# Electronic Supplementary Material (ESI) for Organic Chemistry Frontiers.
# This journal is © the Partner Organisations 2015

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1038533'
_audit_update_record             
;
2015-02-11 deposited with the CCDC.
2015-03-26 downloaded from the CCDC.
;
_audit_creation_date             2014-12-30
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4959)
;
_shelxl_version_number           2013-2
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C56 H48 Cl2 N O Os P2, 2(C H2 Cl2), B F4'
_chemical_formula_sum            'C58 H52 B Cl6 F4 N O Os P2'
_chemical_formula_weight         1330.65
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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                   16.5731(8)
_cell_length_b                   19.6848(7)
_cell_length_c                   18.1839(9)
_cell_angle_alpha                90
_cell_angle_beta                 112.182(2)
_cell_angle_gamma                90
_cell_volume                     5493.2(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      ?
_cell_measurement_theta_min      ?
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.727
_exptl_absorpt_correction_T_max  0.441
_exptl_absorpt_correction_T_min  0.212
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2656
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1019
_diffrn_reflns_av_unetI/netI     0.0854
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            38256
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.020
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7791
_reflns_number_total             9642
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         4.637
_refine_diff_density_min         -2.056
_refine_diff_density_rms         0.183
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     669
_refine_ls_number_reflns         9642
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_gt           0.0643
_refine_ls_restrained_S_all      1.084
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.1025P)²+14.8409P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1710
_refine_ls_wR_factor_ref         0.1873
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1A), C6(H6)
2.b Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C31(H31A,H31B)
2.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C353(H353), C336(H336), C26(H26), C23(H23), C332(H332), C16(H16),
 C322(H322), C12(H12), C13(H13), C362(H362), C326(H326), C364(H364), C324(H324),
  C14(H14), C22(H22), C366(H366), C365(H365), C25(H25), C335(H335), C363(H363),
 C323(H323), C333(H333), C325(H325), C312(H312), C334(H334), C314(H314),
 C313(H313), C352(H352), C356(H356), C342(H342), C354(H354), C355(H355),
 C346(H346), C345(H345), C343(H343), C344(H344), N1(H1), C315(H315), C316(H316)
2.d Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C27(H27A,H27B,H27C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Os1 Os 0.68334(2) 0.78113(2) 0.56035(2) 0.02667(15) Uani 1 1 d . . . . .
P2 P 0.64934(13) 0.83184(10) 0.73958(11) 0.0289(4) Uani 1 1 d . . . . .
P1 P 0.74077(14) 0.77181(10) 0.45876(12) 0.0304(5) Uani 1 1 d . . . . .
Cl1 Cl 0.71211(14) 0.90107(10) 0.55844(11) 0.0370(5) Uani 1 1 d . . . . .
Cl2 Cl 0.54095(13) 0.80300(12) 0.45670(11) 0.0413(5) Uani 1 1 d . . . . .
C341 C 0.7262(6) 0.8387(4) 0.3842(5) 0.043(2) Uani 1 1 d . . . . .
C3 C 0.7429(5) 0.7123(3) 0.7016(4) 0.0250(16) Uani 1 1 d . . . . .
C11 C 0.7469(5) 0.6667(4) 0.7708(4) 0.0291(17) Uani 1 1 d . . . . .
C331 C 0.7522(5) 0.8653(4) 0.8071(4) 0.0310(18) Uani 1 1 d . . . . .
C5 C 0.9133(5) 0.7487(5) 0.7726(5) 0.0379(19) Uani 1 1 d . . . . .
H5A H 0.9128 0.7773 0.8152 0.057 Uiso 1 1 calc GR . . . .
H5B H 0.9560 0.7651 0.7530 0.057 Uiso 1 1 calc GR . . . .
H5C H 0.9276 0.7031 0.7917 0.057 Uiso 1 1 calc GR . . . .
C351 C 0.8585(5) 0.7688(5) 0.5104(5) 0.0340(19) Uani 1 1 d . . . . .
C15 C 0.7919(6) 0.6481(5) 0.9126(5) 0.049(2) Uani 1 1 d . . . . .
H15 H 0.8227 0.6624 0.9644 0.059 Uiso 1 1 calc R . . . .
C361 C 0.7112(5) 0.6977(4) 0.3935(4) 0.0322(18) Uani 1 1 d . . . . .
C353 C 0.9889(7) 0.7084(6) 0.5915(6) 0.057(3) Uani 1 1 d . . . . .
H353 H 1.0170 0.6675 0.6108 0.069 Uiso 1 1 calc R . . . .
C21 C 0.7591(5) 0.6201(4) 0.6003(4) 0.0282(16) Uani 1 1 d . . . . .
C336 C 0.8061(5) 0.9013(4) 0.7770(5) 0.0342(18) Uani 1 1 d . . . . .
H336 H 0.7913 0.9058 0.7225 0.041 Uiso 1 1 calc R . . . .
C26 C 0.8439(5) 0.6030(4) 0.6527(5) 0.0385(19) Uani 1 1 d . . . . .
H26 H 0.8684 0.6251 0.7013 0.046 Uiso 1 1 calc R . . . .
C321 C 0.5900(5) 0.7967(4) 0.7950(5) 0.0361(19) Uani 1 1 d . . . . .
C23 C 0.7700(6) 0.5337(4) 0.5105(5) 0.043(2) Uani 1 1 d . . . . .
H23 H 0.7439 0.5099 0.4632 0.052 Uiso 1 1 calc R . . . .
C332 C 0.7757(6) 0.8582(5) 0.8895(5) 0.043(2) Uani 1 1 d . . . . .
H332 H 0.7399 0.8343 0.9094 0.052 Uiso 1 1 calc R . . . .
C311 C 0.5836(6) 0.8999(4) 0.6812(5) 0.041(2) Uani 1 1 d . . . . .
C16 C 0.7916(5) 0.6874(4) 0.8492(4) 0.0355(19) Uani 1 1 d . . . . .
H16 H 0.8219 0.7283 0.8592 0.043 Uiso 1 1 calc R . . . .
C322 C 0.5697(6) 0.7287(4) 0.7942(6) 0.041(2) Uani 1 1 d . . . . .
H322 H 0.5846 0.6991 0.7615 0.050 Uiso 1 1 calc R . . . .
C12 C 0.7009(5) 0.6066(4) 0.7575(5) 0.0353(19) Uani 1 1 d . . . . .
H12 H 0.6702 0.5924 0.7056 0.042 Uiso 1 1 calc R . . . .
C13 C 0.6996(6) 0.5666(4) 0.8203(5) 0.043(2) Uani 1 1 d . . . . .
H13 H 0.6680 0.5263 0.8102 0.052 Uiso 1 1 calc R . . . .
C362 C 0.6268(6) 0.6715(4) 0.3683(5) 0.040(2) Uani 1 1 d . . . . .
H362 H 0.5874 0.6902 0.3880 0.048 Uiso 1 1 calc R . . . .
C326 C 0.5636(6) 0.8416(5) 0.8419(6) 0.050(2) Uani 1 1 d . . . . .
H326 H 0.5749 0.8878 0.8413 0.060 Uiso 1 1 calc R . . . .
C364 C 0.6599(7) 0.5903(5) 0.2845(5) 0.052(2) Uani 1 1 d . . . . .
H364 H 0.6424 0.5552 0.2476 0.062 Uiso 1 1 calc R . . . .
C324 C 0.5057(7) 0.7480(6) 0.8904(6) 0.061(3) Uani 1 1 d . . . . .
H324 H 0.4806 0.7310 0.9245 0.073 Uiso 1 1 calc R . . . .
C14 C 0.7460(7) 0.5873(5) 0.8985(5) 0.047(2) Uani 1 1 d . . . . .
H14 H 0.7462 0.5606 0.9407 0.057 Uiso 1 1 calc R . . . .
C22 C 0.7243(5) 0.5820(4) 0.5314(4) 0.0324(18) Uani 1 1 d . . . . .
H22 H 0.6668 0.5899 0.4979 0.039 Uiso 1 1 calc R . . . .
C366 C 0.7698(6) 0.6686(5) 0.3617(5) 0.046(2) Uani 1 1 d . . . . .
H366 H 0.8257 0.6862 0.3762 0.056 Uiso 1 1 calc R . . . .
C24 C 0.8551(6) 0.5201(4) 0.5591(5) 0.042(2) Uani 1 1 d . . . . .
C365 C 0.7445(7) 0.6150(5) 0.3100(6) 0.055(3) Uani 1 1 d . . . . .
H365 H 0.7843 0.5951 0.2918 0.066 Uiso 1 1 calc R . . . .
C25 C 0.8909(6) 0.5539(4) 0.6326(5) 0.041(2) Uani 1 1 d . . . . .
H25 H 0.9467 0.5429 0.6678 0.049 Uiso 1 1 calc R . . . .
C335 C 0.8812(6) 0.9299(4) 0.8296(5) 0.041(2) Uani 1 1 d . . . . .
H335 H 0.9170 0.9542 0.8103 0.049 Uiso 1 1 calc R . . . .
C363 C 0.6007(6) 0.6183(5) 0.3147(5) 0.050(2) Uani 1 1 d . . . . .
H363 H 0.5443 0.6013 0.2987 0.060 Uiso 1 1 calc R . . . .
C323 C 0.5275(7) 0.7039(6) 0.8417(7) 0.057(3) Uani 1 1 d . . . . .
H323 H 0.5139 0.6579 0.8408 0.068 Uiso 1 1 calc R . . . .
C333 C 0.8523(6) 0.8869(5) 0.9406(5) 0.049(2) Uani 1 1 d . . . . .
H333 H 0.8685 0.8818 0.9951 0.059 Uiso 1 1 calc R . . . .
C325 C 0.5207(7) 0.8171(6) 0.8894(6) 0.063(3) Uani 1 1 d . . . . .
