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Os N2 95.07(12) . . ?
N1 Os O1 78.64(10) . . ?
N2 Os O1 100.58(11) . . ?
N1 Os O2 169.79(10) . . ?
N2 Os O2 79.16(11) . . ?
O1 Os O2 94.04(9) . . ?
N1 Os Cl2 98.94(8) . . ?
N2 Os Cl2 87.33(8) . . ?
O1 Os Cl2 171.86(7) . . ?
O2 Os Cl2 89.26(7) . . ?
N1 Os Cl1 93.08(9) . . ?
N2 Os Cl1 171.12(8) . . ?
O1 Os Cl1 84.49(7) . . ?
O2 Os Cl1 93.29(7) . . ?
Cl2 Os Cl1 87.90(3) . . ?
C11 O1 Os 114.1(2) . . ?
C12 N1 C31 121.4(3) . . ?
C12 N1 Os 116.6(2) . . ?
C31 N1 Os 122.0(2) . . ?
C21 O2 Os 112.8(2) . . ?
C22 N2 C41 118.2(3) . . ?
C22 N2 Os 114.5(2) . . ?
C41 N2 Os 127.1(2) . . ?
O1 C11 C16 124.0(3) . . ?
O1 C11 C12 115.7(3) . . ?
C16 C11 C12 120.1(3) . . ?
N1 C12 C13 126.7(3) . . ?
N1 C12 C11 111.5(3) . . ?
C13 C12 C11 121.7(3) . . ?
C14 C13 C12 118.6(3) . . ?
C14 C13 H13 123(2) . . ?
C12 C13 H13 118(2) . . ?
C13 C14 C15 118.5(3) . . ?
C13 C14 C18 123.0(3) . . ?
C15 C14 C18 118.6(3) . . ?
C16 C15 C14 125.6(3) . . ?
C16 C15 H15 119(2) . . ?
C14 C15 H15 115(2) . . ?
C15 C16 C11 115.5(3) . . ?
C15 C16 C17 123.4(3) . . ?
C11 C16 C17 121.0(3) . . ?
C172 C17 C16 108.6(3) . . ?
C172 C17 C171 109.5(4) . . ?
C16 C17 C171 111.1(3) . . ?
C172 C17 C173 110.1(3) . . ?
C16 C17 C173 110.5(3) . . ?
C171 C17 C173 107.1(4) . . ?
C182 C18 C181 109.3(4) . . ?
C182 C18 C183 109.7(5) . . ?
C181 C18 C183 108.6(4) . . ?
C182 C18 C14 109.3(4) . . ?
C181 C18 C14 111.3(3) . . ?
C183 C18 C14 108.7(4) . . ?
O2 C21 C26 123.9(3) . . ?
O2 C21 C22 116.3(3) . . ?
C26 C21 C22 119.5(3) . . ?
N2 C22 C23 126.5(3) . . ?
N2 C22 C21 112.6(3) . . ?
C23 C22 C21 120.8(3) . . ?
C24 C23 C22 120.0(3) . . ?
C24 C23 H23 121(2) . . ?
C22 C23 H23 119(2) . . ?
C23 C24 C25 118.2(3) . . ?
C23 C24 C28 123.3(3) . . ?
C25 C24 C28 118.4(3) . . ?
C26 C25 C24 124.4(3) . . ?
C26 C25 H25 119(2) . . ?
C24 C25 H25 116(2) . . ?
C25 C26 C21 116.9(3) . . ?
C25 C26 C27 123.0(3) . . ?
C21 C26 C27 120.1(3) . . ?
C271 C27 C272 110.2(3) . . ?
C271 C27 C273 108.9(3) . . ?
C272 C27 C273 107.0(3) . . ?
C271 C27 C26 109.7(3) . . ?
C272 C27 C26 109.2(3) . . ?
C273 C27 C26 111.8(3) . . ?
C281 C28 C283 108.4(3) . . ?
C281 C28 C282 108.8(3) . . ?
C283 C28 C282 108.9(3) . . ?
C281 C28 C24 112.0(3) . . ?
C283 C28 C24 108.6(3) . . ?
C282 C28 C24 110.1(3) . . ?
C36 C31 C32 121.5(3) . . ?
C36 C31 N1 119.3(3) . . ?
C32 C31 N1 119.1(3) . . ?
C31 C32 C33 116.8(3) . . ?
C31 C32 C42 123.7(3) . . ?
C33 C32 C42 119.0(3) . . ?
C34 C33 C32 121.8(4) . . ?
C34 C33 H33 121(2) . . ?
C32 C33 H33 117(2) . . ?
C33 C34 C35 120.2(4) . . ?
C33 C34 H34 122(3) . . ?
C35 C34 H34 118(3) . . ?
C36 C35 C34 119.6(4) . . ?
C36 C35 H35 120(3) . . ?
C34 C35 H35 120(3) . . ?
C35 C36 C31 120.1(4) . . ?
C35 C36 H36 122(2) . . ?
C31 C36 H36 117(2) . . ?
C46 C41 C42 120.5(3) . . ?
C46 C41 N2 116.0(3) . . ?
C42 C41 N2 123.5(3) . . ?
C43 C42 C41 116.0(3) . . ?
C43 C42 C32 116.1(3) . . ?
C41 C42 C32 127.9(3) . . ?
C44 C43 C42 123.1(4) . . ?
C44 C43 H43 118(2) . . ?
C42 C43 H43 119(2) . . ?
C43 C44 C45 119.4(4) . . ?
C43 C44 H44 115(3) . . ?
C45 C44 H44 126(3) . . ?
C46 C45 C44 119.3(4) . . ?
C46 C45 H45 119(3) . . ?
C44 C45 H45 121(3) . . ?
C45 C46 C41 121.6(4) . . ?
C45 C46 H46 124(2) . . ?
C41 C46 H46 114(2) . . ?
C17 C171 H17C 108(3) . . ?
C17 C171 H17B 115(2) . . ?
H17C C171 H17B 113(3) . . ?
C17 C171 H17A 108(3) . . ?
H17C C171 H17A 102(4) . . ?
H17B C171 H17A 109(4) . . ?
C17 C172 H17F 110(2) . . ?
C17 C172 H17E 114(3) . . ?
H17F C172 H17E 107(3) . . ?
C17 C172 H17D 114(3) . . ?
H17F C172 H17D 103(4) . . ?
H17E C172 H17D 109(4) . . ?
C17 C173 H17I 112(2) . . ?
C17 C173 H17H 111(2) . . ?
H17I C173 H17H 106(3) . . ?
C17 C173 H17G 108(2) . . ?
H17I C173 H17G 111(3) . . ?
H17H C173 H17G 108(3) . . ?
C18 C181 H18A 109(3) . . ?
C18 C181 H18B 109(3) . . ?
H18A C181 H18B 108(4) . . ?
C18 C181 H18C 107(3) . . ?
H18A C181 H18C 119(4) . . ?
H18B C181 H18C 105(4) . . ?
C18 C182 H18D 110(3) . . ?
C18 C182 H18E 112(3) . . ?
H18D C182 H18E 111(4) . . ?
C18 C182 H18F 108(3) . . ?
H18D C182 H18F 99(4) . . ?
H18E C182 H18F 115(4) . . ?
C18 C183 H18G 115(3) . . ?
C18 C183 H18H 108(3) . . ?
H18G C183 H18H 109(4) . . ?
C18 C183 H18I 111(3) . . ?
H18G C183 H18I 107(4) . . ?
H18H C183 H18I 107(5) . . ?
C27 C271 H27C 111(2) . . ?
C27 C271 H27B 111(2) . . ?
H27C C271 H27B 108(3) . . ?
C27 C271 H27A 109(2) . . ?
H27C C271 H27A 109(3) . . ?
H27B C271 H27A 108(3) . . ?
C27 C272 H27F 110(2) . . ?
C27 C272 H27E 112(2) . . ?
H27F C272 H27E 110(3) . . ?
C27 C272 H27D 113(3) . . ?
H27F C272 H27D 106(3) . . ?
H27E C272 H27D 106(4) . . ?
C27 C273 H27I 109(2) . . ?
C27 C273 H27H 113(2) . . ?
H27I C273 H27H 112(3) . . ?
C27 C273 H27G 110(2) . . ?
H27I C273 H27G 107(3) . . ?
H27H C273 H27G 107(3) . . ?
C28 C281 H28C 114(2) . . ?
C28 C281 H28B 109(2) . . ?
H28C C281 H28B 111(3) . . ?
C28 C281 H28A 110(2) . . ?
H28C C281 H28A 108(3) . . ?
H28B C281 H28A 104(3) . . ?
C28 C282 H28F 113(3) . . ?
C28 C282 H28E 110(3) . . ?
H28F C282 H28E 106(4) . . ?
C28 C282 H28D 113(3) . . ?
H28F C282 H28D 107(4) . . ?
H28E C282 H28D 108(4) . . ?
C28 C283 H28I 111(2) . . ?
C28 C283 H28H 111(2) . . ?
H28I C283 H28H 104(3) . . ?
C28 C283 H28G 114(3) . . ?
H28I C283 H28G 109(3) . . ?
H28H C283 H28G 108(3) . . ?
C52 O32 C53 116.4(6) . . ?
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 . . ?
O41 C52 O32 115.4(8) . . ?
O32 C52 O42 111.0(10) . . ?
O41 C52 C51 116.2(8) . . ?
O32 C52 C51 114.5(6) . . ?
O42 C52 C51 125.7(10) . . ?
C54 C53 O32 101.6(7) . . ?
C54 C53 H53A 111.5 . . ?
O32 C53 H53A 111.5 . . ?
C54 C53 H53B 111.5 . . ?
O32 C53 H53B 111.5 . . ?
H53A C53 H53B 109.3 . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?

_refine_diff_density_max         1.196
_refine_diff_density_min         -0.969
_refine_diff_density_rms         0.110

_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_clipospy
_database_code_depnum_ccdc_archive 'CCDC 1994512'
loop_
_audit_author_name
_audit_author_address
'Seth Brown'
;University of Notre Dame
United States of America
;
_audit_update_record             
;
2020-04-02 deposited with the CCDC.	2020-04-29 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT094_clipospy            
;
PROBLEM: Ratio of Maximum / Minimum Residual Density ....       4.32 Report
RESPONSE: There are two large residual peaks on the final difference 
Fourier map within 1 A of the Os atom.  This may be due to unusually 
high mosaicity in the crystal.
;
_vrf_PLAT097_clipospy            
;
PROBLEM: Large Reported Max.  (Positive) Residual Density       8.85 eA-3  
RESPONSE: There are two large residual peaks on the final difference 
Fourier map within 1 A of the Os atom.  This may be due to unusually 
high mosaicity in the crystal.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
2,2'-Biphenylbis((2-oxy-3,5-di-tert-butylphenyl)amido)-bis(pyridine)osmium(IV)
_chemical_name_common            (Clip)Os(py)2
_chemical_melting_point          ?
_chemical_formula_moiety         'C50 H58 N4 O2 Os'
_chemical_formula_sum            'C50 H58 N4 O2 Os'
_chemical_formula_weight         937.20

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/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   9.870(7)
_cell_length_b                   23.816(19)
_cell_length_c                   19.126(14)
_cell_angle_alpha                90
_cell_angle_beta                 90.10(2)
_cell_angle_gamma                90
_cell_volume                     4496(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9021
_cell_measurement_theta_min      2.492
_cell_measurement_theta_max      28.162

_exptl_crystal_description       block
_exptl_crystal_colour            teal
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_F_000             1912
_exptl_transmission_factor_min   0.6282
_exptl_transmission_factor_max   0.7457
_exptl_crystal_size_max          0.309
_exptl_crystal_size_mid          0.104
_exptl_crystal_size_min          0.074
_exptl_absorpt_coefficient_mu    2.879
_shelx_estimated_absorpt_T_min   0.470
_shelx_estimated_absorpt_T_max   0.815
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.6282
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   
;
Blessing, R. H. (1995) Acta Cryst. A51, 33-38.

Sheldrick, G.M. (2008) SADABS v2008/1. Bruker AXS Inc.
Madison, WI USA.
;