H325 H 0.5024 0.8467 0.9198 0.076 Uiso 1 1 calc R . . . .
C312 C 0.6154(7) 0.9647(5) 0.6826(7) 0.057(3) Uani 1 1 d . . . . .
H312 H 0.6723 0.9749 0.7158 0.069 Uiso 1 1 calc R . . . .
C334 C 0.9051(6) 0.9232(5) 0.9116(5) 0.050(2) Uani 1 1 d . . . . .
H334 H 0.9561 0.9430 0.9464 0.060 Uiso 1 1 calc R . . . .
C314 C 0.4776(11) 1.0028(7) 0.5864(7) 0.095(5) Uani 1 1 d . . . . .
H314 H 0.4430 1.0363 0.5533 0.114 Uiso 1 1 calc R . . . .
C313 C 0.5626(9) 1.0149(6) 0.6347(9) 0.081(4) Uani 1 1 d . . . . .
H313 H 0.5857 1.0581 0.6354 0.097 Uiso 1 1 calc R . . . .
C352 C 0.9037(6) 0.7084(5) 0.5407(5) 0.046(2) Uani 1 1 d . . . . .
H352 H 0.8748 0.6671 0.5258 0.056 Uiso 1 1 calc R . . . .
C356 C 0.9064(7) 0.8295(5) 0.5329(6) 0.052(2) Uani 1 1 d . . . . .
H356 H 0.8798 0.8704 0.5116 0.063 Uiso 1 1 calc R . . . .
C342 C 0.6574(7) 0.8826(5) 0.3620(5) 0.054(3) Uani 1 1 d . . . . .
H342 H 0.6178 0.8804 0.3870 0.064 Uiso 1 1 calc R . . . .
C354 C 1.0340(8) 0.7694(7) 0.6147(7) 0.069(3) Uani 1 1 d . . . . .
H354 H 1.0921 0.7695 0.6493 0.082 Uiso 1 1 calc R . . . .
C355 C 0.9916(7) 0.8298(6) 0.5857(6) 0.062(3) Uani 1 1 d . . . . .
H355 H 1.0207 0.8708 0.6018 0.075 Uiso 1 1 calc R . . . .
C346 C 0.7843(8) 0.8424(5) 0.3445(6) 0.061(3) Uani 1 1 d . . . . .
H346 H 0.8305 0.8119 0.3578 0.073 Uiso 1 1 calc R . . . .
C345 C 0.7743(10) 0.8898(6) 0.2865(7) 0.074(4) Uani 1 1 d . . . . .
H345 H 0.8139 0.8920 0.2615 0.089 Uiso 1 1 calc R . . . .
C343 C 0.6450(8) 0.9309(5) 0.3021(6) 0.068(3) Uani 1 1 d . . . . .
H343 H 0.5975 0.9602 0.2872 0.082 Uiso 1 1 calc R . . . .
C344 C 0.7044(10) 0.9346(6) 0.2653(6) 0.084(4) Uani 1 1 d . . . . .
H344 H 0.6975 0.9671 0.2263 0.101 Uiso 1 1 calc R . . . .
O1 O 0.9106(4) 0.4757(3) 0.5425(4) 0.0528(17) Uani 1 1 d . . . . .
C27 C 0.8781(9) 0.4529(6) 0.4620(7) 0.079(4) Uani 1 1 d . . . . .
H27A H 0.8478 0.4894 0.4276 0.118 Uiso 1 1 calc GR . . . .
H27B H 0.8389 0.4156 0.4560 0.118 Uiso 1 1 calc GR . . . .
H27C H 0.9259 0.4384 0.4481 0.118 Uiso 1 1 calc GR . . . .
Cl31 Cl 0.7859(3) 0.2652(2) 0.4548(3) 0.1102(13) Uani 1 1 d . . . . .
Cl32 Cl 0.3141(4) 0.4202(3) -0.0789(3) 0.1387(18) Uani 1 1 d . . . . .
N1 N 0.8085(4) 0.7826(3) 0.6434(4) 0.0312(16) Uani 1 1 d . . . . .
H1 H 0.8486 0.8052 0.6351 0.037 Uiso 1 1 calc R . . . .
Cl3 Cl 0.4356(3) 0.4832(3) 0.0635(3) 0.1389(18) Uani 1 1 d . . . . .
Cl4 Cl 0.6736(5) 0.2089(3) 0.3103(4) 0.208(4) Uani 1 1 d . . . . .
F2 F 0.5552(4) 0.4800(3) 0.3971(4) 0.0709(18) Uani 1 1 d . . . . .
F3 F 0.6497(4) 0.4270(3) 0.3577(4) 0.0637(16) Uani 1 1 d . . . . .
F1 F 0.5168(4) 0.4563(4) 0.2664(3) 0.0774(19) Uani 1 1 d . . . . .
F4 F 0.5311(4) 0.3707(3) 0.3554(4) 0.0741(18) Uani 1 1 d . . . . .
C4 C 0.8251(5) 0.7497(4) 0.7068(4) 0.0281(17) Uani 1 1 d . . . . .
B1 B 0.5621(8) 0.4328(6) 0.3434(6) 0.051(3) Uani 1 1 d . . . . .
C315 C 0.4464(11) 0.9391(9) 0.5896(10) 0.154(10) Uani 1 1 d . . . . .
H315 H 0.3887 0.9298 0.5578 0.185 Uiso 1 1 calc R . . . .
C316 C 0.4970(8) 0.8864(7) 0.6385(8) 0.103(6) Uani 1 1 d . . . . .
H316 H 0.4726 0.8444 0.6417 0.124 Uiso 1 1 calc R . . . .
C32 C 0.3577(10) 0.4903(7) -0.0345(8) 0.088(4) Uani 1 1 d . . . . .
H32A H 0.3113 0.5198 -0.0335 0.105 Uiso 1 1 calc R . . . .
H32B H 0.3853 0.5127 -0.0665 0.105 Uiso 1 1 calc R . . . .
C31 C 0.6983(14) 0.2702(8) 0.3708(15) 0.158(10) Uani 1 1 d . . . . .
H31A H 0.6485 0.2787 0.3853 0.189 Uiso 1 1 calc R . . . .
H31B H 0.7053 0.3100 0.3424 0.189 Uiso 1 1 calc R . . . .
C2 C 0.6657(5) 0.7666(4) 0.6769(4) 0.0279(16) Uani 1 1 d . . . . .
C1 C 0.5935(5) 0.7417(4) 0.6139(4) 0.0293(17) Uani 1 1 d . . . . .
H1A H 0.5332 0.7566 0.6004 0.035 Uiso 1 1 calc R . . . .
C6 C 0.6205(5) 0.6876(4) 0.5766(4) 0.0316(18) Uani 1 1 d . . . . .
H6 H 0.5814 0.6592 0.5335 0.038 Uiso 1 1 calc R . . . .
C7 C 0.7105(5) 0.6751(3) 0.6187(4) 0.0257(16) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Os1 P1 2.383(2) . ?
Os1 Cl1 2.411(2) . ?
Os1 Cl2 2.4388(19) . ?
Os1 N1 2.054(7) . ?
Os1 C2 2.264(7) . ?
Os1 C1 2.206(7) . ?
Os1 C6 2.190(8) . ?
Os1 C7 2.307(7) . ?
P2 C331 1.807(8) . ?
P2 C321 1.792(9) . ?
P2 C311 1.799(8) . ?
P2 C2 1.805(8) . ?
P1 C341 1.839(9) . ?
P1 C351 1.819(9) . ?
P1 C361 1.828(8) . ?
C341 C342 1.365(14) . ?
C341 C346 1.407(13) . ?
C3 C11 1.526(10) . ?
C3 C4 1.520(11) . ?
C3 C2 1.595(11) . ?
C3 C7 1.577(10) . ?
C11 C16 1.396(10) . ?
C11 C12 1.380(11) . ?
C331 C336 1.404(11) . ?
C331 C332 1.406(11) . ?
C5 C4 1.500(10) . ?
C351 C352 1.402(13) . ?
C351 C356 1.407(13) . ?
C15 C16 1.386(12) . ?
C15 C14 1.388(13) . ?
C361 C362 1.396(12) . ?
C361 C366 1.423(12) . ?
C353 C352 1.365(14) . ?
C353 C354 1.393(16) . ?
C21 C26 1.409(11) . ?
C21 C22 1.385(10) . ?
C21 C7 1.461(10) . ?
C336 C335 1.371(11) . ?
C26 C25 1.373(12) . ?
C321 C322 1.379(12) . ?
C321 C326 1.407(12) . ?
C23 C22 1.356(12) . ?
C23 C24 1.379(13) . ?
C332 C333 1.380(12) . ?
C311 C312 1.377(13) . ?
C311 C316 1.377(14) . ?
C322 C323 1.391(13) . ?
C12 C13 1.393(12) . ?
C13 C14 1.398(12) . ?
C362 C363 1.385(12) . ?
C326 C325 1.396(13) . ?
C364 C365 1.388(14) . ?
C364 C363 1.405(14) . ?
C324 C323 1.382(15) . ?
C324 C325 1.383(17) . ?
C366 C365 1.369(12) . ?
C24 C25 1.408(12) . ?
C24 O1 1.381(10) . ?
C335 C334 1.397(12) . ?
C333 C334 1.378(14) . ?
C312 C313 1.387(14) . ?
C314 C313 1.37(2) . ?
C314 C315 1.37(2) . ?
C356 C355 1.375(14) . ?
C342 C343 1.401(13) . ?
C354 C355 1.380(17) . ?
C346 C345 1.371(14) . ?
C345 C344 1.389(18) . ?
C343 C344 1.385(18) . ?
O1 C27 1.429(12) . ?
Cl31 C31 1.67(2) . ?
Cl32 C32 1.625(14) . ?
N1 C4 1.258(10) . ?
Cl3 C32 1.768(15) . ?
Cl4 C31 1.579(18) . ?
F2 B1 1.383(13) . ?
F3 B1 1.379(13) . ?
F1 B1 1.394(11) . ?
F4 B1 1.376(14) . ?
C315 C316 1.42(2) . ?
C2 C1 1.395(10) . ?
C1 C6 1.424(11) . ?
C6 C7 1.419(10) . ?

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
P1 Os1 Cl1 85.71(7) . . ?
P1 Os1 Cl2 88.15(7) . . ?
Cl1 Os1 Cl2 87.42(7) . . ?
N1 Os1 P1 89.0(2) . . ?
N1 Os1 Cl1 81.18(18) . . ?
N1 Os1 Cl2 168.43(18) . . ?
N1 Os1 C2 76.4(3) . . ?
N1 Os1 C1 110.0(3) . . ?
N1 Os1 C6 108.2(3) . . ?
N1 Os1 C7 72.9(3) . . ?
C2 Os1 P1 161.1(2) . . ?
C2 Os1 Cl1 103.5(2) . . ?
C2 Os1 Cl2 108.4(2) . . ?
C2 Os1 C7 61.8(3) . . ?
C1 Os1 P1 148.1(2) . . ?
C1 Os1 Cl1 121.4(2) . . ?
C1 Os1 Cl2 77.6(2) . . ?
C1 Os1 C2 36.3(3) . . ?
C1 Os1 C7 61.7(3) . . ?
C6 Os1 P1 112.9(2) . . ?
C6 Os1 Cl1 158.7(2) . . ?
C6 Os1 Cl2 83.20(19) . . ?
C6 Os1 C2 62.1(3) . . ?
C6 Os1 C1 37.8(3) . . ?
C6 Os1 C7 36.7(3) . . ?
C7 Os1 P1 102.76(19) . . ?
C7 Os1 Cl1 152.49(18) . . ?
C7 Os1 Cl2 118.62(19) . . ?
C321 P2 C331 109.7(4) . . ?
C321 P2 C311 106.3(4) . . ?
C321 P2 C2 109.0(4) . . ?
C311 P2 C331 109.6(4) . . ?
C311 P2 C2 111.0(4) . . ?
C2 P2 C331 111.1(4) . . ?
C341 P1 Os1 122.4(3) . . ?
C351 P1 Os1 105.5(3) . . ?
C351 P1 C341 102.7(4) . . ?
C351 P1 C361 106.3(4) . . ?
C361 P1 Os1 118.5(3) . . ?
C361 P1 C341 99.5(4) . . ?
C342 C341 P1 122.3(8) . . ?
C342 C341 C346 118.2(9) . . ?
C346 C341 P1 119.4(8) . . ?
C11 C3 C2 114.0(6) . . ?
C11 C3 C7 114.1(6) . . ?
C4 C3 C11 118.3(6) . . ?
C4 C3 C2 107.3(6) . . ?
C4 C3 C7 104.9(6) . . ?
C7 C3 C2 95.4(5) . . ?
C16 C11 C3 120.8(7) . . ?
C12 C11 C3 120.7(7) . . ?
C12 C11 C16 118.3(7) . . ?
C336 C331 P2 119.7(6) . . ?
C336 C331 C332 120.3(7) . . ?
C332 C331 P2 119.9(7) . . ?
C352 C351 P1 122.7(7) . . ?
C352 C351 C356 116.5(9) . . ?
C356 C351 P1 120.0(7) . . ?
C16 C15 C14 119.9(8) . . ?
C362 C361 P1 119.8(7) . . ?
C362 C361 C366 118.1(8) . . ?
C366 C361 P1 121.9(6) . . ?
C352 C353 C354 120.3(11) . . ?
C26 C21 C7 121.2(7) . . ?
C22 C21 C26 116.7(7) . . ?
C22 C21 C7 122.1(7) . . ?
C335 C336 C331 118.6(8) . . ?
C25 C26 C21 120.7(7) . . ?
C322 C321 P2 123.5(7) . . ?
C322 C321 C326 119.1(8) . . ?
C326 C321 P2 117.4(7) . . ?
C22 C23 C24 120.1(8) . . ?
C333 C332 C331 119.4(9) . . ?
C312 C311 P2 122.5(7) . . ?
C316 C311 P2 117.3(9) . . ?
C316 C311 C312 120.0(9) . . ?
C15 C16 C11 121.3(8) . . ?
C321 C322 C323 120.8(9) . . ?
C11 C12 C13 121.3(8) . . ?
C12 C13 C14 119.8(8) . . ?
C363 C362 C361 121.2(9) . . ?
C325 C326 C321 120.4(9) . . ?
C365 C364 C363 119.8(8) . . ?
C323 C324 C325 121.2(10) . . ?
C15 C14 C13 119.4(8) . . ?
C23 C22 C21 123.2(8) . . ?
C365 C366 C361 120.6(9) . . ?
C23 C24 C25 118.6(8) . . ?
C23 C24 O1 126.0(8) . . ?
O1 C24 C25 115.4(8) . . ?
C366 C365 C364 120.6(9) . . ?
C26 C25 C24 120.5(8) . . ?
C336 C335 C334 121.5(8) . . ?
C362 C363 C364 119.6(9) . . ?
C324 C323 C322 119.5(10) . . ?
C334 C333 C332 120.7(8) . . ?
C324 C325 C326 119.0(9) . . ?
C311 C312 C313 120.2(11) . . ?
C333 C334 C335 119.4(8) . . ?
C315 C314 C313 116.5(11) . . ?
C314 C313 C312 122.1(12) . . ?
C353 C352 C351 121.9(9) . . ?
C355 C356 C351 121.7(10) . . ?
C341 C342 C343 121.4(11) . . ?
C355 C354 C353 119.2(11) . . ?
C356 C355 C354 120.2(10) . . ?
C345 C346 C341 121.5(11) . . ?
C346 C345 C344 119.5(11) . . ?
C344 C343 C342 119.3(11) . . ?
C343 C344 C345 120.2(10) . . ?
C24 O1 C27 113.4(8) . . ?
C4 N1 Os1 118.5(6) . . ?
C5 C4 C3 128.6(7) . . ?
N1 C4 C3 108.2(7) . . ?
N1 C4 C5 123.2(8) . . ?
F2 B1 F1 109.3(9) . . ?
F3 B1 F2 106.5(9) . . ?
F3 B1 F1 110.3(9) . . ?
F4 B1 F2 110.4(9) . . ?
F4 B1 F3 109.0(9) . . ?
F4 B1 F1 111.2(9) . . ?
C314 C315 C316 123.7(14) . . ?
C311 C316 C315 117.1(15) . . ?
Cl32 C32 Cl3 116.9(9) . . ?
Cl4 C31 Cl31 120.0(11) . . ?
P2 C2 Os1 127.2(4) . . ?
C3 C2 Os1 88.6(4) . . ?
C3 C2 P2 126.5(5) . . ?
C1 C2 Os1 69.5(4) . . ?
C1 C2 P2 118.8(6) . . ?
C1 C2 C3 110.1(7) . . ?
C2 C1 Os1 74.1(4) . . ?
C2 C1 C6 109.1(7) . . ?
C6 C1 Os1 70.5(4) . . ?
C1 C6 Os1 71.7(5) . . ?
C7 C6 Os1 76.2(4) . . ?
C7 C6 C1 109.1(6) . . ?
C3 C7 Os1 87.5(4) . . ?
C21 C7 Os1 126.5(5) . . ?
C21 C7 C3 123.0(6) . . ?
C6 C7 Os1 67.2(4) . . ?
C6 C7 C3 110.1(6) . . ?
C6 C7 C21 124.3(7) . . ?

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

data_1
_database_code_depnum_ccdc_archive 'CCDC 1038534'
_audit_update_record             
;
2014-12-10 deposited with the CCDC.
2015-03-26 downloaded from the CCDC.
;
_audit_creation_date             2014-11-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.11.25 svn.r3098 for OlexSys, GUI svn.r4951)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         
'C56 H48 Cl2 N O Os P2, B F4, 2(H2 O), 0.25(C H Cl3)'
_chemical_formula_sum            'C56.25 H52.25 B Cl2.75 F4 N O3 Os P2'
_chemical_formula_weight         1226.68
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_length_a                   11.9299(3)
_cell_length_b                   14.1946(3)
_cell_length_c                   33.0235(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.5760(10)
_cell_angle_gamma                90.00
_cell_volume                     5529.7(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      ?
_cell_measurement_theta_min      ?
_exptl_absorpt_coefficient_mu    2.553
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            'dark violet'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2458
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0800
_diffrn_reflns_av_unetI/netI     0.0528
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            62557
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.08
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                8011
_reflns_number_total             9691
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         2.144
_refine_diff_density_min         -1.296
_refine_diff_density_rms         0.156
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         9691
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0694
_refine_ls_R_factor_gt           0.0566
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0855P)²+36.6174P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1635
_refine_ls_wR_factor_ref         0.1720
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C1S) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: Cl1C(0.25) Cl1B(0.25) Cl1A(0.25) C1S(0.25) H1S(0.25)
4.a Riding coordinates:
 O1A(H1AA,H1AB), O1B(H1BA,H1BB)
4.b Ternary CH refined with riding coordinates:
 C6(H6), C1(H1A), C1S(H1S)
4.c Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B)
4.d Me refined with riding coordinates:
 C5(H5A,H5B,H5C)
4.e Aromatic/amide H refined with riding coordinates:
 N1(H1), C312(H312), C343(H343), C316(H316), C315(H315), C336(H336),
 C322(H322), C352(H352), C342(H342), C12(H12), C22(H22), C326(H326), C325(H325),
  C314(H314), C346(H346), C323(H323), C313(H313), C345(H345), C23(H23),
 C26(H26), C306(H306), C302(H302), C24(H24), C14(H14), C324(H324), C15(H15),
 C25(H25), C344(H344), C305(H305), C335(H335), C304(H304), C303(H303),
 C332(H332), C334(H334), C333(H333), C353(H353), C356(H356), C354(H354),
 C355(H355), C16(H16), C13(H13)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Os1 Os 0.78208(3) 0.66286(2) 0.656075(9) 0.03522(13) Uani 1 d . . . .