_exptl_crystal_recrystallization_method 
'Crystals were grown by vapor diffusion of acetonitrileinto a solution of the compound in benzene.'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus 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            80737
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_av_R_equivalents  0.0611
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.710
_diffrn_reflns_theta_max         28.308
_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             11154
_reflns_number_gt                9598
_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)+(0.0490P)²+54.7625P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11154
_refine_ls_number_parameters     514
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0606
_refine_ls_wR_factor_ref         0.1544
_refine_ls_wR_factor_gt          0.1495
_refine_ls_goodness_of_fit_ref   1.219
_refine_ls_restrained_S_all      1.219
_refine_ls_shift/su_max          0.002
_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 0.75116(2) 0.99151(2) 0.25696(2) 0.01185(8) Uani 1 1 d . . . . .
O1 O 0.8205(5) 0.9348(2) 0.1850(3) 0.0216(10) Uani 1 1 d . . . . .
N1 N 0.8102(6) 0.9307(3) 0.3209(3) 0.0183(12) Uani 1 1 d . . . . .
O2 O 0.6847(5) 1.0476(2) 0.1830(3) 0.0207(10) Uani 1 1 d . . . . .
N2 N 0.6916(6) 1.0532(3) 0.3177(3) 0.0186(12) Uani 1 1 d . . . . .
N5 N 0.5544(6) 0.9578(3) 0.2537(3) 0.0218(12) Uani 1 1 d . . . . .
N6 N 0.9476(6) 1.0256(3) 0.2536(3) 0.0201(12) Uani 1 1 d . . . . .
C11 C 0.8949(7) 0.8938(3) 0.2136(4) 0.0198(14) Uani 1 1 d . . . . .
C12 C 0.8889(7) 0.8891(3) 0.2883(4) 0.0204(14) Uani 1 1 d . . . . .
C13 C 0.9546(7) 0.8441(3) 0.3219(4) 0.0235(15) Uani 1 1 d . . . . .
H13 H 0.9509 0.8411 0.3714 0.028 Uiso 1 1 calc R U . . .
C14 C 1.0246(7) 0.8043(3) 0.2837(4) 0.0235(15) Uani 1 1 d . . . . .
C15 C 1.0312(7) 0.8099(3) 0.2110(4) 0.0241(15) Uani 1 1 d . . . . .
H15 H 1.0790 0.7823 0.1850 0.029 Uiso 1 1 calc R U . . .
C16 C 0.9709(7) 0.8544(3) 0.1748(4) 0.0214(14) Uani 1 1 d . . . . .
C17 C 0.9853(8) 0.8620(4) 0.0944(4) 0.0289(17) Uani 1 1 d . . . . .
C18 C 1.0931(9) 0.7542(4) 0.3222(5) 0.0348(19) Uani 1 1 d . . . . .
C21 C 0.6091(7) 1.0885(3) 0.2104(4) 0.0201(14) Uani 1 1 d . . . . .
C22 C 0.6125(7) 1.0950(3) 0.2849(4) 0.0207(14) Uani 1 1 d . . . . .
C23 C 0.5442(8) 1.1391(3) 0.3168(4) 0.0261(16) Uani 1 1 d . . . . .
H23 H 0.5453 1.1421 0.3663 0.031 Uiso 1 1 calc R U . . .
C24 C 0.4738(8) 1.1792(3) 0.2773(4) 0.0259(16) Uani 1 1 d . . . . .
C25 C 0.4692(8) 1.1718(3) 0.2041(4) 0.0249(15) Uani 1 1 d . . . . .
H25 H 0.4200 1.1984 0.1770 0.030 Uiso 1 1 calc R U . . .
C26 C 0.5335(7) 1.1273(3) 0.1692(4) 0.0213(14) Uani 1 1 d . . . . .
C27 C 0.5227(8) 1.1183(4) 0.0892(4) 0.0270(16) Uani 1 1 d . . . . .
C28 C 0.4001(9) 1.2278(4) 0.3139(5) 0.036(2) Uani 1 1 d . . . . .
C31 C 0.7155(10) 0.9639(4) 0.4317(4) 0.035(2) Uani 1 1 d . . . . .
C32 C 0.7390(8) 0.9197(3) 0.3824(4) 0.0228(15) Uani 1 1 d . . . . .
C33 C 0.6779(10) 0.8669(4) 0.3933(5) 0.038(2) Uani 1 1 d . . . . .
H33 H 0.6978 0.8371 0.3619 0.046 Uiso 1 1 calc R U . . .
C34 C 0.5899(13) 0.8570(5) 0.4481(7) 0.064(4) Uani 1 1 d . . . . .
H34 H 0.5468 0.8215 0.4528 0.077 Uiso 1 1 calc R U . . .
C35 C 0.5649(17) 0.8993(6) 0.4963(7) 0.083(5) Uani 1 1 d . . . . .
H35 H 0.5055 0.8928 0.5345 0.100 Uiso 1 1 calc R U . . .
C36 C 0.6258(13) 0.9500(5) 0.4886(5) 0.057(3) Uani 1 1 d . . . . .
H36 H 0.6084 0.9781 0.5228 0.068 Uiso 1 1 calc R U . . .
C41 C 0.7712(10) 1.0208(4) 0.4328(4) 0.033(2) Uani 1 1 d . . . . .
C42 C 0.7566(8) 1.0645(3) 0.3826(4) 0.0217(14) Uani 1 1 d . . . . .
C43 C 0.8139(10) 1.1178(4) 0.3950(5) 0.040(2) Uani 1 1 d . . . . .
H43 H 0.8007 1.1470 0.3620 0.048 Uiso 1 1 calc R U . . .
C44 C 0.8911(14) 1.1283(5) 0.4562(6) 0.064(4) Uani 1 1 d . . . . .
H44 H 0.9314 1.1640 0.4637 0.077 Uiso 1 1 calc R U . . .
C45 C 0.9065(15) 1.0865(5) 0.5040(6) 0.069(4) Uani 1 1 d . . . . .
H45 H 0.9563 1.0936 0.5456 0.083 Uiso 1 1 calc R U . . .
C46 C 0.8517(13) 1.0344(5) 0.4934(5) 0.053(3) Uani 1 1 d . . . . .
H46 H 0.8675 1.0060 0.5274 0.064 Uiso 1 1 calc R U . . .
C52 C 0.4700(9) 0.9581(4) 0.3081(5) 0.038(2) Uani 1 1 d . . . . .
H52 H 0.4973 0.9763 0.3500 0.046 Uiso 1 1 calc R U . . .
C53 C 0.3427(9) 0.9325(5) 0.3055(6) 0.049(3) Uani 1 1 d . . . . .
H53 H 0.2857 0.9325 0.3455 0.059 Uiso 1 1 calc R U . . .
C54 C 0.3009(10) 0.9075(4) 0.2450(6) 0.048(3) Uani 1 1 d . . . . .
H54 H 0.2142 0.8903 0.2420 0.057 Uiso 1 1 calc R U . . .
C55 C 0.3872(10) 0.9076(5) 0.1883(6) 0.051(3) Uani 1 1 d . . . . .
H55 H 0.3602 0.8907 0.1455 0.061 Uiso 1 1 calc R U . . .
C56 C 0.5145(9) 0.9327(4) 0.1943(5) 0.037(2) Uani 1 1 d . . . . .
H56 H 0.5743 0.9320 0.1554 0.045 Uiso 1 1 calc R U . . .
C62 C 1.0332(9) 1.0257(4) 0.3098(5) 0.0356(19) Uani 1 1 d . . . . .
H62 H 1.0051 1.0085 0.3522 0.043 Uiso 1 1 calc R U . . .
C63 C 1.1621(10) 1.0507(5) 0.3063(6) 0.049(3) Uani 1 1 d . . . . .
H63 H 1.2179 1.0522 0.3468 0.059 Uiso 1 1 calc R U . . .
C64 C 1.2070(10) 1.0730(4) 0.2449(6) 0.046(2) Uani 1 1 d . . . . .
H64 H 1.2949 1.0890 0.2414 0.055 Uiso 1 1 calc R U . . .
C65 C 1.1207(9) 1.0715(4) 0.1876(6) 0.043(2) Uani 1 1 d . . . . .
H65 H 1.1487 1.0866 0.1439 0.051 Uiso 1 1 calc R U . . .
C66 C 0.9921(8) 1.0476(4) 0.1948(5) 0.0340(19) Uani 1 1 d . . . . .
H66 H 0.9338 1.0473 0.1552 0.041 Uiso 1 1 calc R U . . .
C171 C 1.0771(10) 0.8158(4) 0.0628(5) 0.039(2) Uani 1 1 d . . . . .
H17A H 1.0388 0.7788 0.0733 0.059 Uiso 1 1 calc R U . . .
H17B H 1.1681 0.8186 0.0830 0.059 Uiso 1 1 calc R U . . .
H17C H 1.0823 0.8208 0.0120 0.059 Uiso 1 1 calc R U . . .
C172 C 1.0482(10) 0.9197(4) 0.0772(5) 0.0355(19) Uani 1 1 d . . . . .
H17D H 0.9916 0.9496 0.0969 0.053 Uiso 1 1 calc R U . . .
H17E H 1.0537 0.9243 0.0263 0.053 Uiso 1 1 calc R U . . .
H17F H 1.1394 0.9220 0.0974 0.053 Uiso 1 1 calc R U . . .
C173 C 0.8438(9) 0.8576(5) 0.0582(4) 0.038(2) Uani 1 1 d . . . . .
H17G H 0.7837 0.8867 0.0769 0.057 Uiso 1 1 calc R U . . .
H17H H 0.8048 0.8205 0.0674 0.057 Uiso 1 1 calc R U . . .
H17I H 0.8542 0.8629 0.0077 0.057 Uiso 1 1 calc R U . . .
C181 C 1.1476(11) 0.7094(4) 0.2717(5) 0.044(2) Uani 1 1 d . . . . .
H18A H 1.1903 0.6791 0.2985 0.065 Uiso 1 1 calc R U . . .
H18B H 1.2147 0.7264 0.2405 0.065 Uiso 1 1 calc R U . . .
H18C H 1.0727 0.6941 0.2439 0.065 Uiso 1 1 calc R U . . .
C182 C 1.2131(13) 0.7770(5) 0.3662(7) 0.063(4) Uani 1 1 d . . . . .
H18D H 1.1801 0.8059 0.3984 0.095 Uiso 1 1 calc R U . . .
H18E H 1.2812 0.7933 0.3350 0.095 Uiso 1 1 calc R U . . .
H18F H 1.2537 0.7462 0.3929 0.095 Uiso 1 1 calc R U . . .
C183 C 0.9887(11) 0.7240(4) 0.3695(5) 0.046(2) Uani 1 1 d . . . . .
H18G H 0.9501 0.7510 0.4027 0.069 Uiso 1 1 calc R U . . .
H18H H 1.0338 0.6937 0.3953 0.069 Uiso 1 1 calc R U . . .
H18I H 0.9161 0.7082 0.3405 0.069 Uiso 1 1 calc R U . . .
C271 C 0.4555(9) 1.0621(4) 0.0730(5) 0.0361(19) Uani 1 1 d . . . . .
H27A H 0.5077 1.0317 0.0948 0.054 Uiso 1 1 calc R U . . .
H27B H 0.4525 1.0564 0.0223 0.054 Uiso 1 1 calc R U . . .
H27C H 0.3631 1.0619 0.0916 0.054 Uiso 1 1 calc R U . . .
C272 C 0.6653(9) 1.1199(5) 0.0553(4) 0.039(2) Uani 1 1 d . . . . .
H27D H 0.7086 1.1560 0.0655 0.058 Uiso 1 1 calc R U . . .
H27E H 0.6567 1.1152 0.0046 0.058 Uiso 1 1 calc R U . . .
H27F H 0.7208 1.0894 0.0744 0.058 Uiso 1 1 calc R U . . .
C273 C 0.4398(11) 1.1657(4) 0.0550(5) 0.043(2) Uani 1 1 d . . . . .
H27G H 0.4822 1.2019 0.0654 0.065 Uiso 1 1 calc R U . . .
H27H H 0.3473 1.1652 0.0736 0.065 Uiso 1 1 calc R U . . .
H27I H 0.4371 1.1600 0.0043 0.065 Uiso 1 1 calc R U . . .
C281 C 0.3578(11) 1.2748(4) 0.2628(5) 0.045(2) Uani 1 1 d . . . . .
H28A H 0.2980 1.2593 0.2267 0.068 Uiso 1 1 calc R U . . .
H28B H 0.4388 1.2907 0.2407 0.068 Uiso 1 1 calc R U . . .
H28C H 0.3100 1.3044 0.2885 0.068 Uiso 1 1 calc R U . . .
C282 C 0.4911(12) 1.2551(5) 0.3685(6) 0.052(3) Uani 1 1 d . . . . .
H28D H 0.5201 1.2268 0.4025 0.079 Uiso 1 1 calc R U . . .
H28E H 0.4410 1.2849 0.3926 0.079 Uiso 1 1 calc R U . . .
H28F H 0.5708 1.2712 0.3455 0.079 Uiso 1 1 calc R U . . .
C283 C 0.2677(12) 1.2043(5) 0.3477(6) 0.056(3) Uani 1 1 d . . . . .
H28G H 0.2109 1.1872 0.3114 0.084 Uiso 1 1 calc R U . . .
H28H H 0.2180 1.2350 0.3701 0.084 Uiso 1 1 calc R U . . .
H28I H 0.2913 1.1759 0.3828 0.084 Uiso 1 1 calc R U . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Os N2 1.963(6) . ?
Os N1 1.982(6) . ?
Os O1 2.046(5) . ?
Os O2 2.053(5) . ?
Os N5 2.102(6) . ?
Os N6 2.104(6) . ?
O1 C11 1.339(9) . ?
N1 C32 1.396(9) . ?
N1 C12 1.404(9) . ?
O2 C21 1.335(9) . ?
N2 C22 1.412(9) . ?
N2 C42 1.422(9) . ?
N5 C52 1.334(11) . ?
N5 C56 1.342(10) . ?
N6 C66 1.317(10) . ?
N6 C62 1.366(10) . ?
C11 C16 1.413(10) . ?
C11 C12 1.433(10) . ?
C12 C13 1.406(10) . ?
C13 C14 1.384(10) . ?
C14 C15 1.398(11) . ?
C14 C18 1.555(11) . ?
C15 C16 1.398(11) . ?
C16 C17 1.556(10) . ?
C17 C172 1.544(12) . ?
C17 C171 1.549(12) . ?
C17 C173 1.561(11) . ?
C18 C181 1.538(12) . ?
C18 C182 1.549(14) . ?
C18 C183 1.551(14) . ?
C21 C26 1.424(10) . ?
C21 C22 1.433(10) . ?
C22 C23 1.390(10) . ?
C23 C24 1.401(10) . ?
C24 C25 1.411(11) . ?
C24 C28 1.538(11) . ?
C25 C26 1.404(11) . ?
C26 C27 1.550(10) . ?
C27 C271 1.526(12) . ?
C27 C273 1.538(12) . ?
C27 C272 1.552(11) . ?
C28 C282 1.522(14) . ?
C28 C281 1.543(13) . ?
C28 C283 1.563(14) . ?
C31 C32 1.432(11) . ?
C31 C36 1.443(13) . ?
C31 C41 1.464(13) . ?
C32 C33 1.411(12) . ?
C33 C34 1.383(13) . ?
C34 C35 1.389(19) . ?
C35 C36 1.357(19) . ?
C41 C42 1.422(11) . ?
C41 C46 1.441(13) . ?
C42 C43 1.411(13) . ?
C43 C44 1.417(13) . ?
C44 C45 1.361(18) . ?
C45 C46 1.368(18) . ?
C52 C53 1.398(13) . ?
C53 C54 1.364(16) . ?
C54 C55 1.380(16) . ?
C55 C56 1.396(12) . ?
C62 C63 1.406(12) . ?
C63 C64 1.364(15) . ?
C64 C65 1.387(15) . ?
C65 C66 1.398(12) . ?

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
N2 Os N1 105.7(2) . . ?
N2 Os O1 172.8(2) . . ?
N1 Os O1 80.4(2) . . ?
N2 Os O2 79.9(2) . . ?
N1 Os O2 173.6(2) . . ?
O1 Os O2 94.2(2) . . ?
N2 Os N5 91.5(2) . . ?
N1 Os N5 90.6(2) . . ?
O1 Os N5 92.2(2) . . ?
O2 Os N5 86.2(2) . . ?
N2 Os N6 90.3(2) . . ?
N1 Os N6 91.8(2) . . ?
O1 Os N6 85.7(2) . . ?
O2 Os N6 91.2(2) . . ?
N5 Os N6 176.6(2) . . ?
C11 O1 Os 113.0(4) . . ?
C32 N1 C12 121.4(6) . . ?
C32 N1 Os 120.6(5) . . ?
C12 N1 Os 113.8(4) . . ?
C21 O2 Os 112.5(4) . . ?
C22 N2 C42 120.2(6) . . ?
C22 N2 Os 115.5(5) . . ?
C42 N2 Os 121.5(5) . . ?
C52 N5 C56 118.7(7) . . ?
C52 N5 Os 123.6(6) . . ?
C56 N5 Os 117.7(6) . . ?
C66 N6 C62 117.7(7) . . ?
C66 N6 Os 119.2(5) . . ?
C62 N6 Os 123.1(5) . . ?
O1 C11 C16 124.2(6) . . ?
O1 C11 C12 116.1(6) . . ?
C16 C11 C12 119.6(7) . . ?
N1 C12 C13 126.1(6) . . ?
N1 C12 C11 114.2(6) . . ?
C13 C12 C11 119.7(6) . . ?
C14 C13 C12 120.8(7) . . ?
C13 C14 C15 118.9(7) . . ?
C13 C14 C18 119.5(7) . . ?
C15 C14 C18 121.6(7) . . ?
C16 C15 C14 123.0(7) . . ?
C15 C16 C11 118.0(7) . . ?
C15 C16 C17 122.6(7) . . ?
C11 C16 C17 119.4(7) . . ?
C172 C17 C171 108.3(7) . . ?
C172 C17 C16 110.6(7) . . ?
C171 C17 C16 110.9(7) . . ?
C172 C17 C173 109.0(7) . . ?
C171 C17 C173 107.6(7) . . ?
C16 C17 C173 110.3(6) . . ?
C181 C18 C182 108.4(8) . . ?
C181 C18 C183 106.1(8) . . ?
C182 C18 C183 110.7(9) . . ?
C181 C18 C14 112.8(7) . . ?
C182 C18 C14 108.7(8) . . ?
C183 C18 C14 110.1(7) . . ?
O2 C21 C26 123.3(6) . . ?
O2 C21 C22 117.2(6) . . ?
C26 C21 C22 119.4(7) . . ?
C23 C22 N2 127.3(6) . . ?
C23 C22 C21 120.5(7) . . ?
N2 C22 C21 112.2(6) . . ?
C22 C23 C24 121.2(7) . . ?
C23 C24 C25 117.8(7) . . ?
C23 C24 C28 120.1(7) . . ?
C25 C24 C28 122.0(7) . . ?
C26 C25 C24 123.4(7) . . ?
C25 C26 C21 117.7(6) . . ?
C25 C26 C27 122.9(6) . . ?
C21 C26 C27 119.4(7) . . ?
C271 C27 C273 109.1(7) . . ?
C271 C27 C26 110.5(6) . . ?
C273 C27 C26 110.7(7) . . ?
C271 C27 C272 109.3(7) . . ?
C273 C27 C272 106.7(7) . . ?
C26 C27 C272 110.4(6) . . ?
C282 C28 C24 110.8(7) . . ?
C282 C28 C281 106.5(9) . . ?
C24 C28 C281 112.7(7) . . ?
C282 C28 C283 111.2(9) . . ?
C24 C28 C283 108.3(8) . . ?
C281 C28 C283 107.3(8) . . ?
C32 C31 C36 115.5(9) . . ?
C32 C31 C41 129.0(8) . . ?
C36 C31 C41 115.5(8) . . ?
N1 C32 C33 120.5(7) . . ?
N1 C32 C31 120.0(7) . . ?
C33 C32 C31 119.2(7) . . ?
C34 C33 C32 122.2(10) . . ?
C33 C34 C35 119.5(12) . . ?
C36 C35 C34 119.7(10) . . ?
C35 C36 C31 123.9(10) . . ?
C42 C41 C46 115.8(9) . . ?
C42 C41 C31 129.0(7) . . ?
C46 C41 C31 115.3(8) . . ?
C43 C42 N2 119.9(7) . . ?
C43 C42 C41 120.2(7) . . ?
N2 C42 C41 119.8(7) . . ?
C42 C43 C44 121.0(10) . . ?
C45 C44 C43 118.9(11) . . ?
C44 C45 C46 121.4(10) . . ?
C45 C46 C41 122.6(10) . . ?
N5 C52 C53 122.2(9) . . ?
C54 C53 C52 119.4(10) . . ?
C53 C54 C55 118.6(9) . . ?
C54 C55 C56 119.5(10) . . ?
N5 C56 C55 121.5(9) . . ?
N6 C62 C63 121.4(9) . . ?
C64 C63 C62 120.1(10) . . ?
C63 C64 C65 118.1(9) . . ?
C64 C65 C66 119.2(9) . . ?
N6 C66 C65 123.4(9) . . ?