Cl1 Cl 0.94364(19) 0.55828(14) 0.67104(7) 0.0463(5) Uani 1 d . . . .
P1 P 0.77615(19) 0.64520(15) 0.58670(7) 0.0393(5) Uani 1 d . . . .
Cl2 Cl 0.6706(2) 0.52102(15) 0.66197(7) 0.0502(5) Uani 1 d . . . .
P2 P 0.83653(19) 0.99523(14) 0.66960(7) 0.0391(5) Uani 1 d . . . .
C2 C 0.7583(7) 0.8838(5) 0.6699(2) 0.0325(16) Uani 1 d . . . .
C3 C 0.6534(7) 0.8742(6) 0.6795(3) 0.0394(18) Uani 1 d . . . .
C301 C 0.7976(8) 1.0879(6) 0.7026(3) 0.049(2) Uani 1 d . . . .
N1 N 0.6251(6) 0.7172(5) 0.6522(2) 0.0434(16) Uani 1 d . . . .
H1 H 0.5733 0.6801 0.6388 0.052 Uiso 1 calc . . R .
C312 C 1.0473(7) 0.9431(6) 0.6515(3) 0.0425(19) Uani 1 d . . . .
H312 H 1.0099 0.9289 0.6247 0.051 Uiso 1 calc . . R .
C331 C 0.8128(7) 0.5328(6) 0.5647(3) 0.044(2) Uani 1 d . . . .
C311 C 0.9856(7) 0.9777(5) 0.6815(2) 0.0381(18) Uani 1 d . . . .
C343 C 1.0653(10) 0.7808(8) 0.5662(3) 0.062(3) Uani 1 d . . . .
H343 H 1.1438 0.7748 0.5763 0.075 Uiso 1 calc . . R .
C5 C 0.4541(8) 0.8024(8) 0.6610(4) 0.064(3) Uani 1 d . . . .
H5A H 0.4182 0.7432 0.6507 0.096 Uiso 1 calc . . R .
H5B H 0.4282 0.8535 0.6420 0.096 Uiso 1 calc . . R .
H5C H 0.4335 0.8165 0.6880 0.096 Uiso 1 calc . . R .
C316 C 1.0424(7) 0.9977(6) 0.7207(3) 0.0432(19) Uani 1 d . . . .
H316 H 1.0018 1.0218 0.7411 0.052 Uiso 1 calc . . R .
C351 C 0.6340(8) 0.6682(7) 0.5604(3) 0.050(2) Uani 1 d . . . .
C315 C 1.1599(8) 0.9820(6) 0.7298(3) 0.051(2) Uani 1 d . . . .
H315 H 1.1982 0.9943 0.7566 0.061 Uiso 1 calc . . R .
C11 C 0.8684(7) 0.7462(5) 0.7847(2) 0.0398(18) Uani 1 d . . . .
C336 C 0.8054(9) 0.4484(6) 0.5839(3) 0.055(2) Uani 1 d . . . .
H336 H 0.7834 0.4469 0.6104 0.066 Uiso 1 calc . . R .
C341 C 0.8692(8) 0.7259(6) 0.5644(3) 0.046(2) Uani 1 d . . . .
C322 C 0.8875(9) 1.0861(6) 0.6001(3) 0.051(2) Uani 1 d . . . .
H322 H 0.9566 1.1035 0.6166 0.061 Uiso 1 calc . . R .
C21 C 0.5926(7) 0.9452(6) 0.7034(3) 0.046(2) Uani 1 d . . . .
C352 C 0.5887(8) 0.7587(7) 0.5600(3) 0.050(2) Uani 1 d . . . .
H352 H 0.6352 0.8095 0.5712 0.060 Uiso 1 calc . . R .
C342 C 0.9856(9) 0.7164(7) 0.5792(3) 0.058(3) Uani 1 d . . . .
H342 H 1.0112 0.6673 0.5978 0.070 Uiso 1 calc . . R .
C12 C 0.7981(9) 0.6973(6) 0.8061(3) 0.050(2) Uani 1 d . . . .
H12 H 0.7419 0.6571 0.7919 0.060 Uiso 1 calc . . R .
C321 C 0.8073(8) 1.0320(6) 0.6171(3) 0.046(2) Uani 1 d . . . .
C22 C 0.5483(8) 1.0277(6) 0.6867(3) 0.051(2) Uani 1 d . . . .
H22 H 0.5561 1.0444 0.6594 0.061 Uiso 1 calc . . R .
C326 C 0.7029(8) 1.0115(6) 0.5926(3) 0.049(2) Uani 1 d . . . .
H326 H 0.6463 0.9771 0.6036 0.059 Uiso 1 calc . . R .
C325 C 0.6833(9) 1.0417(7) 0.5523(3) 0.060(3) Uani 1 d . . . .
H325 H 0.6130 1.0281 0.5358 0.072 Uiso 1 calc . . R .
C314 C 1.2195(8) 0.9491(6) 0.7002(3) 0.051(2) Uani 1 d . . . .
H314 H 1.2991 0.9396 0.7065 0.061 Uiso 1 calc . . R .
C346 C 0.8355(10) 0.7938(7) 0.5354(3) 0.058(2) Uani 1 d . . . .
H346 H 0.7580 0.7980 0.5236 0.070 Uiso 1 calc . . R .
C323 C 0.8663(10) 1.1140(7) 0.5596(3) 0.061(3) Uani 1 d . . . .
H323 H 0.9220 1.1488 0.5482 0.073 Uiso 1 calc . . R .
C313 C 1.1636(8) 0.9300(6) 0.6615(3) 0.050(2) Uani 1 d . . . .
H313 H 1.2055 0.9073 0.6412 0.060 Uiso 1 calc . . R .
C345 C 0.9151(13) 0.8570(8) 0.5230(4) 0.075(4) Uani 1 d . . . .
H345 H 0.8906 0.9044 0.5034 0.089 Uiso 1 calc . . R .
C23 C 0.4913(8) 1.0872(7) 0.7106(4) 0.062(3) Uani 1 d . . . .
H23 H 0.4628 1.1459 0.6997 0.074 Uiso 1 calc . . R .
C26 C 0.5769(8) 0.9186(7) 0.7422(3) 0.054(2) Uani 1 d . . . .
H26 H 0.6055 0.8599 0.7531 0.065 Uiso 1 calc . . R .
C306 C 0.7937(8) 1.0705(8) 0.7432(3) 0.060(3) Uani 1 d . . . .
H306 H 0.8114 1.0098 0.7545 0.072 Uiso 1 calc . . R .
C302 C 0.7740(9) 1.1765(7) 0.6865(4) 0.072(3) Uani 1 d . . . .
H302 H 0.7779 1.1890 0.6585 0.086 Uiso 1 calc . . R .
C24 C 0.4763(9) 1.0619(8) 0.7491(4) 0.069(3) Uani 1 d . . . .
H24 H 0.4363 1.1024 0.7649 0.083 Uiso 1 calc . . R .
C14 C 0.8878(11) 0.7659(8) 0.8681(3) 0.070(3) Uani 1 d . . . .
H14 H 0.8948 0.7722 0.8970 0.084 Uiso 1 calc . . R .
C324 C 0.7657(10) 1.0919(7) 0.5358(3) 0.065(3) Uani 1 d . . . .
H324 H 0.7522 1.1109 0.5079 0.078 Uiso 1 calc . . R .
C15 C 0.9582(11) 0.8172(8) 0.8468(3) 0.069(3) Uani 1 d . . . .
H15 H 1.0125 0.8592 0.8610 0.083 Uiso 1 calc . . R .
C25 C 0.5192(10) 0.9776(9) 0.7654(3) 0.069(3) Uani 1 d . . . .
H25 H 0.5092 0.9600 0.7924 0.083 Uiso 1 calc . . R .
C344 C 1.0283(11) 0.8506(8) 0.5394(4) 0.072(3) Uani 1 d . . . .
H344 H 1.0807 0.8952 0.5318 0.086 Uiso 1 calc . . R .
C305 C 0.7632(12) 1.1438(11) 0.7676(4) 0.090(4) Uani 1 d . . . .
H305 H 0.7606 1.1329 0.7958 0.109 Uiso 1 calc . . R .
C335 C 0.8294(11) 0.3653(7) 0.5655(4) 0.069(3) Uani 1 d . . . .
H335 H 0.8216 0.3075 0.5792 0.083 Uiso 1 calc . . R .
C304 C 0.7378(12) 1.2289(11) 0.7516(6) 0.104(6) Uani 1 d . . . .
H304 H 0.7148 1.2774 0.7684 0.125 Uiso 1 calc . . R .
O1 O 0.7817(5) 0.6840(4) 0.72173(16) 0.0368(12) Uani 1 d . . . .
C7 C 0.9523(7) 0.7642(6) 0.7166(2) 0.0403(18) Uani 1 d . . . .
H7A H 0.9721 0.8299 0.7248 0.048 Uiso 1 calc . . R .
H7B H 1.0209 0.7250 0.7239 0.048 Uiso 1 calc . . R .
C4 C 0.5824(7) 0.7928(6) 0.6646(2) 0.0399(18) Uani 1 d . . . .
C303 C 0.7444(11) 1.2470(8) 0.7119(6) 0.094(5) Uani 1 d . . . .
H303 H 0.7286 1.3086 0.7013 0.113 Uiso 1 calc . . R .
C6 C 0.9155(7) 0.7603(5) 0.6710(2) 0.0352(17) Uani 1 d . . . .
H6 H 0.9795 0.7517 0.6549 0.042 Uiso 1 calc . . R .
C1 C 0.8221(7) 0.8102(6) 0.6497(2) 0.0376(18) Uani 1 d . . . .
H1A H 0.8326 0.8275 0.6211 0.045 Uiso 1 calc . . R .
C8 C 0.8600(7) 0.7295(5) 0.7398(3) 0.0373(18) Uani 1 d . . . .
C332 C 0.8455(10) 0.5334(8) 0.5260(3) 0.070(3) Uani 1 d . . . .
H332 H 0.8498 0.5912 0.5119 0.084 Uiso 1 calc . . R .
C334 C 0.8641(10) 0.3640(8) 0.5279(4) 0.069(3) Uani 1 d . . . .
H334 H 0.8823 0.3064 0.5157 0.082 Uiso 1 calc . . R .
C333 C 0.8721(11) 0.4487(9) 0.5081(4) 0.081(4) Uani 1 d . . . .
H333 H 0.8959 0.4495 0.4819 0.097 Uiso 1 calc . . R .
C353 C 0.4770(11) 0.7756(9) 0.5437(3) 0.078(4) Uani 1 d . . . .
H353 H 0.4487 0.8382 0.5429 0.093 Uiso 1 calc . . R .
C356 C 0.5647(11) 0.5939(8) 0.5458(4) 0.088(4) Uani 1 d . . . .
H356 H 0.5926 0.5312 0.5470 0.106 Uiso 1 calc . . R .
C354 C 0.4081(13) 0.7052(12) 0.5292(6) 0.123(7) Uani 1 d . . . .
H354 H 0.3307 0.7171 0.5189 0.148 Uiso 1 calc . . R .
C355 C 0.4520(12) 0.6138(12) 0.5293(6) 0.126(7) Uani 1 d . . . .
H355 H 0.4042 0.5640 0.5179 0.151 Uiso 1 calc . . R .
C16 C 0.9493(9) 0.8071(7) 0.8053(3) 0.056(2) Uani 1 d . . . .
H16 H 0.9981 0.8416 0.7905 0.067 Uiso 1 calc . . R .
C13 C 0.8073(10) 0.7054(7) 0.8479(3) 0.062(3) Uani 1 d . . . .
H13 H 0.7592 0.6702 0.8627 0.075 Uiso 1 calc . . R .
F4 F 0.2839(7) -0.0814(6) 0.5713(3) 0.100(2) Uani 1 d . . . .
F3 F 0.3835(11) 0.0270(8) 0.5427(3) 0.169(5) Uani 1 d . . . .
F2 F 0.3662(11) 0.0388(9) 0.6109(3) 0.173(5) Uani 1 d . . . .
B1 B 0.3314(17) 0.0059(10) 0.5737(4) 0.085(5) Uani 1 d . . . .
F1 F 0.2289(15) 0.0625(11) 0.5637(6) 0.237(8) Uani 1 d . . . .
O1A O 0.6541(10) 0.6831(8) 0.4438(2) 0.122(4) Uani 1 d . . . .
H1AA H 0.7197 0.6593 0.4505 0.147 Uiso 1 d . . R .
H1AB H 0.6147 0.6450 0.4277 0.147 Uiso 1 d . . R .
O1B O 0.4531(7) 0.7196(8) 0.3857(3) 0.121(4) Uani 1 d . . . .
H1BA H 0.5015 0.7173 0.3693 0.145 Uiso 1 d . . R .
H1BB H 0.3913 0.7403 0.3726 0.145 Uiso 1 d . . R .
Cl1C Cl 0.7317(14) 0.3993(9) 0.3847(5) 0.102(5) Uani 0.25 d . . . .
Cl1B Cl 0.7182(12) 0.5500(12) 0.3396(5) 0.109(5) Uani 0.25 d . . . .
Cl1A Cl 0.8633(17) 0.5257(12) 0.4166(6) 0.119(6) Uani 0.25 d . . . .
C1S C 0.799(2) 0.496(2) 0.3776(8) 0.027(6) Uani 0.25 d . . . U
H1S H 0.8613 0.4718 0.3632 0.033 Uiso 0.25 calc . . R .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Os1 Cl1 2.425(2) . ?
Os1 P1 2.295(2) . ?
Os1 Cl2 2.436(2) . ?
Os1 N1 2.012(7) . ?
Os1 O1 2.190(5) . ?
Os1 C6 2.111(8) . ?
Os1 C1 2.163(8) . ?
P1 C331 1.834(8) . ?
P1 C351 1.816(10) . ?
P1 C341 1.825(9) . ?
P2 C2 1.838(8) . ?
P2 C301 1.812(8) . ?
P2 C311 1.780(9) . ?
P2 C321 1.793(9) . ?
C2 C3 1.342(11) . ?
C2 C1 1.506(11) . ?
C3 C21 1.529(11) . ?
C3 C4 1.473(12) . ?
C301 C306 1.372(14) . ?
C301 C302 1.377(14) . ?
N1 C4 1.282(11) . ?
C312 C311 1.409(11) . ?
C312 C313 1.390(13) . ?
C331 C336 1.366(13) . ?
C331 C332 1.388(13) . ?
C311 C316 1.397(12) . ?
C343 C342 1.430(14) . ?
C343 C344 1.358(17) . ?
C5 C4 1.523(12) . ?
C316 C315 1.407(13) . ?
C351 C352 1.394(13) . ?
C351 C356 1.381(14) . ?
C315 C314 1.373(13) . ?
C11 C12 1.366(12) . ?
C11 C8 1.489(11) . ?
C11 C16 1.395(13) . ?
C336 C335 1.376(13) . ?
C341 C342 1.408(14) . ?
C341 C346 1.376(13) . ?
C322 C321 1.407(12) . ?
C322 C323 1.382(13) . ?
C21 C22 1.367(13) . ?
C21 C26 1.375(13) . ?
C352 C353 1.381(14) . ?
C12 C13 1.373(13) . ?
C321 C326 1.411(13) . ?
C22 C23 1.399(13) . ?
C326 C325 1.384(13) . ?
C325 C324 1.388(15) . ?
C314 C313 1.378(14) . ?
C346 C345 1.411(15) . ?
C323 C324 1.370(15) . ?
C345 C344 1.380(18) . ?
C23 C24 1.360(15) . ?
C26 C25 1.386(13) . ?
C306 C305 1.396(15) . ?
C302 C303 1.384(16) . ?
C24 C25 1.379(16) . ?
C14 C15 1.379(16) . ?
C14 C13 1.383(15) . ?
C15 C16 1.368(14) . ?
C305 C304 1.34(2) . ?
C335 C334 1.367(16) . ?
C304 C303 1.35(2) . ?
O1 C8 1.216(9) . ?
C7 C6 1.505(11) . ?
C7 C8 1.515(11) . ?
C6 C1 1.416(11) . ?
C332 C333 1.397(15) . ?
C334 C333 1.378(17) . ?
C353 C354 1.337(19) . ?
C356 C355 1.403(17) . ?
C354 C355 1.40(2) . ?
F4 B1 1.360(16) . ?
F3 B1 1.308(17) . ?
F2 B1 1.321(17) . ?
B1 F1 1.46(2) . ?
Cl1C C1S 1.63(3) . ?
Cl1B C1S 1.65(3) . ?
Cl1A C1S 1.46(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
Cl1 Os1 Cl2 84.51(8) . . ?
P1 Os1 Cl1 92.40(8) . . ?
P1 Os1 Cl2 93.07(8) . . ?
N1 Os1 Cl1 162.1(2) . . ?
N1 Os1 P1 95.1(2) . . ?
N1 Os1 Cl2 78.9(2) . . ?
N1 Os1 O1 82.6(2) . . ?
N1 Os1 C6 115.2(3) . . ?
N1 Os1 C1 80.8(3) . . ?
O1 Os1 Cl1 90.07(15) . . ?
O1 Os1 P1 177.53(15) . . ?
O1 Os1 Cl2 87.28(15) . . ?
C6 Os1 Cl1 78.7(2) . . ?
C6 Os1 P1 102.4(2) . . ?
C6 Os1 Cl2 157.6(2) . . ?
C6 Os1 O1 78.0(2) . . ?
C6 Os1 C1 38.7(3) . . ?
C1 Os1 Cl1 115.6(2) . . ?
C1 Os1 P1 89.0(2) . . ?
C1 Os1 Cl2 159.7(2) . . ?
C1 Os1 O1 89.8(2) . . ?
C331 P1 Os1 121.2(3) . . ?
C351 P1 Os1 110.3(3) . . ?
C351 P1 C331 103.1(4) . . ?
C351 P1 C341 105.9(5) . . ?
C341 P1 Os1 113.8(3) . . ?
C341 P1 C331 101.0(4) . . ?
C301 P2 C2 116.5(4) . . ?
C311 P2 C2 111.7(4) . . ?
C311 P2 C301 107.8(4) . . ?
C311 P2 C321 107.4(4) . . ?
C321 P2 C2 103.3(4) . . ?
C321 P2 C301 109.8(4) . . ?
C3 C2 P2 125.5(6) . . ?
C3 C2 C1 125.8(7) . . ?
C1 C2 P2 107.7(6) . . ?
C2 C3 C21 125.9(7) . . ?
C2 C3 C4 120.7(7) . . ?
C4 C3 C21 113.3(7) . . ?
C306 C301 P2 120.4(8) . . ?
C306 C301 C302 120.4(9) . . ?
C302 C301 P2 119.2(8) . . ?
C4 N1 Os1 135.4(6) . . ?
C313 C312 C311 119.1(8) . . ?
C336 C331 P1 122.9(7) . . ?
C336 C331 C332 118.6(8) . . ?
C332 C331 P1 118.4(7) . . ?