_refine_diff_density_max         8.846
_refine_diff_density_min         -2.047
_refine_diff_density_rms         0.207

_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_meclampos
_database_code_depnum_ccdc_archive 'CCDC 1994513'
loop_
_audit_author_name
_audit_author_address
'Seth Brown'
;University of Notre Dame
United States of America
;
_audit_update_record             
;
2020-04-02 deposited with the CCDC.	2020-04-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 [Tris(2-(3',5'-di-tert-butyl-2'-oxyphenyl)amido-4-
methylphenyl)amine]osmium(VI)
;
_chemical_name_common            (MeClamp)Os
_chemical_melting_point          ?
_chemical_formula_moiety         'C63 H78 N4 O3 Os'
_chemical_formula_sum            'C63 H78 N4 O3 Os'
_chemical_formula_weight         1129.49

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                   12.2048(11)
_cell_length_b                   28.050(3)
_cell_length_c                   17.3586(16)
_cell_angle_alpha                90
_cell_angle_beta                 92.9257(13)
_cell_angle_gamma                90
_cell_volume                     5934.9(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9767
_cell_measurement_theta_min      4.919
_cell_measurement_theta_max      56.522

_exptl_crystal_description       block
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_F_000             2336
_exptl_transmission_factor_min   0.7157
_exptl_transmission_factor_max   0.8621
_exptl_crystal_size_max          0.327
_exptl_crystal_size_mid          0.179
_exptl_crystal_size_min          0.108
_exptl_absorpt_coefficient_mu    2.189
_shelx_estimated_absorpt_T_min   0.7157
_shelx_estimated_absorpt_T_max   0.8621
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.7157
_exptl_absorpt_correction_T_max  0.8621
_exptl_absorpt_process_details   
;
Blessing, R. H. (1995) Acta Cryst. A51, 33-38.

Sheldrick, G.M. (2008) SADABS v2008/1. Bruker AXS Inc.
Madison, WI USA.
;

_exptl_crystal_recrystallization_method 
;
 Crystals were grown by diffusion of acetonitrile into
a dichloromethane 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            159593
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_av_R_equivalents  0.0932
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.381
_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             14762
_reflns_number_gt                11650
_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          
;
 All hydrogen atoms were found on difference Fourier maps and
their positions were allowed to refine freely.  In all but one
case, their isotropic thermal parameters were also refined, but
the thermal parameter H25 consistently failed to refine 
satisfactorily, and was fixed to 1.2x the equivalent isotropic
thermal parameter of C25 (to which it is bonded).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0289P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         14762
_refine_ls_number_parameters     951
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0297
_refine_ls_wR_factor_ref         0.0573
_refine_ls_wR_factor_gt          0.0536
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_restrained_S_all      1.002
_refine_ls_shift/su_max          0.002
_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 0.33884(2) 0.19711(2) 0.33762(2) 0.01446(3) Uani 1 1 d . . . . .
O1 O 0.36985(12) 0.18762(5) 0.22838(8) 0.0171(3) Uani 1 1 d . . . . .
O2 O 0.26695(12) 0.25912(6) 0.30725(9) 0.0178(3) Uani 1 1 d . . . . .
O3 O 0.20303(13) 0.15653(6) 0.32331(8) 0.0177(3) Uani 1 1 d . . . . .
N1 N 0.43098(15) 0.13796(7) 0.34447(10) 0.0164(4) Uani 1 1 d . . . . .
N2 N 0.45840(15) 0.24218(7) 0.36409(10) 0.0150(4) Uani 1 1 d . . . . .
N3 N 0.28570(14) 0.19464(7) 0.44341(10) 0.0140(4) Uani 1 1 d . . . . .
N10 N 0.50663(15) 0.17883(7) 0.48913(10) 0.0153(4) Uani 1 1 d . . . . .
C11 C 0.42291(18) 0.14812(8) 0.21125(12) 0.0158(5) Uani 1 1 d . . . . .
C12 C 0.46045(18) 0.11961(8) 0.27464(12) 0.0164(5) Uani 1 1 d . . . . .
C13 C 0.52376(19) 0.07884(9) 0.26241(13) 0.0187(5) Uani 1 1 d . . . . .
C14 C 0.54525(19) 0.06546(8) 0.18840(13) 0.0186(5) Uani 1 1 d . . . . .
C15 C 0.50312(19) 0.09387(9) 0.12591(13) 0.0210(5) Uani 1 1 d . . . . .
C16 C 0.44206(18) 0.13489(9) 0.13486(12) 0.0185(5) Uani 1 1 d . . . . .
C17 C 0.3965(2) 0.16564(10) 0.06728(13) 0.0253(6) Uani 1 1 d . . . . .
C18 C 0.6150(2) 0.02169(9) 0.17083(13) 0.0236(5) Uani 1 1 d . . . . .
C21 C 0.32542(18) 0.29780(8) 0.32556(11) 0.0148(4) Uani 1 1 d . . . . .
C22 C 0.43130(19) 0.28991(8) 0.36055(12) 0.0171(5) Uani 1 1 d . . . . .
C23 C 0.4945(2) 0.32779(9) 0.38989(13) 0.0184(5) Uani 1 1 d . . . . .
C24 C 0.4569(2) 0.37412(9) 0.38110(13) 0.0209(5) Uani 1 1 d . . . . .
C25 C 0.3555(2) 0.38173(10) 0.33983(14) 0.0236(5) Uani 1 1 d . . . . .
H25 H 0.330(2) 0.4105(11) 0.3337(14) 0.028 Uiso 1 1 d . U . . .
C26 C 0.28816(18) 0.34492(9) 0.31077(13) 0.0177(5) Uani 1 1 d . . . . .
C27 C 0.1797(2) 0.35419(9) 0.26457(15) 0.0247(5) Uani 1 1 d . . . . .
C28 C 0.5223(2) 0.41497(9) 0.41944(14) 0.0265(6) Uani 1 1 d . . . . .
C31 C 0.15382(18) 0.14457(8) 0.38684(12) 0.0167(5) Uani 1 1 d . . . . .
C32 C 0.19682(18) 0.16594(8) 0.45570(12) 0.0160(5) Uani 1 1 d . . . . .
C33 C 0.15481(19) 0.15559(9) 0.52698(13) 0.0196(5) Uani 1 1 d . . . . .
C34 C 0.06904(19) 0.12415(9) 0.53122(13) 0.0211(5) Uani 1 1 d . . . . .
C35 C 0.0278(2) 0.10259(9) 0.46201(14) 0.0225(5) Uani 1 1 d . . . . .
C36 C 0.06729(19) 0.11124(8) 0.38989(13) 0.0191(5) Uani 1 1 d . . . . .
C37 C 0.0267(2) 0.08409(9) 0.31713(14) 0.0240(5) Uani 1 1 d . . . . .
C38 C 0.0267(2) 0.11187(10) 0.61061(14) 0.0266(6) Uani 1 1 d . . . . .
C111 C 0.46320(18) 0.13216(8) 0.48450(13) 0.0166(5) Uani 1 1 d . . . . .
C112 C 0.43549(18) 0.11000(8) 0.41327(12) 0.0163(5) Uani 1 1 d . . . . .
C113 C 0.39470(19) 0.06366(9) 0.41260(13) 0.0183(5) Uani 1 1 d . . . . .
C114 C 0.37505(19) 0.03914(9) 0.47992(14) 0.0209(5) Uani 1 1 d . . . . .
C115 C 0.3989(2) 0.06211(9) 0.54978(14) 0.0233(5) Uani 1 1 d . . . . .
C116 C 0.44317(19) 0.10758(9) 0.55207(13) 0.0213(5) Uani 1 1 d . . . . .
C117 C 0.3254(3) -0.01005(11) 0.4777(2) 0.0305(6) Uani 1 1 d . . . . .
C171 C 0.2707(2) 0.16785(12) 0.06957(17) 0.0331(7) Uani 1 1 d . . . . .
C172 C 0.4249(3) 0.14429(15) -0.00994(16) 0.0455(9) Uani 1 1 d . . . . .
C173 C 0.4439(3) 0.21617(12) 0.07325(18) 0.0363(7) Uani 1 1 d . . . . .
C181 C 0.7210(3) 0.03824(12) 0.1357(2) 0.0379(7) Uani 1 1 d . . . . .
C182 C 0.6451(3) -0.00754(11) 0.24334(17) 0.0308(6) Uani 1 1 d . . . . .
C183 C 0.5513(3) -0.01124(11) 0.11417(18) 0.0367(7) Uani 1 1 d . . . . .
C211 C 0.59042(18) 0.19343(8) 0.44026(12) 0.0169(5) Uani 1 1 d . . . . .
C212 C 0.56904(18) 0.22819(8) 0.38318(12) 0.0155(5) Uani 1 1 d . . . . .
C213 C 0.6543(2) 0.24570(9) 0.34110(14) 0.0205(5) Uani 1 1 d . . . . .
C214 C 0.76038(19) 0.22844(9) 0.35294(14) 0.0230(5) Uani 1 1 d . . . . .
C215 C 0.7798(2) 0.19253(10) 0.40695(15) 0.0257(6) Uani 1 1 d . . . . .
C216 C 0.6961(2) 0.17539(9) 0.45036(14) 0.0219(5) Uani 1 1 d . . . . .
C217 C 0.8523(3) 0.24876(14) 0.3077(2) 0.0346(7) Uani 1 1 d . . . . .
C271 C 0.0844(3) 0.33325(14) 0.3066(2) 0.0463(9) Uani 1 1 d . . . . .
C272 C 0.1584(3) 0.40746(11) 0.2521(2) 0.0343(7) Uani 1 1 d . . . . .
C273 C 0.1858(3) 0.33078(12) 0.18478(17) 0.0352(7) Uani 1 1 d . . . . .
C281 C 0.5091(3) 0.41168(13) 0.50713(17) 0.0400(7) Uani 1 1 d . . . . .
C282 C 0.6445(2) 0.41032(11) 0.40386(18) 0.0311(6) Uani 1 1 d . . . . .
C283 C 0.4842(3) 0.46349(11) 0.3902(2) 0.0434(8) Uani 1 1 d . . . . .
C311 C 0.44664(18) 0.21598(8) 0.52408(12) 0.0154(5) Uani 1 1 d . . . . .
C312 C 0.33484(18) 0.22207(8) 0.50513(12) 0.0155(5) Uani 1 1 d . . . . .
C313 C 0.2761(2) 0.25812(9) 0.53843(14) 0.0208(5) Uani 1 1 d . . . . .
C314 C 0.3267(2) 0.28990(9) 0.59027(14) 0.0237(5) Uani 1 1 d . . . . .
C315 C 0.4388(2) 0.28450(9) 0.60677(14) 0.0236(5) Uani 1 1 d . . . . .
C316 C 0.4979(2) 0.24796(9) 0.57505(13) 0.0199(5) Uani 1 1 d . . . . .
C317 C 0.2621(3) 0.32946(13) 0.6247(2) 0.0418(8) Uani 1 1 d . . . . .
C371 C 0.1207(3) 0.05372(11) 0.28898(18) 0.0324(7) Uani 1 1 d . . . . .
C372 C -0.0695(3) 0.05119(12) 0.33237(18) 0.0350(7) Uani 1 1 d . . . . .
C373 C -0.0108(3) 0.11923(11) 0.25358(17) 0.0313(7) Uani 1 1 d . . . . .
C381 C -0.0742(2) 0.07944(12) 0.60508(18) 0.0342(7) Uani 1 1 d . . . . .
C382 C 0.1182(3) 0.08512(14) 0.65730(18) 0.0416(8) Uani 1 1 d . . . . .
C383 C -0.0014(3) 0.15734(13) 0.6532(2) 0.0450(8) Uani 1 1 d . . . . .
H27H H 0.1968(18) 0.2942(8) 0.1877(12) 0.007(5) Uiso 1 1 d . . . . .
H113 H 0.3761(18) 0.0501(8) 0.3674(13) 0.010(6) Uiso 1 1 d . . . . .
H213 H 0.6385(18) 0.2688(9) 0.3044(13) 0.014(6) Uiso 1 1 d . . . . .
H315 H 0.476(2) 0.3049(9) 0.6398(14) 0.021(7) Uiso 1 1 d . . . . .
H38C H -0.059(2) 0.0467(11) 0.5785(16) 0.035(8) Uiso 1 1 d . . . . .
H23 H 0.558(2) 0.3201(9) 0.4163(14) 0.018(6) Uiso 1 1 d . . . . .
H18C H 0.766(2) 0.0099(11) 0.1230(17) 0.046(9) Uiso 1 1 d . . . . .
H116 H 0.458(2) 0.1227(9) 0.5991(14) 0.022(7) Uiso 1 1 d . . . . .
H28C H 0.532(2) 0.3811(11) 0.5272(15) 0.031(8) Uiso 1 1 d . . . . .
H316 H 0.575(2) 0.2454(8) 0.5855(13) 0.018(6) Uiso 1 1 d . . . . .
H33 H 0.186(2) 0.1696(9) 0.5715(14) 0.019(6) Uiso 1 1 d . . . . .
H38B H -0.136(2) 0.0956(11) 0.5718(16) 0.042(8) Uiso 1 1 d . . . . .
H313 H 0.203(2) 0.2621(9) 0.5249(14) 0.021(7) Uiso 1 1 d . . . . .
H28I H 0.491(3) 0.4673(11) 0.3360(19) 0.050(10) Uiso 1 1 d . . . . .
H27F H 0.092(3) 0.4120(11) 0.2250(17) 0.042(8) Uiso 1 1 d . . . . .
H37C H 0.096(2) 0.0361(10) 0.2407(16) 0.035(8) Uiso 1 1 d . . . . .
H28F H 0.676(2) 0.3804(10) 0.4208(15) 0.029(7) Uiso 1 1 d . . . . .
H28B H 0.430(3) 0.4188(11) 0.5202(17) 0.046(9) Uiso 1 1 d . . . . .
H18B H 0.701(2) 0.0528(10) 0.0873(17) 0.034(8) Uiso 1 1 d . . . . .
H37I H 0.044(2) 0.1418(10) 0.2432(15) 0.033(8) Uiso 1 1 d . . . . .
H15 H 0.5192(19) 0.0838(8) 0.0764(13) 0.015(6) Uiso 1 1 d . . . . .
H37B H 0.183(3) 0.0729(11) 0.2743(16) 0.045(9) Uiso 1 1 d . . . . .
H115 H 0.386(2) 0.0477(9) 0.5937(14) 0.024(7) Uiso 1 1 d . . . . .
H27E H 0.149(2) 0.4244(11) 0.3022(17) 0.043(9) Uiso 1 1 d . . . . .
H28H H 0.529(2) 0.4887(11) 0.4130(16) 0.038(8) Uiso 1 1 d . . . . .
H38E H 0.184(3) 0.1063(12) 0.6656(16) 0.047(9) Uiso 1 1 d . . . . .
H27A H 0.097(2) 0.2989(11) 0.3137(17) 0.039(9) Uiso 1 1 d . . . . .
H18F H 0.688(2) -0.0352(10) 0.2305(14) 0.024(7) Uiso 1 1 d . . . . .
H18I H 0.597(3) -0.0395(12) 0.1033(17) 0.047(9) Uiso 1 1 d . . . . .
H37F H -0.095(2) 0.0353(10) 0.2837(17) 0.037(8) Uiso 1 1 d . . . . .
H38A H -0.101(3) 0.0724(11) 0.6546(18) 0.051(9) Uiso 1 1 d . . . . .
H37E H -0.052(2) 0.0278(11) 0.3716(17) 0.039(8) Uiso 1 1 d . . . . .
H35 H -0.027(2) 0.0810(9) 0.4665(14) 0.026(7) Uiso 1 1 d . . . . .
H28E H 0.660(2) 0.4143(10) 0.3465(17) 0.039(8) Uiso 1 1 d . . . . .
H216 H 0.712(2) 0.1519(10) 0.4871(15) 0.030(7) Uiso 1 1 d . . . . .
H28G H 0.414(3) 0.4704(11) 0.4041(16) 0.040(9) Uiso 1 1 d . . . . .
H37H H -0.067(2) 0.1366(11) 0.2709(16) 0.035(9) Uiso 1 1 d . . . . .
H18E H 0.578(2) -0.0179(10) 0.2674(16) 0.037(8) Uiso 1 1 d . . . . .
H17F H 0.502(3) 0.1417(10) -0.0158(15) 0.037(8) Uiso 1 1 d . . . . .
H13 H 0.552(2) 0.0612(10) 0.3046(15) 0.031(7) Uiso 1 1 d . . . . .
H28D H 0.687(2) 0.4343(11) 0.4304(16) 0.042(9) Uiso 1 1 d . . . . .
H215 H 0.850(2) 0.1797(9) 0.4151(14) 0.026(7) Uiso 1 1 d . . . . .
H17A H 0.235(2) 0.1332(11) 0.0706(15) 0.038(8) Uiso 1 1 d . . . . .
H37G H -0.036(2) 0.1019(11) 0.2066(18) 0.050(9) Uiso 1 1 d . . . . .
H18A H 0.761(3) 0.0602(13) 0.1692(19) 0.057(11) Uiso 1 1 d . . . . .
H27D H 0.217(3) 0.4218(11) 0.2241(16) 0.042(9) Uiso 1 1 d . . . . .
H28A H 0.551(3) 0.4361(12) 0.5358(18) 0.052(9) Uiso 1 1 d . . . . .
H37A H 0.143(2) 0.0311(11) 0.3245(18) 0.046(9) Uiso 1 1 d . . . . .
H18H H 0.536(2) 0.0050(10) 0.0658(17) 0.037(8) Uiso 1 1 d . . . . .
H18D H 0.686(3) 0.0098(11) 0.2805(18) 0.045(9) Uiso 1 1 d . . . . .
H38D H 0.141(3) 0.0533(13) 0.6290(19) 0.057(10) Uiso 1 1 d . . . . .
H17E H 0.398(3) 0.1650(12) -0.0523(19) 0.058(10) Uiso 1 1 d . . . . .
H18G H 0.481(3) -0.0195(11) 0.1334(16) 0.041(9) Uiso 1 1 d . . . . .
H37D H -0.129(2) 0.0680(10) 0.3524(15) 0.029(8) Uiso 1 1 d . . . . .
H27G H 0.115(3) 0.3367(11) 0.1588(17) 0.052(9) Uiso 1 1 d . . . . .
H17D H 0.393(3) 0.1129(13) -0.0185(19) 0.055(11) Uiso 1 1 d . . . . .
H17G H 0.415(2) 0.2359(10) 0.0298(16) 0.031(7) Uiso 1 1 d . . . . .
H11A H 0.371(3) -0.0315(14) 0.504(2) 0.069(12) Uiso 1 1 d . . . . .
H38G H 0.061(3) 0.1803(11) 0.6618(17) 0.043(9) Uiso 1 1 d . . . . .
H17B H 0.240(3) 0.1864(11) 0.0234(19) 0.052(9) Uiso 1 1 d . . . . .
H11B H 0.320(3) -0.0219(15) 0.434(3) 0.090(15) Uiso 1 1 d . . . . .
H17H H 0.426(3) 0.2323(12) 0.121(2) 0.060(11) Uiso 1 1 d . . . . .
H38F H 0.088(3) 0.0773(11) 0.7078(19) 0.054(10) Uiso 1 1 d . . . . .
H17C H 0.247(2) 0.1828(10) 0.1130(17) 0.038(8) Uiso 1 1 d . . . . .
H21A H 0.912(4) 0.2324(18) 0.313(3) 0.107(17) Uiso 1 1 d . . . . .
H27B H 0.014(3) 0.3412(12) 0.2737(18) 0.055(10) Uiso 1 1 d . . . . .
H38H H -0.019(3) 0.1486(13) 0.705(2) 0.068(11) Uiso 1 1 d . . . . .
H38I H -0.060(2) 0.1738(11) 0.6241(17) 0.039(9) Uiso 1 1 d . . . . .
H11C H 0.265(4) -0.0103(15) 0.501(2) 0.088(15) Uiso 1 1 d . . . . .
H21B H 0.835(3) 0.2530(14) 0.256(2) 0.076(13) Uiso 1 1 d . . . . .
H17I H 0.525(3) 0.2171(13) 0.068(2) 0.074(12) Uiso 1 1 d . . . . .
H21C H 0.864(4) 0.2771(19) 0.322(3) 0.095(17) Uiso 1 1 d . . . . .
H31A H 0.300(4) 0.3555(17) 0.635(2) 0.093(15) Uiso 1 1 d . . . . .
H31B H 0.201(3) 0.3395(14) 0.592(2) 0.086(13) Uiso 1 1 d . . . . .
H27C H 0.084(2) 0.3448(10) 0.3536(16) 0.022(8) Uiso 1 1 d . . . . .
H27I H 0.244(3) 0.3473(14) 0.160(2) 0.075(13) Uiso 1 1 d . . . . .
H31C H 0.236(4) 0.3209(17) 0.672(3) 0.111(18) 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 N2 1.9671(18) . ?
Os O1 1.9707(15) . ?
Os N3 1.9796(17) . ?
Os N1 2.0046(19) . ?
Os O2 2.0063(15) . ?
Os O3 2.0156(15) . ?
Os N10 3.2899(18) . ?
O1 C11 1.325(3) . ?
O2 C21 1.328(3) . ?
O3 C31 1.326(3) . ?
N1 C12 1.381(3) . ?
N1 C112 1.427(3) . ?
N2 C22 1.380(3) . ?