C312 C311 P2 120.2(7) . . ?
C316 C311 P2 120.4(6) . . ?
C316 C311 C312 119.4(8) . . ?
C344 C343 C342 119.7(11) . . ?
C311 C316 C315 119.7(8) . . ?
C352 C351 P1 120.2(7) . . ?
C356 C351 P1 119.9(8) . . ?
C356 C351 C352 119.3(10) . . ?
C314 C315 C316 120.5(9) . . ?
C12 C11 C8 118.7(8) . . ?
C12 C11 C16 119.6(8) . . ?
C16 C11 C8 121.6(8) . . ?
C331 C336 C335 120.9(9) . . ?
C342 C341 P1 115.3(7) . . ?
C346 C341 P1 126.0(8) . . ?
C346 C341 C342 118.7(9) . . ?
C323 C322 C321 120.4(10) . . ?
C22 C21 C3 122.8(8) . . ?
C22 C21 C26 120.9(8) . . ?
C26 C21 C3 116.2(8) . . ?
C353 C352 C351 120.9(10) . . ?
C341 C342 C343 120.0(10) . . ?
C11 C12 C13 121.1(9) . . ?
C322 C321 P2 119.9(7) . . ?
C322 C321 C326 118.5(8) . . ?
C326 C321 P2 121.5(7) . . ?
C21 C22 C23 118.7(9) . . ?
C325 C326 C321 119.8(9) . . ?
C326 C325 C324 120.5(10) . . ?
C315 C314 C313 119.8(9) . . ?
C341 C346 C345 120.5(11) . . ?
C324 C323 C322 120.5(10) . . ?
C314 C313 C312 121.5(8) . . ?
C344 C345 C346 120.4(11) . . ?
C24 C23 C22 120.8(10) . . ?
C21 C26 C25 119.8(10) . . ?
C301 C306 C305 118.6(12) . . ?
C301 C302 C303 118.9(13) . . ?
C23 C24 C25 120.1(9) . . ?
C15 C14 C13 121.0(10) . . ?
C323 C324 C325 120.3(10) . . ?
C16 C15 C14 119.5(10) . . ?
C24 C25 C26 119.7(11) . . ?
C343 C344 C345 120.5(10) . . ?
C304 C305 C306 120.7(14) . . ?
C334 C335 C336 121.7(11) . . ?
C305 C304 C303 120.8(12) . . ?
C8 O1 Os1 116.4(5) . . ?
C6 C7 C8 111.7(7) . . ?
C3 C4 C5 118.6(8) . . ?
N1 C4 C3 121.8(7) . . ?
N1 C4 C5 119.5(8) . . ?
C304 C303 C302 120.5(13) . . ?
C7 C6 Os1 110.7(5) . . ?
C1 C6 Os1 72.6(5) . . ?
C1 C6 C7 124.7(7) . . ?
C2 C1 Os1 119.6(5) . . ?
C6 C1 Os1 68.7(4) . . ?
C6 C1 C2 122.6(7) . . ?
C11 C8 C7 120.4(7) . . ?
O1 C8 C11 120.4(7) . . ?
O1 C8 C7 119.2(7) . . ?
C331 C332 C333 119.8(11) . . ?
C335 C334 C333 118.1(10) . . ?
C334 C333 C332 120.9(11) . . ?
C354 C353 C352 121.1(12) . . ?
C351 C356 C355 118.1(12) . . ?
C353 C354 C355 118.8(12) . . ?
C354 C355 C356 121.7(13) . . ?
C15 C16 C11 120.0(9) . . ?
C12 C13 C14 118.7(10) . . ?
F4 B1 F1 99.3(15) . . ?
F3 B1 F4 114.0(11) . . ?
F3 B1 F2 121.7(16) . . ?
F3 B1 F1 100.1(14) . . ?
F2 B1 F4 116.5(13) . . ?
F2 B1 F1 98.8(14) . . ?
Cl1C C1S Cl1B 104.7(17) . . ?
Cl1A C1S Cl1C 108.8(18) . . ?
Cl1A C1S Cl1B 135(2) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Chloroform, n-hexane'
####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1038535'
_audit_update_record             
;
2015-02-11 deposited with the CCDC.
2015-03-26 downloaded from the CCDC.
;
_audit_creation_date             2014-11-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C48 H40 Cl N3 O Os P, 2(C H2 Cl2), B F4'
_chemical_formula_sum            'C50 H43 B Cl5 F4 N3 O Os P'
_chemical_formula_weight         1187.10
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_length_a                   12.0746(3)
_cell_length_b                   18.8448(3)
_cell_length_c                   20.9677(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.0230(10)
_cell_angle_gamma                90.00
_cell_volume                     4771.06(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8087
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      0
_exptl_absorpt_coefficient_mu    3.044
_exptl_absorpt_correction_T_max  0.401
_exptl_absorpt_correction_T_min  0.175
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2356
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.3
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0945
_diffrn_reflns_av_unetI/netI     0.0642
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            70908
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.11
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                8348
_reflns_number_total             10901
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         2.133
_refine_diff_density_min         -2.640
_refine_diff_density_rms         0.219
_refine_ls_extinction_coef       0.0029(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.170
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         10901
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0526
_refine_ls_restrained_S_all      1.170
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1054P)²+3.6588P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1396
_refine_ls_wR_factor_ref         0.1954
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Others
 Fixed Uiso: H1(0.034) H23(0.094) H11(0.042) H22(0.058) H12(0.045) H15(0.046)
 H14(0.052) H5A(0.058) H5B(0.058) H5C(0.058) H303(0.049) H304(0.059)
 H306(0.044) H305(0.054) H26(0.061) H325(0.074) H326(0.056) H25(0.092)
 H322(0.057) H324(0.084) H24(0.109) H323(0.074) H313(0.054) H1A(0.029)
 H34(0.042) H31(0.047) H6(0.04) H37(0.042) H312(0.042) H314(0.059) H39(0.047)
 H315(0.049) H33(0.056) H40(0.048) H316(0.043) H38(0.049) H1SA(0.075)
 H1SB(0.075) H32(0.055) H2SA(0.097) H2SB(0.097) H16A(0.1) H16B(0.1) H16C(0.1)
 Fixed X: H1(0.7284) H23(1.1259) H11(0.9861) H22(0.9867) H12(1.1092)
 H15(1.1521) H14(1.2744) H5A(0.9135) H5B(0.9977) H5C(0.8858) H303(0.4789)
 H304(0.4112) H306(0.6628) H305(0.4964) H26(1.073) H325(0.9319) H326(0.8359)
 H25(1.2153) H322(0.952) H324(1.0421) H24(1.2394) H323(1.0502) H313(0.5847)
 H1A(0.7742) H34(0.6335) H31(0.7832) H6(0.926) H37(0.5301) H312(0.6185)
 H314(0.7186) H39(0.4121) H315(0.8829) H33(0.743) H40(0.512) H316(0.9139)
 H38(0.4192) H1SA(0.5365) H1SB(0.5405) H32(0.8112) H2SA(1.6609) H2SB(1.7129)
 H16A(1.1976) H16B(1.3262) H16C(1.2711)
 Fixed Y: H1(3.6276) H23(3.5266) H11(3.5888) H22(3.566) H12(3.6723)
 H15(3.5765) H14(3.6612) H5A(3.6644) H5B(3.6557) H5C(3.696) H303(3.5414)
 H304(3.5106) H306(3.3755) H305(3.4242) H26(3.4202) H325(3.4382) H326(3.4667)
 H25(3.3818) H322(3.2866) H324(3.3386) H24(3.4334) H323(3.2629) H313(3.1855)
 H1A(3.4081) H34(3.4523) H31(3.6165) H6(3.4714) H37(3.3723) H312(3.2945)
 H314(3.1332) H39(3.2955) H315(3.1918) H33(3.5435) H40(3.3804) H316(3.303)
 H38(3.2916) H1SA(3.8052) H1SB(3.7222) H32(3.6277) H2SA(3.5698) H2SB(3.6346)
 H16A(3.7839) H16B(3.7943) H16C(3.7253)
 Fixed Z: H1(-0.2037) H23(-0.3932) H11(-0.0317) H22(-0.3266) H12(0.0063) H15(-
 0.1963) H14(-0.1599) H5A(-0.2833) H5B(-0.2269) H5C(-0.216) H303(-0.2558) H304(-
 0.356) H306(-0.3809) H305(-0.4167) H26(-0.1975) H325(-0.4769) H326(-0.3849)
 H25(-0.2639) H322(-0.3034) H324(-0.4808) H24(-0.3622) H323(-0.3958) H313(-
 0.2238) H1A(-0.1202) H34(0.0677) H31(-0.0684) H6(-0.0601) H37(0.0223) H312(-
 0.2686) H314(-0.1599) H39(-0.142) H315(-0.1391) H33(0.1081) H40(-0.1953) H316(-
 0.1832) H38(-0.0318) H1SA(-0.1399) H1SB(-0.1357) H32(0.0398) H2SA(0.6081)
 H2SB(0.572) H16A(0.0048) H16B(0.0096) H16C(0.0369)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
Os1 Os 0.680815(19) 3.503767(11) -0.166274(11) 0.02855(14) Uani 1 d . . .
C21 C 1.0172(5) 3.4974(3) -0.2561(4) 0.0319(15) Uani 1 d . . .
N1 N 0.7643(4) 3.5883(2) -0.2010(2) 0.0287(10) Uani 1 d . . .
H1 H 0.7284 3.6276 -0.2037 0.034 Uiso 1 calc . . R
C7 C 0.9660(5) 3.5220(3) -0.1407(3) 0.0313(12) Uani 1 d . . .
C23 C 1.1154(10) 3.5052(5) -0.3537(6) 0.078(4) Uani 1 d . . .