N2 C212 1.429(3) . ?
N3 C32 1.376(3) . ?
N3 C312 1.426(3) . ?
N10 C111 1.413(3) . ?
N10 C211 1.422(3) . ?
N10 C311 1.427(3) . ?
C11 C16 1.408(3) . ?
C11 C12 1.417(3) . ?
C12 C13 1.402(3) . ?
C13 C14 1.376(3) . ?
C13 H13 0.93(3) . ?
C14 C15 1.421(3) . ?
C14 C18 1.533(3) . ?
C15 C16 1.384(3) . ?
C15 H15 0.94(2) . ?
C16 C17 1.537(3) . ?
C17 C172 1.524(4) . ?
C17 C173 1.533(4) . ?
C17 C171 1.539(4) . ?
C18 C181 1.530(4) . ?
C18 C182 1.531(4) . ?
C18 C183 1.532(4) . ?
C21 C26 1.417(3) . ?
C21 C22 1.417(3) . ?
C22 C23 1.394(3) . ?
C23 C24 1.384(3) . ?
C23 H23 0.91(2) . ?
C24 C25 1.413(3) . ?
C24 C28 1.530(3) . ?
C25 C26 1.398(3) . ?
C25 H25 0.87(3) . ?
C26 C27 1.534(3) . ?
C27 C271 1.523(4) . ?
C27 C272 1.530(4) . ?
C27 C273 1.538(4) . ?
C28 C283 1.517(4) . ?
C28 C282 1.535(4) . ?
C28 C281 1.542(4) . ?
C31 C36 1.413(3) . ?
C31 C32 1.414(3) . ?
C32 C33 1.394(3) . ?
C33 C34 1.373(3) . ?
C33 H33 0.93(2) . ?
C34 C35 1.415(3) . ?
C34 C38 1.535(3) . ?
C35 C36 1.386(3) . ?
C35 H35 0.91(3) . ?
C36 C37 1.535(3) . ?
C37 C372 1.527(4) . ?
C37 C371 1.530(4) . ?
C37 C373 1.532(4) . ?
C38 C383 1.522(4) . ?
C38 C381 1.531(4) . ?
C38 C382 1.540(4) . ?
C111 C116 1.393(3) . ?
C111 C112 1.410(3) . ?
C112 C113 1.392(3) . ?
C113 C114 1.387(3) . ?
C113 H113 0.89(2) . ?
C114 C115 1.391(3) . ?
C114 C117 1.507(4) . ?
C115 C116 1.385(3) . ?
C115 H115 0.88(3) . ?
C116 H116 0.93(2) . ?
C117 H11A 0.92(4) . ?
C117 H11B 0.82(4) . ?
C117 H11C 0.85(4) . ?
C171 H17A 1.06(3) . ?
C171 H17B 1.01(3) . ?
C171 H17C 0.92(3) . ?
C172 H17F 0.96(3) . ?
C172 H17E 0.98(3) . ?
C172 H17D 0.97(3) . ?
C173 H17G 0.98(3) . ?
C173 H17H 0.98(3) . ?
C173 H17I 1.00(4) . ?
C181 H18C 1.00(3) . ?
C181 H18B 0.95(3) . ?
C181 H18A 0.96(3) . ?
C182 H18F 0.97(3) . ?
C182 H18E 0.98(3) . ?
C182 H18D 0.93(3) . ?
C183 H18I 0.99(3) . ?
C183 H18H 0.96(3) . ?
C183 H18G 0.97(3) . ?
C211 C216 1.389(3) . ?
C211 C212 1.405(3) . ?
C212 C213 1.391(3) . ?
C213 C214 1.388(3) . ?
C213 H213 0.92(2) . ?
C214 C215 1.388(4) . ?
C214 C217 1.514(4) . ?
C215 C216 1.385(3) . ?
C215 H215 0.94(3) . ?
C216 H216 0.93(3) . ?
C217 H21A 0.86(5) . ?
C217 H21B 0.92(4) . ?
C217 H21C 0.84(5) . ?
C271 H27A 0.98(3) . ?
C271 H27B 1.03(3) . ?
C271 H27C 0.88(3) . ?
C272 H27F 0.92(3) . ?
C272 H27E 1.00(3) . ?
C272 H27D 0.97(3) . ?
C273 H27H 1.04(2) . ?
C273 H27G 0.97(3) . ?
C273 H27I 0.97(4) . ?
C281 H28C 0.96(3) . ?
C281 H28B 1.03(3) . ?
C281 H28A 0.97(3) . ?
C282 H28F 0.96(3) . ?
C282 H28E 1.03(3) . ?
C282 H28D 0.96(3) . ?
C283 H28I 0.96(3) . ?
C283 H28H 0.96(3) . ?
C283 H28G 0.92(3) . ?
C311 C316 1.387(3) . ?
C311 C312 1.398(3) . ?
C312 C313 1.383(3) . ?
C313 C314 1.389(3) . ?
C313 H313 0.92(2) . ?
C314 C315 1.391(3) . ?
C314 C317 1.503(4) . ?
C315 C316 1.384(4) . ?
C315 H315 0.91(3) . ?
C316 H316 0.95(2) . ?
C317 H31A 0.88(5) . ?
C317 H31B 0.95(4) . ?
C317 H31C 0.93(5) . ?
C371 H37C 1.01(3) . ?
C371 H37B 0.98(3) . ?
C371 H37A 0.92(3) . ?
C372 H37F 0.99(3) . ?
C372 H37E 0.96(3) . ?
C372 H37D 0.94(3) . ?
C373 H37I 0.95(3) . ?
C373 H37H 0.91(3) . ?
C373 H37G 0.98(3) . ?
C381 H38C 1.05(3) . ?
C381 H38B 1.03(3) . ?
C381 H38A 0.95(3) . ?
C382 H38E 1.00(3) . ?
C382 H38D 1.06(3) . ?
C382 H38F 0.99(3) . ?
C383 H38G 1.00(3) . ?
C383 H38H 0.97(4) . ?
C383 H38I 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
N2 Os O1 97.76(7) . . ?
N2 Os N3 94.59(7) . . ?
O1 Os N3 167.41(7) . . ?
N2 Os N1 96.36(8) . . ?
O1 Os N1 79.07(7) . . ?
N3 Os N1 97.20(7) . . ?
N2 Os O2 79.26(7) . . ?
O1 Os O2 88.12(6) . . ?
N3 Os O2 96.58(7) . . ?
N1 Os O2 165.83(7) . . ?
N2 Os O3 170.82(7) . . ?
O1 Os O3 90.13(6) . . ?
N3 Os O3 77.78(7) . . ?
N1 Os O3 89.72(7) . . ?
O2 Os O3 96.39(6) . . ?
N2 Os N10 59.30(6) . . ?
O1 Os N10 127.30(5) . . ?
N3 Os N10 58.20(6) . . ?
N1 Os N10 59.95(6) . . ?
O2 Os N10 126.24(5) . . ?
O3 Os N10 119.01(5) . . ?
C11 O1 Os 116.69(13) . . ?
C21 O2 Os 115.02(13) . . ?
C31 O3 Os 116.44(13) . . ?
C12 N1 C112 121.92(19) . . ?
C12 N1 Os 115.27(14) . . ?
C112 N1 Os 120.13(14) . . ?
C22 N2 C212 119.89(19) . . ?
C22 N2 Os 116.10(14) . . ?
C212 N2 Os 123.97(15) . . ?
C32 N3 C312 120.24(18) . . ?
C32 N3 Os 117.55(14) . . ?
C312 N3 Os 122.20(14) . . ?
C111 N10 C211 120.80(18) . . ?
C111 N10 C311 120.11(18) . . ?
C211 N10 C311 116.35(18) . . ?
C111 N10 Os 83.26(12) . . ?
C211 N10 Os 85.15(12) . . ?
C311 N10 Os 85.07(11) . . ?
O1 C11 C16 122.6(2) . . ?
O1 C11 C12 116.11(19) . . ?
C16 C11 C12 121.3(2) . . ?
N1 C12 C13 127.4(2) . . ?
N1 C12 C11 112.5(2) . . ?
C13 C12 C11 120.1(2) . . ?
C14 C13 C12 119.8(2) . . ?
C14 C13 H13 120.6(16) . . ?
C12 C13 H13 119.6(16) . . ?
C13 C14 C15 118.7(2) . . ?
C13 C14 C18 122.6(2) . . ?
C15 C14 C18 118.7(2) . . ?
C16 C15 C14 123.8(2) . . ?
C16 C15 H15 119.6(15) . . ?
C14 C15 H15 116.5(14) . . ?
C15 C16 C11 116.2(2) . . ?
C15 C16 C17 123.8(2) . . ?
C11 C16 C17 120.0(2) . . ?
C172 C17 C173 108.7(3) . . ?
C172 C17 C16 111.1(2) . . ?
C173 C17 C16 110.3(2) . . ?
C172 C17 C171 108.1(2) . . ?
C173 C17 C171 109.6(2) . . ?
C16 C17 C171 109.0(2) . . ?
C181 C18 C182 108.6(2) . . ?
C181 C18 C183 109.8(2) . . ?
C182 C18 C183 107.3(2) . . ?
C181 C18 C14 109.0(2) . . ?
C182 C18 C14 112.2(2) . . ?
C183 C18 C14 110.0(2) . . ?
O2 C21 C26 123.72(19) . . ?
O2 C21 C22 116.23(19) . . ?
C26 C21 C22 120.0(2) . . ?
N2 C22 C23 126.6(2) . . ?
N2 C22 C21 112.5(2) . . ?
C23 C22 C21 120.9(2) . . ?
C24 C23 C22 120.1(2) . . ?
C24 C23 H23 123.3(16) . . ?
C22 C23 H23 116.6(16) . . ?
C23 C24 C25 118.3(2) . . ?
C23 C24 C28 119.5(2) . . ?
C25 C24 C28 122.1(2) . . ?
C26 C25 C24 123.7(2) . . ?
C26 C25 H25 116.2(18) . . ?
C24 C25 H25 120.0(18) . . ?
C25 C26 C21 116.5(2) . . ?
C25 C26 C27 122.6(2) . . ?
C21 C26 C27 120.9(2) . . ?
C271 C27 C272 108.4(2) . . ?
C271 C27 C26 110.1(2) . . ?
C272 C27 C26 112.0(2) . . ?
C271 C27 C273 109.9(3) . . ?
C272 C27 C273 107.8(2) . . ?
C26 C27 C273 108.6(2) . . ?
C283 C28 C24 112.5(2) . . ?
C283 C28 C282 107.5(2) . . ?
C24 C28 C282 110.5(2) . . ?
C283 C28 C281 109.8(3) . . ?
C24 C28 C281 107.8(2) . . ?
C282 C28 C281 108.7(2) . . ?
O3 C31 C36 124.7(2) . . ?
O3 C31 C32 115.56(19) . . ?
C36 C31 C32 119.6(2) . . ?
N3 C32 C33 126.0(2) . . ?
N3 C32 C31 112.23(19) . . ?
C33 C32 C31 121.6(2) . . ?
C34 C33 C32 119.8(2) . . ?
C34 C33 H33 120.3(15) . . ?
C32 C33 H33 119.9(15) . . ?
C33 C34 C35 117.9(2) . . ?
C33 C34 C38 119.0(2) . . ?
C35 C34 C38 123.0(2) . . ?
C36 C35 C34 124.6(2) . . ?
C36 C35 H35 119.1(16) . . ?
C34 C35 H35 116.4(16) . . ?
C35 C36 C31 116.4(2) . . ?
C35 C36 C37 122.9(2) . . ?
C31 C36 C37 120.5(2) . . ?
C372 C37 C371 108.4(2) . . ?
C372 C37 C373 108.1(2) . . ?
C371 C37 C373 109.2(2) . . ?
C372 C37 C36 112.1(2) . . ?
C371 C37 C36 108.84(19) . . ?
C373 C37 C36 110.2(2) . . ?
C383 C38 C381 109.1(2) . . ?
C383 C38 C34 110.0(2) . . ?
C381 C38 C34 112.5(2) . . ?
C383 C38 C382 109.1(3) . . ?
C381 C38 C382 107.6(2) . . ?
C34 C38 C382 108.3(2) . . ?
C116 C111 C112 118.4(2) . . ?
C116 C111 N10 119.5(2) . . ?
C112 C111 N10 122.1(2) . . ?
C113 C112 C111 119.3(2) . . ?
C113 C112 N1 120.5(2) . . ?
C111 C112 N1 119.3(2) . . ?
C114 C113 C112 122.2(2) . . ?
C114 C113 H113 118.9(15) . . ?
C112 C113 H113 118.7(15) . . ?
C113 C114 C115 117.9(2) . . ?
C113 C114 C117 121.3(2) . . ?
C115 C114 C117 120.8(2) . . ?
C116 C115 C114 121.0(2) . . ?
C116 C115 H115 118.8(17) . . ?
C114 C115 H115 120.1(17) . . ?
C115 C116 C111 121.1(2) . . ?
C115 C116 H116 120.3(16) . . ?
C111 C116 H116 118.6(16) . . ?
C114 C117 H11A 111(2) . . ?
C114 C117 H11B 114(3) . . ?
H11A C117 H11B 102(3) . . ?
C114 C117 H11C 111(3) . . ?
H11A C117 H11C 106(3) . . ?
H11B C117 H11C 113(4) . . ?
C17 C171 H17A 111.9(15) . . ?
C17 C171 H17B 109.6(18) . . ?
H17A C171 H17B 110(2) . . ?
C17 C171 H17C 113.0(19) . . ?
H17A C171 H17C 105(2) . . ?
H17B C171 H17C 107(3) . . ?
C17 C172 H17F 113.2(17) . . ?
C17 C172 H17E 110.1(19) . . ?
H17F C172 H17E 105(2) . . ?
C17 C172 H17D 113(2) . . ?
H17F C172 H17D 108(3) . . ?
H17E C172 H17D 108(3) . . ?
C17 C173 H17G 110.5(16) . . ?
C17 C173 H17H 113(2) . . ?
H17G C173 H17H 108(3) . . ?
C17 C173 H17I 113(2) . . ?
H17G C173 H17I 103(3) . . ?
H17H C173 H17I 109(3) . . ?
C18 C181 H18C 109.4(17) . . ?
C18 C181 H18B 107.5(17) . . ?
H18C C181 H18B 105(2) . . ?
C18 C181 H18A 112(2) . . ?
H18C C181 H18A 112(3) . . ?
H18B C181 H18A 111(3) . . ?
C18 C182 H18F 110.5(15) . . ?
C18 C182 H18E 109.6(16) . . ?
H18F C182 H18E 109(2) . . ?
C18 C182 H18D 112.7(19) . . ?
H18F C182 H18D 108(2) . . ?
H18E C182 H18D 107(2) . . ?
C18 C183 H18I 109.4(18) . . ?
C18 C183 H18H 110.2(17) . . ?
H18I C183 H18H 107(2) . . ?
C18 C183 H18G 110.8(17) . . ?
H18I C183 H18G 113(3) . . ?
H18H C183 H18G 106(2) . . ?
C216 C211 C212 118.7(2) . . ?
C216 C211 N10 120.8(2) . . ?
C212 C211 N10 120.48(19) . . ?
C213 C212 C211 119.9(2) . . ?
C213 C212 N2 120.3(2) . . ?
C211 C212 N2 119.57(19) . . ?
C214 C213 C212 121.1(2) . . ?
C214 C213 H213 120.5(14) . . ?
C212 C213 H213 118.4(14) . . ?
C215 C214 C213 118.6(2) . . ?
C215 C214 C217 121.2(2) . . ?
C213 C214 C217 120.2(3) . . ?
C216 C215 C214 120.9(2) . . ?
C216 C215 H215 118.8(16) . . ?
C214 C215 H215 120.2(16) . . ?
C215 C216 C211 120.7(2) . . ?
C215 C216 H216 118.7(16) . . ?
C211 C216 H216 120.6(16) . . ?
C214 C217 H21A 113(3) . . ?
C214 C217 H21B 115(2) . . ?
H21A C217 H21B 109(4) . . ?
C214 C217 H21C 109(3) . . ?
H21A C217 H21C 110(4) . . ?
H21B C217 H21C 101(4) . . ?
C27 C271 H27A 108.6(18) . . ?
C27 C271 H27B 106.6(18) . . ?
H27A C271 H27B 114(3) . . ?
C27 C271 H27C 110.3(18) . . ?
H27A C271 H27C 105(3) . . ?
H27B C271 H27C 113(3) . . ?
C27 C272 H27F 110.2(19) . . ?
C27 C272 H27E 111.5(17) . . ?
H27F C272 H27E 104(2) . . ?
C27 C272 H27D 110.7(18) . . ?
H27F C272 H27D 109(3) . . ?
H27E C272 H27D 111(2) . . ?
C27 C273 H27H 113.1(12) . . ?
C27 C273 H27G 105.3(19) . . ?
H27H C273 H27G 108(2) . . ?
C27 C273 H27I 106(2) . . ?
H27H C273 H27I 114(3) . . ?
H27G C273 H27I 112(3) . . ?
C28 C281 H28C 111.6(16) . . ?
C28 C281 H28B 110.8(17) . . ?
H28C C281 H28B 111(2) . . ?
C28 C281 H28A 112.5(18) . . ?
H28C C281 H28A 108(2) . . ?
H28B C281 H28A 103(2) . . ?
C28 C282 H28F 113.1(16) . . ?
C28 C282 H28E 112.8(16) . . ?
H28F C282 H28E 108(2) . . ?
C28 C282 H28D 111.6(18) . . ?
H28F C282 H28D 106(2) . . ?
H28E C282 H28D 106(2) . . ?
C28 C283 H28I 113(2) . . ?
C28 C283 H28H 111.3(17) . . ?
H28I C283 H28H 104(3) . . ?
C28 C283 H28G 112.0(19) . . ?
H28I C283 H28G 112(3) . . ?
H28H C283 H28G 104(2) . . ?
C316 C311 C312 118.3(2) . . ?
C316 C311 N10 121.3(2) . . ?
C312 C311 N10 120.35(19) . . ?
C313 C312 C311 120.8(2) . . ?
C313 C312 N3 120.1(2) . . ?
C311 C312 N3 118.6(2) . . ?
C312 C313 C314 121.2(2) . . ?
C312 C313 H313 120.0(16) . . ?
C314 C313 H313 118.8(16) . . ?
C313 C314 C315 117.6(2) . . ?
C313 C314 C317 120.5(2) . . ?
C315 C314 C317 121.9(2) . . ?
C316 C315 C314 121.7(2) . . ?
C316 C315 H315 117.7(16) . . ?
C314 C315 H315 120.6(16) . . ?
C315 C316 C311 120.4(2) . . ?
C315 C316 H316 120.7(14) . . ?
C311 C316 H316 118.9(14) . . ?
C314 C317 H31A 114(3) . . ?
C314 C317 H31B 113(2) . . ?
H31A C317 H31B 105(4) . . ?
C314 C317 H31C 112(3) . . ?
H31A C317 H31C 104(4) . . ?
H31B C317 H31C 107(4) . . ?
C37 C371 H37C 109.9(16) . . ?
C37 C371 H37B 112.8(18) . . ?
H37C C371 H37B 105(2) . . ?
C37 C371 H37A 111.9(19) . . ?
H37C C371 H37A 107(2) . . ?
H37B C371 H37A 110(3) . . ?
C37 C372 H37F 109.6(16) . . ?
C37 C372 H37E 113.0(17) . . ?
H37F C372 H37E 110(2) . . ?
C37 C372 H37D 111.9(18) . . ?
H37F C372 H37D 109(2) . . ?
H37E C372 H37D 103(2) . . ?
C37 C373 H37I 112.2(17) . . ?
C37 C373 H37H 108.1(18) . . ?
H37I C373 H37H 105(3) . . ?
C37 C373 H37G 110.3(18) . . ?
H37I C373 H37G 111(2) . . ?
H37H C373 H37G 110(2) . . ?
C38 C381 H38C 113.0(15) . . ?
C38 C381 H38B 109.8(16) . . ?
H38C C381 H38B 106(2) . . ?
C38 C381 H38A 112.0(19) . . ?
H38C C381 H38A 107(2) . . ?
H38B C381 H38A 109(2) . . ?
C38 C382 H38E 109.9(18) . . ?
C38 C382 H38D 111.3(18) . . ?
H38E C382 H38D 110(3) . . ?
C38 C382 H38F 106.4(19) . . ?
H38E C382 H38F 110(2) . . ?
H38D C382 H38F 110(3) . . ?
C38 C383 H38G 115.0(18) . . ?
C38 C383 H38H 108(2) . . ?
H38G C383 H38H 103(3) . . ?
C38 C383 H38I 108.9(18) . . ?
H38G C383 H38I 108(3) . . ?
H38H C383 H38I 114(3) . . ?

_refine_diff_density_max         1.685
_refine_diff_density_min         -1.078
_refine_diff_density_rms         0.091

_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_meclampru
_database_code_depnum_ccdc_archive 'CCDC 1994514'
loop_
_audit_author_name
_audit_author_address
'Seth Brown'
;University of Notre Dame
United States of America
;
_audit_update_record             
;
2020-04-02 deposited with the CCDC.	2020-04-29 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT220_meclampru           
;
PROBLEM: Non-Solvent  Resd 1  C   Ueq(max)/Ueq(min) Range        6.1 Ratio 
RESPONSE: The main molecule contains both well-fixed atoms such as the
central Ru and poorly fixed atoms such as tert-butyl groups.  In 
particular, the tert-butyl group centered on C38 has unresolved
disorder that leads to large thermal parameters.
;
_vrf_PLAT241_meclampru           
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of        C73 Check 
RESPONSE: C73 and C74 are part of a lattice C6D6 molecule which shows
large and variable thermal parameters.
;
_vrf_PLAT242_meclampru           
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        C74 Check 
RESPONSE: C73 and C74 are part of a lattice C6D6 molecule which shows
large and variable thermal parameters.
;
_vrf_PLAT245_meclampru           
;
PROBLEM: U(iso) H38G      Smaller than U(eq) C383      by      0.072 Ang**2
RESPONSE: C383 shows unresolved disorder, and the attached hydrogens show
highly variable thermal parameters.
;
_vrf_PLAT390_meclampru           
;
PROBLEM: Deviating Methyl C383      X-C-H Bond Angle ....        100 Degree
RESPONSE: The hydrogens found on the difference map show angles that 
deviate slightly from ideality.
;
_vrf_PLAT391_meclampru           
;
PROBLEM: Deviating Methyl C117      H-C-H Bond Angle ....         99 Degree
RESPONSE: The hydrogens found on the difference map show angles that 
deviate slightly from ideality.
;
# end Validation Reply Form


_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 [Tris(2-(3',5'-di-tert-butyl-2'-oxyphenyl)amido-4-
methylphenyl)amine]ruthenium(VI)
;
_chemical_name_common            '(MeClamp)Ru . C6D6'
_chemical_melting_point          ?
_chemical_formula_moiety         'C63 H78 N4 O3 Ru, C6 D6'
_chemical_formula_sum            'C69 H78 D6 N4 O3 Ru'
_chemical_formula_weight         1124.50

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru 0.0552 3.2960 '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           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

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

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

_cell_length_a                   25.7596(3)
_cell_length_b                   17.4114(2)
_cell_length_c                   27.7512(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     12446.7(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9681
_cell_measurement_theta_min      3.45
_cell_measurement_theta_max      71.91

_exptl_crystal_description       tablet
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_F_000             4752
_exptl_transmission_factor_min   0.6498
_exptl_transmission_factor_max   0.7536
_exptl_crystal_size_max          0.159
_exptl_crystal_size_mid          0.112
_exptl_crystal_size_min          0.103
_exptl_absorpt_coefficient_mu    2.401
_shelx_estimated_absorpt_T_min   0.701
_shelx_estimated_absorpt_T_max   0.790
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6498
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_process_details   
;
Blessing, R. H. (1995) Acta Cryst. A51, 33-38.