H23 H 1.1259 3.5266 -0.3932 0.094 Uiso 1 calc . . R
C11 C 1.0436(5) 3.6035(3) -0.0580(3) 0.0349(13) Uani 1 d . . .
H11 H 0.9861 3.5888 -0.0317 0.042 Uiso 1 calc . . R
C10 C 1.0509(5) 3.5739(3) -0.1186(3) 0.0294(12) Uani 1 d . . .
C3 C 0.9252(5) 3.5180(3) -0.2100(3) 0.0270(12) Uani 1 d . . .
C22 C 1.0323(6) 3.5288(4) -0.3140(3) 0.0485(17) Uani 1 d . . .
H22 H 0.9867 3.5660 -0.3266 0.058 Uiso 1 calc . . R
O1 O 1.2815(4) 3.7259(3) -0.0572(2) 0.0535(13) Uani 1 d . . .
C13 C 1.2033(5) 3.6762(3) -0.0737(3) 0.0361(14) Uani 1 d . . .
C12 C 1.1174(5) 3.6540(3) -0.0346(3) 0.0373(14) Uani 1 d . . .
H12 H 1.1092 3.6723 0.0063 0.045 Uiso 1 calc . . R
C15 C 1.1418(5) 3.5962(3) -0.1560(3) 0.0382(14) Uani 1 d . . .
H15 H 1.1521 3.5765 -0.1963 0.046 Uiso 1 calc . . R
C14 C 1.2160(6) 3.6468(4) -0.1341(3) 0.0432(16) Uani 1 d . . .
H14 H 1.2744 3.6612 -0.1599 0.052 Uiso 1 calc . . R
Cl1 Cl 0.52714(13) 3.58461(9) -0.15027(8) 0.0414(4) Uani 1 d . . .
C4 C 0.8662(5) 3.5892(3) -0.2196(3) 0.0301(12) Uani 1 d . . .
C5 C 0.9207(5) 3.6574(3) -0.2381(3) 0.0386(14) Uani 1 d . . .
H5A H 0.9135 3.6644 -0.2833 0.058 Uiso 1 calc . . GR
H5B H 0.9977 3.6557 -0.2269 0.058 Uiso 1 calc . . GR
H5C H 0.8858 3.6960 -0.2160 0.058 Uiso 1 calc . . GR
C303 C 0.5176(6) 3.5090(3) -0.2807(4) 0.0406(17) Uani 1 d . . .
H303 H 0.4789 3.5414 -0.2558 0.049 Uiso 1 calc . . R
C304 C 0.4754(7) 3.4891(4) -0.3410(4) 0.049(2) Uani 1 d . . .
H304 H 0.4112 3.5106 -0.3560 0.059 Uiso 1 calc . . R
P1 P 0.79346(12) 3.39638(8) -0.26645(7) 0.0289(3) Uani 1 d . . .
C306 C 0.6258(5) 3.4092(3) -0.3566(3) 0.0364(14) Uani 1 d . . .
H306 H 0.6628 3.3755 -0.3809 0.044 Uiso 1 calc . . R
C321 C 0.8830(5) 3.3787(3) -0.3339(3) 0.0373(14) Uani 1 d . . .
C301 C 0.6687(5) 3.4314(3) -0.2979(3) 0.0334(13) Uani 1 d . . .
C305 C 0.5271(6) 3.4385(4) -0.3780(3) 0.0453(16) Uani 1 d . . .
H305 H 0.4964 3.4242 -0.4167 0.054 Uiso 1 calc . . R
C302 C 0.6169(5) 3.4803(3) -0.2580(3) 0.0337(13) Uani 1 d . . .
C26 C 1.0843(6) 3.4419(4) -0.2369(4) 0.0506(18) Uani 1 d . . .
H26 H 1.0730 3.4202 -0.1975 0.061 Uiso 1 calc . . R
C325 C 0.9365(7) 3.4086(5) -0.4415(3) 0.062(2) Uani 1 d . . .
H325 H 0.9319 3.4382 -0.4769 0.074 Uiso 1 calc . . R
C326 C 0.8779(6) 3.4254(4) -0.3868(3) 0.0463(17) Uani 1 d . . .
H326 H 0.8359 3.4667 -0.3849 0.056 Uiso 1 calc . . R
C25 C 1.1690(7) 3.4185(5) -0.2769(6) 0.077(3) Uani 1 d . . .
H25 H 1.2153 3.3818 -0.2639 0.092 Uiso 1 calc . . R
C322 C 0.9480(6) 3.3177(4) -0.3378(3) 0.0476(17) Uani 1 d . . .
H322 H 0.9520 3.2866 -0.3034 0.057 Uiso 1 calc . . R
C324 C 1.0016(6) 3.3485(6) -0.4442(4) 0.070(3) Uani 1 d . . .
H324 H 1.0421 3.3386 -0.4808 0.084 Uiso 1 calc . . R
C24 C 1.1839(8) 3.4495(6) -0.3351(6) 0.091(4) Uani 1 d . . .
H24 H 1.2394 3.4334 -0.3622 0.109 Uiso 1 calc . . R
C323 C 1.0068(6) 3.3035(5) -0.3933(4) 0.062(2) Uani 1 d . . .
H323 H 1.0502 3.2629 -0.3958 0.074 Uiso 1 calc . . R
Cl1B Cl 0.6364(2) 3.76047(12) -0.22161(11) 0.0655(6) Uani 1 d . . .
Cl1A Cl 0.68848(19) 3.76991(13) -0.08628(10) 0.0713(6) Uani 1 d . . .
Cl2B Cl 1.7018(3) 3.5396(2) 0.50642(13) 0.1056(11) Uani 1 d . . .
Cl2A Cl 1.5294(2) 3.63076(13) 0.55622(14) 0.0895(8) Uani 1 d . . .
C313 C 0.6511(6) 3.2088(4) -0.2158(3) 0.0451(17) Uani 1 d . . .
H313 H 0.5847 3.1855 -0.2238 0.054 Uiso 1 calc . . R
N3 N 0.5857(4) 3.4248(2) -0.1216(2) 0.0277(10) Uani 1 d . . .
F4 F 1.0841(4) 3.1749(2) -0.1044(2) 0.0692(13) Uani 1 d . . .
C1 C 0.8248(4) 3.4396(3) -0.1380(2) 0.0242(11) Uani 1 d . . .
H1A H 0.7742 3.4081 -0.1202 0.029 Uiso 1 calc . . R
N2 N 0.6990(4) 3.5274(3) -0.0655(2) 0.0349(11) Uani 1 d . . .
C2 C 0.8309(4) 3.4592(3) -0.2050(3) 0.0245(11) Uani 1 d . . .
C34 C 0.6665(5) 3.4850(4) 0.0405(3) 0.0350(14) Uani 1 d . . .
H34 H 0.6335 3.4523 0.0677 0.042 Uiso 1 calc . . R
C31 C 0.7548(5) 3.5822(3) -0.0410(3) 0.0393(14) Uani 1 d . . .
H31 H 0.7832 3.6165 -0.0684 0.047 Uiso 1 calc . . R
C35 C 0.6536(4) 3.4794(3) -0.0252(3) 0.0291(12) Uani 1 d . . .
C6 C 0.9112(5) 3.4776(3) -0.1033(3) 0.0330(13) Uani 1 d . . .
H6 H 0.9260 3.4714 -0.0601 0.040 Uiso 1 calc . . R
C37 C 0.5266(5) 3.3733(3) -0.0220(3) 0.0348(13) Uani 1 d . . .
H37 H 0.5301 3.3723 0.0223 0.042 Uiso 1 calc . . R
C36 C 0.5883(5) 3.4233(3) -0.0562(3) 0.0292(12) Uani 1 d . . .
C312 C 0.6712(5) 3.2742(3) -0.2419(3) 0.0348(13) Uani 1 d . . .
H312 H 0.6185 3.2945 -0.2686 0.042 Uiso 1 calc . . R
F3 F 1.1932(5) 3.2435(3) -0.0421(3) 0.103(2) Uani 1 d . . .
C314 C 0.7312(6) 3.1779(4) -0.1774(3) 0.0492(17) Uani 1 d . . .
H314 H 0.7186 3.1332 -0.1599 0.059 Uiso 1 calc . . R
C39 C 0.4559(5) 3.3275(3) -0.1194(3) 0.0394(15) Uani 1 d . . .
H39 H 0.4121 3.2955 -0.1420 0.047 Uiso 1 calc . . R
C311 C 0.7677(4) 3.3108(3) -0.2294(3) 0.0305(12) Uani 1 d . . .
C315 C 0.8294(5) 3.2128(3) -0.1649(3) 0.0408(15) Uani 1 d . . .
H315 H 0.8829 3.1918 -0.1391 0.049 Uiso 1 calc . . R
C33 C 0.7295(6) 3.5402(4) 0.0645(3) 0.0463(16) Uani 1 d . . .
H33 H 0.7430 3.5435 0.1081 0.056 Uiso 1 calc . . R
C40 C 0.5177(5) 3.3782(3) -0.1511(3) 0.0397(15) Uani 1 d . . .
H40 H 0.5120 3.3804 -0.1953 0.048 Uiso 1 calc . . R
C316 C 0.8477(5) 3.2794(3) -0.1912(3) 0.0358(14) Uani 1 d . . .
H316 H 0.9139 3.3030 -0.1832 0.043 Uiso 1 calc . . R
F2 F 1.0559(6) 3.2918(4) -0.0967(4) 0.144(3) Uani 1 d . . .
C38 C 0.4603(5) 3.3251(3) -0.0542(3) 0.0409(15) Uani 1 d . . .
H38 H 0.4192 3.2916 -0.0318 0.049 Uiso 1 calc . . R
C1S C 0.5847(7) 3.7643(4) -0.1437(4) 0.062(2) Uani 1 d . . .