Sheldrick, G.M. (2008) SADABS v2008/1. Bruker AXS Inc.
Madison, WI USA.
;

_exptl_crystal_recrystallization_method 
;
 Crystals were grown by liquid-liquid diffusion of 
acetonitrile into a solution of the complex in C6D6.
;


_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.33
_diffrn_reflns_number            218296
_diffrn_reflns_av_unetI/netI     0.0229
_diffrn_reflns_av_R_equivalents  0.0578
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         3.185
_diffrn_reflns_theta_max         72.153
_diffrn_reflns_theta_full        67.679
_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 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             12266
_reflns_number_gt                11058
_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          
;
 All hydrogens in (MeClamp)Ru were found on difference Fourier
maps and refined isotropically.  All deuterium atoms in the
lattice C6D6 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)+(0.0411P)²+6.9874P] 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_number_reflns         12266
_refine_ls_number_parameters     1016
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0297
_refine_ls_wR_factor_ref         0.0784
_refine_ls_wR_factor_gt          0.0754
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru Ru 0.39507(2) 0.14785(2) 0.20835(2) 0.01621(5) Uani 1 1 d . . . . .
O1 O 0.37185(4) 0.24643(6) 0.17604(4) 0.0207(2) Uani 1 1 d . . . . .
N1 N 0.32312(5) 0.12062(8) 0.18921(5) 0.0178(3) Uani 1 1 d . . . . .
O2 O 0.47030(4) 0.17866(7) 0.21786(4) 0.0202(2) Uani 1 1 d . . . . .
N2 N 0.42730(5) 0.11286(7) 0.14677(5) 0.0185(3) Uani 1 1 d . . . . .
O3 O 0.37067(4) 0.17942(7) 0.27442(4) 0.0211(2) Uani 1 1 d . . . . .
N3 N 0.40653(5) 0.05120(8) 0.24513(5) 0.0189(3) Uani 1 1 d . . . . .
N10 N 0.36825(5) -0.02084(8) 0.16012(5) 0.0198(3) Uani 1 1 d . . . . .
C11 C 0.32716(6) 0.24170(9) 0.15395(6) 0.0192(3) Uani 1 1 d . . . . .
C12 C 0.29756(6) 0.17275(9) 0.16175(6) 0.0190(3) Uani 1 1 d . . . . .
C13 C 0.24852(7) 0.16236(9) 0.13989(6) 0.0204(3) Uani 1 1 d . . . . .
H13 H 0.2300(8) 0.1160(13) 0.1450(8) 0.027(5) Uiso 1 1 d . . . . .
C14 C 0.22912(6) 0.21848(9) 0.11019(6) 0.0210(3) Uani 1 1 d . . . . .
C15 C 0.25974(7) 0.28548(9) 0.10169(6) 0.0229(3) Uani 1 1 d . . . . .
H15 H 0.2449(8) 0.3260(12) 0.0808(8) 0.025(5) Uiso 1 1 d . . . . .
C16 C 0.30796(6) 0.29893(9) 0.12171(6) 0.0210(3) Uani 1 1 d . . . . .
C17 C 0.34053(7) 0.37028(10) 0.10962(6) 0.0237(3) Uani 1 1 d . . . . .
C18 C 0.17710(7) 0.21089(10) 0.08399(6) 0.0248(3) Uani 1 1 d . . . . .
C21 C 0.50217(6) 0.15719(9) 0.18381(6) 0.0196(3) Uani 1 1 d . . . . .
C22 C 0.47905(6) 0.12146(9) 0.14243(6) 0.0196(3) Uani 1 1 d . . . . .
C23 C 0.50961(7) 0.09524(10) 0.10350(6) 0.0226(3) Uani 1 1 d . . . . .
H23 H 0.4926(8) 0.0717(12) 0.0770(8) 0.025(5) Uiso 1 1 d . . . . .
C24 C 0.56244(7) 0.10347(10) 0.10532(6) 0.0254(3) Uani 1 1 d . . . . .
C25 C 0.58506(7) 0.13808(10) 0.14718(7) 0.0257(3) Uani 1 1 d . . . . .
H25 H 0.6222(8) 0.1442(11) 0.1490(8) 0.021(5) Uiso 1 1 d . . . . .
C26 C 0.55723(7) 0.16432(9) 0.18626(6) 0.0219(3) Uani 1 1 d . . . . .
C27 C 0.58268(7) 0.19587(10) 0.23225(6) 0.0252(3) Uani 1 1 d . . . . .
C28 C 0.59789(7) 0.07342(13) 0.06511(7) 0.0322(4) Uani 1 1 d . . . . .
C31 C 0.36731(6) 0.12309(10) 0.30551(6) 0.0207(3) Uani 1 1 d . . . . .
C32 C 0.38875(7) 0.05060(10) 0.29116(6) 0.0216(3) Uani 1 1 d . . . . .
C33 C 0.38737(8) -0.01327(11) 0.32255(6) 0.0286(4) Uani 1 1 d . . . . .
H33 H 0.4009(8) -0.0611(14) 0.3112(8) 0.031(6) Uiso 1 1 d . . . . .
C34 C 0.36443(9) -0.00577(11) 0.36697(7) 0.0352(4) Uani 1 1 d . . . . .
C35 C 0.34170(8) 0.06580(11) 0.37975(6) 0.0318(4) Uani 1 1 d . . . . .
H35 H 0.3232(9) 0.0712(14) 0.4107(9) 0.036(6) Uiso 1 1 d . . . . .
C36 C 0.34193(7) 0.13017(10) 0.35093(6) 0.0248(3) Uani 1 1 d . . . . .
C37 C 0.31367(7) 0.20437(11) 0.36443(6) 0.0285(4) Uani 1 1 d . . . . .
C38 C 0.35968(12) -0.07225(13) 0.40294(7) 0.0517(7) Uani 1 1 d . . . . .
C111 C 0.32511(6) -0.01962(9) 0.19218(6) 0.0194(3) Uani 1 1 d . . . . .
C112 C 0.30026(6) 0.04981(9) 0.20406(5) 0.0185(3) Uani 1 1 d . . . . .
C113 C 0.25863(6) 0.04942(10) 0.23591(6) 0.0221(3) Uani 1 1 d . . . . .
H113 H 0.2436(8) 0.0984(12) 0.2459(7) 0.021(5) Uiso 1 1 d . . . . .
C114 C 0.24231(7) -0.01860(10) 0.25783(6) 0.0256(3) Uani 1 1 d . . . . .
C115 C 0.26733(7) -0.08696(10) 0.24601(7) 0.0276(4) Uani 1 1 d . . . . .
H115 H 0.2570(9) -0.1343(13) 0.2596(8) 0.031(6) Uiso 1 1 d . . . . .
C116 C 0.30791(7) -0.08755(10) 0.21315(6) 0.0244(3) Uani 1 1 d . . . . .
H116 H 0.3235(9) -0.1343(14) 0.2036(8) 0.029(6) Uiso 1 1 d . . . . .
C117 C 0.19982(9) -0.01712(14) 0.29510(8) 0.0393(5) Uani 1 1 d . . . . .
H11A H 0.1675(13) 0.0052(19) 0.2835(11) 0.065(9) Uiso 1 1 d . . . . .
H11B H 0.1926(12) -0.066(2) 0.3075(11) 0.066(9) Uiso 1 1 d . . . . .
H11C H 0.2079(14) 0.020(2) 0.3212(14) 0.087(11) Uiso 1 1 d . . . . .
C211 C 0.36389(6) 0.02191(9) 0.11687(6) 0.0195(3) Uani 1 1 d . . . . .
C212 C 0.39561(6) 0.08535(10) 0.10839(6) 0.0194(3) Uani 1 1 d . . . . .
C213 C 0.38934(7) 0.12897(10) 0.06680(6) 0.0229(3) Uani 1 1 d . . . . .
H213 H 0.4113(9) 0.1731(13) 0.0626(8) 0.027(5) Uiso 1 1 d . . . . .
C214 C 0.34933(7) 0.11285(10) 0.03451(6) 0.0257(3) Uani 1 1 d . . . . .
C215 C 0.31727(7) 0.05023(10) 0.04357(6) 0.0253(3) Uani 1 1 d . . . . .
H215 H 0.2896(9) 0.0387(13) 0.0217(8) 0.033(6) Uiso 1 1 d . . . . .
C216 C 0.32503(7) 0.00423(10) 0.08391(6) 0.0232(3) Uani 1 1 d . . . . .
H216 H 0.3030(9) -0.0396(13) 0.0900(8) 0.029(5) Uiso 1 1 d . . . . .
C217 C 0.33980(10) 0.16559(14) -0.00751(8) 0.0392(5) Uani 1 1 d . . . . .
H21A H 0.3696(13) 0.1760(19) -0.0233(12) 0.064(9) Uiso 1 1 d . . . . .
H21B H 0.3151(13) 0.1412(18) -0.0314(12) 0.070(10) Uiso 1 1 d . . . . .
H21C H 0.3258(15) 0.213(2) 0.0037(14) 0.098(13) Uiso 1 1 d . . . . .
C131 C 0.41809(6) -0.03941(9) 0.17901(6) 0.0200(3) Uani 1 1 d . . . . .
C132 C 0.43446(6) -0.01065(9) 0.22385(6) 0.0201(3) Uani 1 1 d . . . . .
C133 C 0.48198(7) -0.03374(10) 0.24295(6) 0.0237(3) Uani 1 1 d . . . . .
H133 H 0.4929(8) -0.0127(12) 0.2731(8) 0.026(5) Uiso 1 1 d . . . . .
C134 C 0.51511(7) -0.08152(10) 0.21723(7) 0.0271(4) Uani 1 1 d . . . . .
C135 C 0.50004(7) -0.10526(10) 0.17127(7) 0.0268(4) Uani 1 1 d . . . . .
H135 H 0.5220(9) -0.1372(13) 0.1530(8) 0.029(5) Uiso 1 1 d . . . . .
C136 C 0.45173(7) -0.08579(10) 0.15284(6) 0.0239(3) Uani 1 1 d . . . . .
H136 H 0.4414(9) -0.1050(14) 0.1225(9) 0.036(6) Uiso 1 1 d . . . . .
C137 C 0.56600(8) -0.10692(14) 0.23887(10) 0.0400(5) Uani 1 1 d . . . . .
H13A H 0.5796(11) -0.0710(18) 0.2598(11) 0.057(8) Uiso 1 1 d . . . . .
H13B H 0.5631(13) -0.152(2) 0.2547(13) 0.072(10) Uiso 1 1 d . . . . .
H13C H 0.5908(16) -0.109(2) 0.2152(14) 0.090(12) Uiso 1 1 d . . . . .
C171 C 0.39541(8) 0.34731(13) 0.09341(10) 0.0401(5) Uani 1 1 d . . . . .
H17A H 0.3934(11) 0.3160(19) 0.0645(12) 0.063(9) Uiso 1 1 d . . . . .
H17B H 0.4146(11) 0.3214(18) 0.1174(11) 0.056(8) Uiso 1 1 d . . . . .
H17C H 0.4164(10) 0.3970(15) 0.0858(9) 0.044(7) Uiso 1 1 d . . . . .
C172 C 0.34305(9) 0.42190(12) 0.15422(8) 0.0363(4) Uani 1 1 d . . . . .
H17D H 0.3551(10) 0.3954(15) 0.1798(10) 0.041(7) Uiso 1 1 d . . . . .
H17E H 0.3062(11) 0.4422(15) 0.1625(10) 0.049(7) Uiso 1 1 d . . . . .
H17F H 0.3657(10) 0.4655(15) 0.1464(9) 0.040(6) Uiso 1 1 d . . . . .
C173 C 0.31691(8) 0.41631(11) 0.06777(7) 0.0321(4) Uani 1 1 d . . . . .
H17G H 0.2834(10) 0.4378(15) 0.0765(9) 0.041(6) Uiso 1 1 d . . . . .
H17H H 0.3136(10) 0.3834(16) 0.0388(10) 0.047(7) Uiso 1 1 d . . . . .
H17I H 0.3403(9) 0.4609(14) 0.0602(8) 0.034(6) Uiso 1 1 d . . . . .
C181 C 0.15024(8) 0.13441(11) 0.09493(8) 0.0329(4) Uani 1 1 d . . . . .
H18A H 0.1444(10) 0.1301(14) 0.1301(10) 0.040(6) Uiso 1 1 d . . . . .
H18B H 0.1728(10) 0.0958(15) 0.0841(9) 0.038(6) Uiso 1 1 d . . . . .
H18C H 0.1174(10) 0.1341(14) 0.0784(9) 0.039(6) Uiso 1 1 d . . . . .
C182 C 0.14078(8) 0.27622(12) 0.09900(9) 0.0373(5) Uani 1 1 d . . . . .
H18D H 0.1567(10) 0.3271(16) 0.0940(10) 0.047(7) Uiso 1 1 d . . . . .
H18E H 0.1326(10) 0.2727(15) 0.1331(10) 0.043(7) Uiso 1 1 d . . . . .
H18F H 0.1079(10) 0.2712(15) 0.0817(9) 0.042(7) Uiso 1 1 d . . . . .
C183 C 0.18706(10) 0.21407(15) 0.02941(8) 0.0412(5) Uani 1 1 d . . . . .
H18G H 0.2097(12) 0.1724(19) 0.0198(11) 0.064(9) Uiso 1 1 d . . . . .
H18H H 0.1534(11) 0.2093(16) 0.0121(10) 0.051(7) Uiso 1 1 d . . . . .
H18I H 0.2033(11) 0.2628(17) 0.0207(10) 0.052(7) Uiso 1 1 d . . . . .
C271 C 0.56905(9) 0.14286(13) 0.27466(8) 0.0376(5) Uani 1 1 d . . . . .
H27A H 0.5819(11) 0.1658(16) 0.3051(10) 0.048(7) Uiso 1 1 d . . . . .
H27B H 0.5844(12) 0.0906(19) 0.2700(12) 0.067(9) Uiso 1 1 d . . . . .
H27C H 0.5312(11) 0.1366(15) 0.2798(10) 0.044(7) Uiso 1 1 d . . . . .
C272 C 0.64189(8) 0.19979(13) 0.22786(8) 0.0372(5) Uani 1 1 d . . . . .
H27D H 0.6527(10) 0.2355(16) 0.2021(9) 0.042(7) Uiso 1 1 d . . . . .
H27E H 0.6565(10) 0.2191(15) 0.2587(9) 0.044(7) Uiso 1 1 d . . . . .
H27F H 0.6578(11) 0.1502(16) 0.2210(10) 0.049(8) Uiso 1 1 d . . . . .
C273 C 0.56253(8) 0.27713(11) 0.24221(8) 0.0347(4) Uani 1 1 d . . . . .
H27G H 0.5708(11) 0.3123(17) 0.2138(10) 0.052(8) Uiso 1 1 d . . . . .
H27H H 0.5261(11) 0.2771(16) 0.2487(10) 0.050(7) Uiso 1 1 d . . . . .
H27I H 0.5795(10) 0.2965(15) 0.2698(10) 0.043(7) Uiso 1 1 d . . . . .
C281 C 0.62980(12) 0.1399(2) 0.04425(11) 0.0526(8) Uani 0.899(4) 1 d . . P A 1
H28A H 0.6523(14) 0.160(2) 0.0708(13) 0.064(10) Uiso 0.899(4) 1 d . . P A 1
H28B H 0.6515(13) 0.119(2) 0.0203(13) 0.060(9) Uiso 0.899(4) 1 d . . P A 1
H28C H 0.6054(14) 0.184(2) 0.0285(14) 0.071(11) Uiso 0.899(4) 1 d . . P A 1
C282 C 0.56674(9) 0.03808(19) 0.02309(9) 0.0409(6) Uani 0.899(4) 1 d . . P A 1
H28D H 0.5914(12) 0.0235(18) -0.0016(11) 0.050(8) Uiso 0.899(4) 1 d . . P A 1
H28E H 0.5469(11) -0.0092(17) 0.0345(10) 0.043(7) Uiso 0.899(4) 1 d . . P A 1
H28F H 0.5428(12) 0.0814(18) 0.0082(11) 0.050(8) Uiso 0.899(4) 1 d . . P A 1
C283 C 0.63332(13) 0.0113(2) 0.08549(10) 0.0537(8) Uani 0.899(4) 1 d . . P A 1
H28G H 0.6585(13) -0.0089(19) 0.0603(12) 0.061(9) Uiso 0.899(4) 1 d . . P A 1
H28H H 0.6552(14) 0.032(2) 0.1104(13) 0.066(10) Uiso 0.899(4) 1 d . . P A 1
H28I H 0.6124(14) -0.030(2) 0.1015(14) 0.061(11) Uiso 0.899(4) 1 d . . P A 1
C284 C 0.6046(12) -0.0161(19) 0.0788(10) 0.0526(8) Uani 0.101(4) 1 d . . P A 2
H28J H 0.6276 -0.0408 0.0554 0.063 Uiso 0.101(4) 1 calc R U P A 2
H28K H 0.5706 -0.0413 0.0782 0.063 Uiso 0.101(4) 1 calc R U P A 2
H28L H 0.6196 -0.0205 0.1111 0.063 Uiso 0.101(4) 1 calc R U P A 2
C285 C 0.6555(8) 0.1065(15) 0.0692(8) 0.0409(6) Uani 0.101(4) 1 d . . P A 2
H28M H 0.6768 0.0858 0.0430 0.049 Uiso 0.101(4) 1 calc R U P A 2
H28N H 0.6705 0.0914 0.1003 0.049 Uiso 0.101(4) 1 calc R U P A 2
H28O H 0.6546 0.1627 0.0670 0.049 Uiso 0.101(4) 1 calc R U P A 2
C286 C 0.5768(11) 0.087(2) 0.0201(9) 0.0537(8) Uani 0.101(4) 1 d . . P A 2
H28P H 0.6004 0.0673 -0.0048 0.064 Uiso 0.101(4) 1 calc R U P A 2
H28Q H 0.5719 0.1423 0.0156 0.064 Uiso 0.101(4) 1 calc R U P A 2
H28R H 0.5432 0.0609 0.0175 0.064 Uiso 0.101(4) 1 calc R U P A 2
C371 C 0.35192(9) 0.27158(12) 0.36624(7) 0.0337(4) Uani 1 1 d . . . . .
H37A H 0.3692(10) 0.2785(14) 0.3358(9) 0.039(6) Uiso 1 1 d . . . . .
H37B H 0.3329(10) 0.3200(15) 0.3749(9) 0.040(6) Uiso 1 1 d . . . . .
H37C H 0.3782(10) 0.2613(14) 0.3916(9) 0.038(6) Uiso 1 1 d . . . . .
C372 C 0.27128(9) 0.22086(15) 0.32671(8) 0.0420(5) Uani 1 1 d . . . . .
H37D H 0.2535(11) 0.2713(17) 0.3352(10) 0.054(8) Uiso 1 1 d . . . . .
H37E H 0.2459(11) 0.1765(17) 0.3276(10) 0.051(7) Uiso 1 1 d . . . . .
H37F H 0.2861(10) 0.2260(15) 0.2943(9) 0.044(7) Uiso 1 1 d . . . . .
C373 C 0.28678(9) 0.19800(14) 0.41351(8) 0.0379(5) Uani 1 1 d . . . . .
H37G H 0.2694(10) 0.2490(15) 0.4208(9) 0.043(7) Uiso 1 1 d . . . . .
H37H H 0.3105(10) 0.1866(15) 0.4379(9) 0.041(7) Uiso 1 1 d . . . . .
H37I H 0.2620(10) 0.1561(15) 0.4149(9) 0.040(7) Uiso 1 1 d . . . . .
C381 C 0.38069(13) -0.04763(16) 0.45203(8) 0.0509(6) Uani 1 1 d . . . . .
H38A H 0.3625(12) -0.006(2) 0.4644(12) 0.067(10) Uiso 1 1 d . . . . .
H38B H 0.3801(12) -0.0919(19) 0.4732(11) 0.064(9) Uiso 1 1 d . . . . .
H38C H 0.4182(14) -0.0333(19) 0.4490(12) 0.072(10) Uiso 1 1 d . . . . .
C382 C 0.30080(18) -0.0911(2) 0.40894(13) 0.0879(14) Uani 1 1 d . . . . .
H38D H 0.3001(17) -0.138(2) 0.4281(16) 0.108(14) Uiso 1 1 d . . . . .
H38E H 0.2843(17) -0.104(3) 0.3766(17) 0.112(14) Uiso 1 1 d . . . . .
H38F H 0.282(2) -0.041(4) 0.428(2) 0.19(3) Uiso 1 1 d . . . . .
C383 C 0.3872(3) -0.14328(19) 0.38592(13) 0.112(2) Uani 1 1 d . . . . .
H38G H 0.4293(10) -0.1243(16) 0.3907(10) 0.040(8) Uiso 1 1 d . . . . .
H38H H 0.3804(19) -0.160(3) 0.3568(19) 0.118(17) Uiso 1 1 d . . . . .
H38I H 0.3848(16) -0.183(3) 0.4103(16) 0.109(14) Uiso 1 1 d . . . . .
C71 C 0.5094(2) 0.8735(3) 0.5920(3) 0.151(3) Uani 1 1 d . . . . .
D71 D 0.5133 0.9076 0.6185 0.182 Uiso 1 1 calc R U . . .
C72 C 0.4997(3) 0.9023(5) 0.5450(5) 0.207(6) Uani 1 1 d . . . . .
D72 D 0.4947 0.9555 0.5389 0.249 Uiso 1 1 calc R U . . .
C73 C 0.4978(3) 0.8441(6) 0.5063(4) 0.236(7) Uani 1 1 d . . . . .
D73 D 0.4931 0.8622 0.4743 0.284 Uiso 1 1 calc R U . . .
C74 C 0.50255(14) 0.7606(4) 0.51310(18) 0.122(2) Uani 1 1 d . . . . .
D74 D 0.5007 0.7248 0.4873 0.147 Uiso 1 1 calc R U . . .
C75 C 0.50980(16) 0.7396(3) 0.5598(2) 0.1096(17) Uani 1 1 d . . . . .
D75 D 0.5128 0.6866 0.5675 0.132 Uiso 1 1 calc R U . . .
C76 C 0.51313(17) 0.7969(3) 0.5984(2) 0.1142(18) Uani 1 1 d . . . . .
D76 D 0.5183 0.7786 0.6303 0.137 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ru N1 1.9856(13) . ?
Ru N3 1.9902(13) . ?
Ru N2 1.9951(13) . ?
Ru O3 2.0149(11) . ?
Ru O1 2.0269(11) . ?
Ru O2 2.0280(11) . ?
Ru N10 3.3008(14) . ?
O1 C11 1.307(2) . ?
N1 C12 1.356(2) . ?
N1 C112 1.427(2) . ?
O2 C21 1.306(2) . ?
N2 C22 1.347(2) . ?
N2 C212 1.425(2) . ?
O3 C31 1.309(2) . ?
N3 C32 1.357(2) . ?
N3 C132 1.423(2) . ?
N10 C211 1.417(2) . ?
N10 C111 1.424(2) . ?
N10 C131 1.424(2) . ?
C11 C16 1.428(2) . ?
C11 C12 1.439(2) . ?
C12 C13 1.413(2) . ?
C13 C14 1.372(2) . ?
C13 H13 0.95(2) . ?
C14 C15 1.428(2) . ?
C14 C18 1.530(2) . ?
C15 C16 1.381(2) . ?
C15 H15 0.99(2) . ?
C16 C17 1.536(2) . ?
C17 C172 1.531(3) . ?
C17 C171 1.536(3) . ?
C17 C173 1.537(2) . ?
C18 C182 1.531(2) . ?
C18 C181 1.531(3) . ?
C18 C183 1.537(3) . ?
C21 C26 1.426(2) . ?
C21 C22 1.435(2) . ?
C22 C23 1.412(2) . ?
C23 C24 1.370(2) . ?
C23 H23 0.95(2) . ?
C24 C25 1.432(3) . ?
C24 C28 1.534(2) . ?
C25 C26 1.378(2) . ?
C25 H25 0.96(2) . ?
C26 C27 1.537(2) . ?
C27 C272 1.532(2) . ?
C27 C273 1.532(3) . ?
C27 C271 1.536(3) . ?
C28 C286 1.38(2) . ?
C28 C283 1.524(3) . ?
C28 C281 1.534(4) . ?
C28 C282 1.544(3) . ?
C28 C285 1.60(2) . ?
C28 C284 1.61(3) . ?
C31 C36 1.425(2) . ?
C31 C32 1.434(2) . ?
C32 C33 1.413(2) . ?
C33 C34 1.373(3) . ?
C33 H33 0.96(2) . ?
C34 C35 1.422(3) . ?
C34 C38 1.533(3) . ?
C35 C36 1.377(3) . ?
C35 H35 0.99(2) . ?
C36 C37 1.529(2) . ?
C37 C371 1.531(3) . ?
C37 C373 1.532(2) . ?
C37 C372 1.540(3) . ?
C38 C383 1.502(4) . ?
C38 C381 1.527(3) . ?
C38 C382 1.561(5) . ?
C111 C116 1.390(2) . ?
C111 C112 1.407(2) . ?
C112 C113 1.390(2) . ?
C113 C114 1.396(2) . ?
C113 H113 0.98(2) . ?
C114 C115 1.393(3) . ?
C114 C117 1.506(2) . ?
C115 C116 1.387(3) . ?
C115 H115 0.95(2) . ?
C116 H116 0.95(2) . ?
C117 H11A 0.97(3) . ?
C117 H11B 0.93(3) . ?
C117 H11C 0.99(4) . ?
C211 C216 1.391(2) . ?
C211 C212 1.394(2) . ?
C212 C213 1.391(2) . ?
C213 C214 1.394(2) . ?
C213 H213 0.96(2) . ?
C214 C215 1.391(3) . ?
C214 C217 1.504(2) . ?
C215 C216 1.391(2) . ?
C215 H215 0.96(2) . ?
C216 H216 0.97(2) . ?
C217 H21A 0.90(3) . ?
C217 H21B 1.01(3) . ?
C217 H21C 0.96(4) . ?
C131 C136 1.389(2) . ?
C131 C132 1.406(2) . ?
C132 C133 1.393(2) . ?
C133 C134 1.389(3) . ?
C133 H133 0.96(2) . ?
C134 C135 1.396(3) . ?
C134 C137 1.508(3) . ?
C135 C136 1.387(3) . ?
C135 H135 0.94(2) . ?
C136 H136 0.94(2) . ?
C137 H13A 0.92(3) . ?
C137 H13B 0.90(4) . ?
C137 H13C 0.92(4) . ?
C171 H17A 0.97(3) . ?
C171 H17B 0.94(3) . ?
C171 H17C 1.04(3) . ?
C172 H17D 0.90(3) . ?
C172 H17E 1.04(3) . ?
C172 H17F 0.98(3) . ?
C173 H17G 0.97(3) . ?
C173 H17H 0.99(3) . ?
C173 H17I 1.00(2) . ?
C181 H18A 0.99(3) . ?
C181 H18B 0.94(3) . ?
C181 H18C 0.96(3) . ?
C182 H18D 0.99(3) . ?
C182 H18E 0.97(3) . ?
C182 H18F 0.98(3) . ?
C183 H18G 0.97(3) . ?
C183 H18H 1.00(3) . ?
C183 H18I 0.98(3) . ?
C271 H27A 0.99(3) . ?
C271 H27B 1.00(3) . ?
C271 H27C 0.99(3) . ?
C272 H27D 0.99(3) . ?
C272 H27E 1.00(3) . ?
C272 H27F 0.98(3) . ?
C273 H27G 1.02(3) . ?
C273 H27H 0.95(3) . ?
C273 H27I 0.94(3) . ?
C281 H28A 1.00(4) . ?
C281 H28B 0.94(4) . ?
C281 H28C 1.09(4) . ?
C282 H28D 0.97(3) . ?
C282 H28E 1.02(3) . ?
C282 H28F 1.06(3) . ?
C283 H28G 1.02(3) . ?
C283 H28H 0.96(4) . ?
C283 H28I 1.00(4) . ?
C284 H28J 0.9800 . ?
C284 H28K 0.9800 . ?
C284 H28L 0.9800 . ?
C285 H28M 0.9800 . ?
C285 H28N 0.9800 . ?
C285 H28O 0.9800 . ?
C286 H28P 0.9800 . ?
C286 H28Q 0.9800 . ?
C286 H28R 0.9800 . ?
C371 H37A 0.96(3) . ?
C371 H37B 1.00(3) . ?
C371 H37C 0.99(3) . ?
C372 H37D 1.02(3) . ?
C372 H37E 1.01(3) . ?
C372 H37F 0.98(3) . ?
C373 H37G 1.01(3) . ?
C373 H37H 0.93(3) . ?
C373 H37I 0.97(3) . ?
C381 H38A 0.93(3) . ?
C381 H38B 0.97(3) . ?
C381 H38C 1.00(3) . ?
C382 H38D 0.98(4) . ?
C382 H38E 1.02(5) . ?
C382 H38F 1.13(6) . ?
C383 H38G 1.14(3) . ?
C383 H38H 0.88(5) . ?
C383 H38I 0.97(5) . ?
C71 C76 1.350(7) . ?
C71 C72 1.419(12) . ?
C71 D71 0.9500 . ?
C72 C73 1.478(15) . ?
C72 D72 0.9500 . ?
C73 C74 1.471(11) . ?
C73 D73 0.9500 . ?
C74 C75 1.359(6) . ?
C74 D74 0.9500 . ?
C75 C76 1.467(7) . ?
C75 D75 0.9500 . ?
C76 D76 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ru N3 94.23(5) . . ?
N1 Ru N2 94.95(5) . . ?
N3 Ru N2 96.86(5) . . ?
N1 Ru O3 90.99(5) . . ?
N3 Ru O3 79.06(5) . . ?
N2 Ru O3 173.04(5) . . ?
N1 Ru O1 78.95(5) . . ?
N3 Ru O1 170.66(5) . . ?
N2 Ru O1 90.14(5) . . ?
O3 Ru O1 94.56(5) . . ?
N1 Ru O2 171.89(5) . . ?
N3 Ru O2 90.87(5) . . ?
N2 Ru O2 78.15(5) . . ?
O3 Ru O2 96.17(5) . . ?
O1 Ru O2 96.64(5) . . ?
N1 Ru N10 58.91(4) . . ?
N3 Ru N10 59.11(5) . . ?
N2 Ru N10 57.87(4) . . ?
O3 Ru N10 123.12(4) . . ?
O1 Ru N10 120.82(4) . . ?
O2 Ru N10 119.22(4) . . ?
C11 O1 Ru 114.46(10) . . ?
C12 N1 C112 122.71(13) . . ?
C12 N1 Ru 116.35(11) . . ?
C112 N1 Ru 120.94(10) . . ?
C21 O2 Ru 115.50(10) . . ?
C22 N2 C212 122.52(13) . . ?
C22 N2 Ru 117.03(11) . . ?
C212 N2 Ru 120.30(10) . . ?
C31 O3 Ru 114.59(10) . . ?
C32 N3 C132 123.73(14) . . ?
C32 N3 Ru 116.06(11) . . ?
C132 N3 Ru 120.12(10) . . ?
C211 N10 C111 117.37(13) . . ?
C211 N10 C131 120.17(13) . . ?
C111 N10 C131 118.49(13) . . ?
C211 N10 Ru 83.83(9) . . ?
C111 N10 Ru 84.07(9) . . ?
C131 N10 Ru 82.19(9) . . ?
O1 C11 C16 123.72(14) . . ?
O1 C11 C12 116.68(14) . . ?
C16 C11 C12 119.54(15) . . ?
N1 C12 C13 126.14(15) . . ?
N1 C12 C11 112.70(14) . . ?
C13 C12 C11 121.08(14) . . ?
C14 C13 C12 119.47(15) . . ?
C14 C13 H13 120.9(13) . . ?
C12 C13 H13 119.6(13) . . ?
C13 C14 C15 118.69(15) . . ?
C13 C14 C18 122.86(15) . . ?
C15 C14 C18 118.40(14) . . ?
C16 C15 C14 124.67(15) . . ?
C16 C15 H15 117.5(12) . . ?
C14 C15 H15 117.7(12) . . ?
C15 C16 C11 116.46(15) . . ?
C15 C16 C17 122.73(15) . . ?
C11 C16 C17 120.79(15) . . ?
C172 C17 C16 108.75(14) . . ?
C172 C17 C171 110.53(18) . . ?
C16 C17 C171 110.85(14) . . ?
C172 C17 C173 108.76(16) . . ?
C16 C17 C173 111.74(15) . . ?
C171 C17 C173 106.18(16) . . ?
C14 C18 C182 109.98(14) . . ?
C14 C18 C181 112.12(14) . . ?
C182 C18 C181 108.43(16) . . ?
C14 C18 C183 108.60(15) . . ?
C182 C18 C183 110.09(17) . . ?
C181 C18 C183 107.59(16) . . ?
O2 C21 C26 124.46(15) . . ?
O2 C21 C22 116.24(14) . . ?
C26 C21 C22 119.25(15) . . ?
N2 C22 C23 125.73(15) . . ?
N2 C22 C21 112.78(14) . . ?
C23 C22 C21 121.40(15) . . ?
C24 C23 C22 119.44(16) . . ?
C24 C23 H23 122.2(13) . . ?
C22 C23 H23 118.4(13) . . ?
C23 C24 C25 118.57(15) . . ?
C23 C24 C28 121.94(16) . . ?
C25 C24 C28 119.43(16) . . ?
C26 C25 C24 124.48(16) . . ?
C26 C25 H25 116.0(12) . . ?
C24 C25 H25 119.5(12) . . ?
C25 C26 C21 116.83(15) . . ?
C25 C26 C27 123.40(15) . . ?
C21 C26 C27 119.69(15) . . ?
C272 C27 C273 108.09(16) . . ?
C272 C27 C271 108.38(17) . . ?
C273 C27 C271 109.83(17) . . ?
C272 C27 C26 112.00(15) . . ?
C273 C27 C26 109.60(15) . . ?
C271 C27 C26 108.91(15) . . ?
C283 C28 C281 110.8(2) . . ?
C286 C28 C24 111.4(10) . . ?
C283 C28 C24 109.18(17) . . ?
C281 C28 C24 109.63(18) . . ?
C283 C28 C282 108.0(2) . . ?
C281 C28 C282 107.1(2) . . ?
C24 C28 C282 112.09(16) . . ?
C286 C28 C285 111.6(17) . . ?
C24 C28 C285 112.2(7) . . ?
C286 C28 C284 114.8(18) . . ?
C24 C28 C284 102.8(9) . . ?
C285 C28 C284 103.5(14) . . ?
O3 C31 C36 123.26(16) . . ?
O3 C31 C32 116.79(14) . . ?
C36 C31 C32 119.90(15) . . ?
N3 C32 C33 126.51(16) . . ?
N3 C32 C31 112.62(15) . . ?
C33 C32 C31 120.77(15) . . ?
C34 C33 C32 119.30(17) . . ?
C34 C33 H33 122.4(14) . . ?
C32 C33 H33 118.2(14) . . ?
C33 C34 C35 118.97(17) . . ?
C33 C34 C38 123.15(19) . . ?
C35 C34 C38 117.81(18) . . ?
C36 C35 C34 124.54(16) . . ?
C36 C35 H35 115.5(14) . . ?
C34 C35 H35 120.0(14) . . ?
C35 C36 C31 116.43(16) . . ?
C35 C36 C37 122.91(16) . . ?
C31 C36 C37 120.53(16) . . ?
C36 C37 C371 110.34(15) . . ?
C36 C37 C373 111.83(17) . . ?
C371 C37 C373 108.49(15) . . ?
C36 C37 C372 109.19(15) . . ?
C371 C37 C372 109.65(18) . . ?
C373 C37 C372 107.28(17) . . ?
C383 C38 C381 110.1(3) . . ?
C383 C38 C34 112.3(2) . . ?
C381 C38 C34 109.90(18) . . ?
C383 C38 C382 108.6(4) . . ?
C381 C38 C382 108.0(2) . . ?
C34 C38 C382 107.8(2) . . ?
C116 C111 C112 119.20(15) . . ?
C116 C111 N10 119.83(15) . . ?
C112 C111 N10 120.95(14) . . ?
C113 C112 C111 119.72(15) . . ?
C113 C112 N1 120.42(14) . . ?
C111 C112 N1 119.14(14) . . ?
C112 C113 C114 120.91(16) . . ?
C112 C113 H113 118.8(12) . . ?
C114 C113 H113 119.8(12) . . ?
C115 C114 C113 118.87(16) . . ?
C115 C114 C117 120.84(17) . . ?
C113 C114 C117 120.24(17) . . ?
C116 C115 C114 120.65(16) . . ?
C116 C115 H115 118.0(14) . . ?
C114 C115 H115 121.4(14) . . ?
C115 C116 C111 120.59(16) . . ?
C115 C116 H116 120.7(14) . . ?
C111 C116 H116 118.6(14) . . ?
C114 C117 H11A 113.7(18) . . ?
C114 C117 H11B 112(2) . . ?
H11A C117 H11B 108(3) . . ?
C114 C117 H11C 111(2) . . ?
H11A C117 H11C 99(3) . . ?
H11B C117 H11C 111(3) . . ?
C216 C211 C212 119.09(15) . . ?
C216 C211 N10 119.87(15) . . ?
C212 C211 N10 120.87(14) . . ?
C213 C212 C211 120.32(15) . . ?
C213 C212 N2 120.21(15) . . ?
C211 C212 N2 118.42(14) . . ?
C212 C213 C214 120.61(16) . . ?
C212 C213 H213 117.9(13) . . ?
C214 C213 H213 121.2(13) . . ?
C215 C214 C213 118.73(16) . . ?
C215 C214 C217 121.45(17) . . ?
C213 C214 C217 119.73(18) . . ?
C214 C215 C216 120.77(16) . . ?
C214 C215 H215 119.5(14) . . ?
C216 C215 H215 119.7(14) . . ?
C211 C216 C215 120.36(16) . . ?
C211 C216 H216 118.9(13) . . ?
C215 C216 H216 120.7(13) . . ?
C214 C217 H21A 111(2) . . ?
C214 C217 H21B 110.8(18) . . ?
H21A C217 H21B 107(3) . . ?
C214 C217 H21C 110(2) . . ?
H21A C217 H21C 108(3) . . ?
H21B C217 H21C 110(3) . . ?
C136 C131 C132 118.85(15) . . ?
C136 C131 N10 120.13(15) . . ?
C132 C131 N10 121.01(14) . . ?
C133 C132 C131 119.83(15) . . ?
C133 C132 N3 120.30(15) . . ?
C131 C132 N3 119.02(14) . . ?
C134 C133 C132 121.14(16) . . ?
C134 C133 H133 119.9(13) . . ?
C132 C133 H133 118.7(13) . . ?
C133 C134 C135 118.43(16) . . ?
C133 C134 C137 120.32(18) . . ?
C135 C134 C137 121.25(18) . . ?
C136 C135 C134 120.93(16) . . ?
C136 C135 H135 119.1(14) . . ?
C134 C135 H135 119.9(14) . . ?
C135 C136 C131 120.58(16) . . ?
C135 C136 H136 119.7(14) . . ?
C131 C136 H136 119.7(15) . . ?
C134 C137 H13A 112.4(18) . . ?
C134 C137 H13B 112(2) . . ?
H13A C137 H13B 108(3) . . ?
C134 C137 H13C 109(2) . . ?
H13A C137 H13C 102(3) . . ?
H13B C137 H13C 112(3) . . ?
C17 C171 H17A 109.8(18) . . ?
C17 C171 H17B 113.6(18) . . ?
H17A C171 H17B 110(3) . . ?
C17 C171 H17C 108.7(14) . . ?
H17A C171 H17C 109(2) . . ?
H17B C171 H17C 105(2) . . ?
C17 C172 H17D 110.6(16) . . ?
C17 C172 H17E 109.9(15) . . ?
H17D C172 H17E 108(2) . . ?
C17 C172 H17F 107.4(15) . . ?
H17D C172 H17F 112(2) . . ?
H17E C172 H17F 109(2) . . ?
C17 C173 H17G 111.4(15) . . ?
C17 C173 H17H 110.2(16) . . ?
H17G C173 H17H 110(2) . . ?
C17 C173 H17I 108.9(13) . . ?
H17G C173 H17I 107(2) . . ?
H17H C173 H17I 109(2) . . ?
C18 C181 H18A 109.3(15) . . ?
C18 C181 H18B 106.2(15) . . ?
H18A C181 H18B 111(2) . . ?
C18 C181 H18C 107.9(15) . . ?
H18A C181 H18C 110(2) . . ?
H18B C181 H18C 113(2) . . ?
C18 C182 H18D 112.1(16) . . ?
C18 C182 H18E 110.5(16) . . ?
H18D C182 H18E 107(2) . . ?
C18 C182 H18F 109.3(15) . . ?
H18D C182 H18F 112(2) . . ?
H18E C182 H18F 107(2) . . ?
C18 C183 H18G 110.1(19) . . ?
C18 C183 H18H 109.1(16) . . ?
H18G C183 H18H 109(2) . . ?
C18 C183 H18I 110.2(16) . . ?
H18G C183 H18I 109(2) . . ?
H18H C183 H18I 109(2) . . ?
C27 C271 H27A 109.5(16) . . ?
C27 C271 H27B 110.9(19) . . ?
H27A C271 H27B 110(2) . . ?
C27 C271 H27C 113.7(15) . . ?
H27A C271 H27C 104(2) . . ?
H27B C271 H27C 108(2) . . ?
C27 C272 H27D 111.5(15) . . ?
C27 C272 H27E 108.9(15) . . ?
H27D C272 H27E 108(2) . . ?
C27 C272 H27F 113.3(17) . . ?
H27D C272 H27F 107(2) . . ?
H27E C272 H27F 108(2) . . ?
C27 C273 H27G 110.1(16) . . ?
C27 C273 H27H 111.5(16) . . ?
H27G C273 H27H 111(2) . . ?
C27 C273 H27I 108.6(16) . . ?
H27G C273 H27I 108(2) . . ?
H27H C273 H27I 108(2) . . ?
C28 C281 H28A 108(2) . . ?
C28 C281 H28B 107(2) . . ?
H28A C281 H28B 108(3) . . ?
C28 C281 H28C 112.2(19) . . ?
H28A C281 H28C 112(3) . . ?
H28B C281 H28C 109(3) . . ?
C28 C282 H28D 107.3(18) . . ?
C28 C282 H28E 110.3(16) . . ?
H28D C282 H28E 110(2) . . ?
C28 C282 H28F 108.3(17) . . ?
H28D C282 H28F 107(2) . . ?
H28E C282 H28F 114(2) . . ?
C28 C283 H28G 111.9(19) . . ?
C28 C283 H28H 111(2) . . ?
H28G C283 H28H 104(3) . . ?
C28 C283 H28I 110(2) . . ?
H28G C283 H28I 114(3) . . ?
H28H C283 H28I 105(3) . . ?
C28 C284 H28J 109.5 . . ?
C28 C284 H28K 109.5 . . ?
H28J C284 H28K 109.5 . . ?
C28 C284 H28L 109.5 . . ?
H28J C284 H28L 109.5 . . ?
H28K C284 H28L 109.5 . . ?
C28 C285 H28M 109.5 . . ?
C28 C285 H28N 109.5 . . ?
H28M C285 H28N 109.5 . . ?
C28 C285 H28O 109.5 . . ?
H28M C285 H28O 109.5 . . ?
H28N C285 H28O 109.5 . . ?
C28 C286 H28P 109.5 . . ?
C28 C286 H28Q 109.5 . . ?
H28P C286 H28Q 109.5 . . ?
C28 C286 H28R 109.5 . . ?
H28P C286 H28R 109.5 . . ?
H28Q C286 H28R 109.5 . . ?
C37 C371 H37A 111.4(15) . . ?
C37 C371 H37B 109.7(14) . . ?
H37A C371 H37B 109(2) . . ?
C37 C371 H37C 108.9(14) . . ?
H37A C371 H37C 109(2) . . ?
H37B C371 H37C 108(2) . . ?
C37 C372 H37D 108.7(16) . . ?
C37 C372 H37E 107.5(16) . . ?
H37D C372 H37E 111(2) . . ?
C37 C372 H37F 111.3(15) . . ?
H37D C372 H37F 108(2) . . ?
H37E C372 H37F 110(2) . . ?
C37 C373 H37G 108.3(14) . . ?
C37 C373 H37H 111.4(16) . . ?
H37G C373 H37H 109(2) . . ?
C37 C373 H37I 112.8(15) . . ?
H37G C373 H37I 111(2) . . ?
H37H C373 H37I 104(2) . . ?
C38 C381 H38A 112(2) . . ?
C38 C381 H38B 108.2(19) . . ?
H38A C381 H38B 113(3) . . ?
C38 C381 H38C 109.6(19) . . ?
H38A C381 H38C 109(3) . . ?
H38B C381 H38C 105(3) . . ?
C38 C382 H38D 105(3) . . ?
C38 C382 H38E 111(2) . . ?
H38D C382 H38E 107(3) . . ?
C38 C382 H38F 108(3) . . ?
H38D C382 H38F 112(4) . . ?
H38E C382 H38F 114(4) . . ?
C38 C383 H38G 99.9(14) . . ?
C38 C383 H38H 118(3) . . ?
H38G C383 H38H 113(4) . . ?
C38 C383 H38I 110(3) . . ?
H38G C383 H38I 101(3) . . ?
H38H C383 H38I 113(4) . . ?
C76 C71 C72 118.8(8) . . ?
C76 C71 D71 120.6 . . ?
C72 C71 D71 120.6 . . ?
C71 C72 C73 115.6(7) . . ?
C71 C72 D72 122.2 . . ?
C73 C72 D72 122.2 . . ?
C74 C73 C72 125.5(7) . . ?
C74 C73 D73 117.2 . . ?
C72 C73 D73 117.2 . . ?
C75 C74 C73 113.6(7) . . ?
C75 C74 D74 123.2 . . ?
C73 C74 D74 123.2 . . ?
C74 C75 C76 121.4(6) . . ?
C74 C75 D75 119.3 . . ?
C76 C75 D75 119.3 . . ?
C71 C76 C75 124.9(6) . . ?
C71 C76 D76 117.6 . . ?
C75 C76 D76 117.6 . . ?

_refine_diff_density_max         0.631
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.053

_shelxl_version_number           2013-4