H1SA H 0.5365 3.8052 -0.1399 0.075 Uiso 1 calc . . R
H1SB H 0.5405 3.7222 -0.1357 0.075 Uiso 1 calc . . R
C32 C 0.7714(6) 3.5893(4) 0.0239(3) 0.0459(17) Uani 1 d . . .
H32 H 0.8112 3.6277 0.0398 0.055 Uiso 1 calc . . R
F1 F 1.2016(7) 3.2515(5) -0.1457(4) 0.171(4) Uani 1 d . . .
B1 B 1.1350(8) 3.2402(5) -0.0974(4) 0.053(2) Uani 1 d . . .
C2S C 1.6602(8) 3.5960(5) 0.5683(5) 0.081(3) Uani 1 d . . .
H2SA H 1.6609 3.5698 0.6081 0.097 Uiso 1 calc . . R
H2SB H 1.7129 3.6346 0.5720 0.097 Uiso 1 calc . . R
C16 C 1.2680(7) 3.7602(4) 0.0035(4) 0.067(2) Uani 1 d . . .
H16A H 1.1976 3.7839 0.0048 0.100 Uiso 1 calc . . GR
H16B H 1.3262 3.7943 0.0096 0.100 Uiso 1 calc . . GR
H16C H 1.2711 3.7253 0.0369 0.100 Uiso 1 calc . . GR


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Os1 N1 2.022(5) . ?
Os1 Cl1 2.4242(16) . ?
Os1 C302 2.119(6) . ?
Os1 N3 2.100(5) . ?
Os1 C1 2.199(5) . ?
Os1 N2 2.170(5) . ?
Os1 C2 2.157(5) . ?
C21 C3 1.523(9) . ?
C21 C22 1.362(10) . ?
C21 C26 1.384(9) . ?
N1 C4 1.290(7) . ?
C7 C10 1.492(8) . ?
C7 C3 1.535(8) . ?
C7 C6 1.323(9) . ?
C23 C22 1.378(12) . ?
C23 C24 1.391(17) . ?
C11 C10 1.390(8) . ?
C11 C12 1.392(9) . ?
C10 C15 1.413(8) . ?
C3 C4 1.532(8) . ?
C3 C2 1.593(7) . ?
O1 C13 1.374(7) . ?
O1 C16 1.437(9) . ?
C13 C12 1.387(9) . ?
C13 C14 1.391(9) . ?
C15 C14 1.386(9) . ?
C4 C5 1.496(8) . ?
C303 C304 1.414(12) . ?
C303 C302 1.397(9) . ?
C304 C305 1.380(11) . ?
P1 C321 1.811(6) . ?
P1 C301 1.771(6) . ?
P1 C2 1.807(6) . ?
P1 C311 1.817(6) . ?
C306 C301 1.399(8) . ?
C306 C305 1.387(9) . ?
C321 C326 1.417(9) . ?
C321 C322 1.395(9) . ?
C301 C302 1.394(9) . ?
C26 C25 1.394(11) . ?
C325 C326 1.384(10) . ?
C325 C324 1.380(13) . ?
C25 C24 1.365(15) . ?
C322 C323 1.389(10) . ?
C324 C323 1.363(13) . ?
Cl1B C1S 1.749(9) . ?
Cl1A C1S 1.741(8) . ?
Cl2B C2S 1.750(10) . ?
Cl2A C2S 1.728(10) . ?
C313 C312 1.370(9) . ?
C313 C314 1.387(10) . ?
N3 C36 1.373(7) . ?
N3 C40 1.352(8) . ?
F4 B1 1.383(10) . ?
C1 C2 1.455(7) . ?
C1 C6 1.459(8) . ?
N2 C31 1.335(8) . ?
N2 C35 1.355(8) . ?
C34 C35 1.390(9) . ?
C34 C33 1.383(10) . ?
C31 C32 1.383(9) . ?
C35 C36 1.470(8) . ?
C37 C36 1.399(8) . ?
C37 C38 1.386(9) . ?
C312 C311 1.378(8) . ?
F3 B1 1.356(10) . ?
C314 C315 1.381(9) . ?
C39 C40 1.383(9) . ?
C39 C38 1.369(9) . ?
C311 C316 1.387(8) . ?
C315 C316 1.388(8) . ?
C33 C32 1.355(10) . ?
F2 B1 1.364(11) . ?
F1 B1 1.311(11) . ?

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 Os1 Cl1 86.36(13) . . ?
N1 Os1 C302 91.1(2) . . ?
N1 Os1 N3 172.77(18) . . ?
N1 Os1 C1 97.82(19) . . ?
N1 Os1 N2 97.97(19) . . ?
N1 Os1 C2 75.64(18) . . ?
C302 Os1 Cl1 88.74(19) . . ?
C302 Os1 C1 114.7(2) . . ?
C302 Os1 N2 164.4(2) . . ?
C302 Os1 C2 83.3(2) . . ?
N3 Os1 Cl1 87.99(13) . . ?
N3 Os1 C302 93.3(2) . . ?
N3 Os1 C1 85.55(19) . . ?
N3 Os1 N2 76.51(19) . . ?
N3 Os1 C2 110.58(18) . . ?
C1 Os1 Cl1 155.95(14) . . ?
N2 Os1 Cl1 79.24(15) . . ?
N2 Os1 C1 76.7(2) . . ?
C2 Os1 Cl1 160.11(14) . . ?
C2 Os1 C1 39.01(19) . . ?
C2 Os1 N2 111.2(2) . . ?
C22 C21 C3 123.6(6) . . ?
C22 C21 C26 120.6(7) . . ?
C26 C21 C3 115.8(6) . . ?
C4 N1 Os1 126.5(4) . . ?
C10 C7 C3 123.0(5) . . ?
C6 C7 C10 125.1(6) . . ?
C6 C7 C3 111.7(6) . . ?
C22 C23 C24 120.5(10) . . ?
C10 C11 C12 123.7(6) . . ?
C11 C10 C7 120.2(5) . . ?
C11 C10 C15 116.0(5) . . ?
C15 C10 C7 123.8(5) . . ?
C21 C3 C7 112.3(5) . . ?
C21 C3 C4 118.6(5) . . ?
C21 C3 C2 112.7(5) . . ?
C7 C3 C2 101.5(4) . . ?
C4 C3 C7 103.4(5) . . ?
C4 C3 C2 106.6(4) . . ?
C21 C22 C23 119.7(9) . . ?
C13 O1 C16 116.8(6) . . ?
O1 C13 C12 124.9(6) . . ?
O1 C13 C14 115.2(6) . . ?
C12 C13 C14 120.0(6) . . ?
C13 C12 C11 118.5(6) . . ?
C14 C15 C10 121.4(6) . . ?
C15 C14 C13 120.4(6) . . ?
N1 C4 C3 113.1(5) . . ?
N1 C4 C5 120.6(5) . . ?
C5 C4 C3 125.6(5) . . ?
C302 C303 C304 120.7(7) . . ?
C305 C304 C303 121.6(7) . . ?
C321 P1 C311 105.8(3) . . ?
C301 P1 C321 106.6(3) . . ?
C301 P1 C2 103.6(3) . . ?
C301 P1 C311 110.1(3) . . ?
C2 P1 C321 121.9(3) . . ?
C2 P1 C311 108.6(3) . . ?
C305 C306 C301 119.0(6) . . ?
C326 C321 P1 118.2(5) . . ?
C322 C321 P1 122.2(5) . . ?
C322 C321 C326 119.4(6) . . ?
C306 C301 P1 122.1(5) . . ?
C302 C301 P1 113.9(5) . . ?
C302 C301 C306 124.0(6) . . ?
C304 C305 C306 118.8(7) . . ?
C303 C302 Os1 122.7(5) . . ?
C301 C302 Os1 121.3(5) . . ?
C301 C302 C303 115.9(6) . . ?
C21 C26 C25 119.6(8) . . ?
C324 C325 C326 120.8(8) . . ?
C325 C326 C321 119.0(7) . . ?
C24 C25 C26 120.0(9) . . ?
C323 C322 C321 119.7(7) . . ?
C323 C324 C325 120.3(7) . . ?
C25 C24 C23 119.6(9) . . ?
C324 C323 C322 120.9(8) . . ?
C312 C313 C314 119.1(7) . . ?
C36 N3 Os1 116.6(4) . . ?
C40 N3 Os1 126.1(4) . . ?
C40 N3 C36 117.1(5) . . ?
C2 C1 Os1 68.9(3) . . ?
C2 C1 C6 108.7(5) . . ?
C6 C1 Os1 115.5(4) . . ?
C31 N2 Os1 125.7(4) . . ?
C31 N2 C35 118.7(6) . . ?
C35 N2 Os1 115.4(4) . . ?
C3 C2 Os1 110.7(3) . . ?
C3 C2 P1 126.0(4) . . ?
P1 C2 Os1 108.3(2) . . ?
C1 C2 Os1 72.1(3) . . ?
C1 C2 C3 106.0(4) . . ?
C1 C2 P1 120.7(4) . . ?
C33 C34 C35 118.7(6) . . ?
N2 C31 C32 121.7(6) . . ?
N2 C35 C34 121.4(6) . . ?
N2 C35 C36 114.9(5) . . ?
C34 C35 C36 123.6(6) . . ?
C7 C6 C1 111.9(5) . . ?
C38 C37 C36 120.0(6) . . ?
N3 C36 C35 116.0(5) . . ?
N3 C36 C37 121.0(5) . . ?
C37 C36 C35 122.9(5) . . ?
C313 C312 C311 121.6(6) . . ?
C315 C314 C313 120.5(6) . . ?
C38 C39 C40 118.8(6) . . ?
C312 C311 P1 120.5(5) . . ?
C312 C311 C316 119.0(5) . . ?
C316 C311 P1 120.4(4) . . ?
C314 C315 C316 119.5(6) . . ?
C32 C33 C34 119.4(6) . . ?
N3 C40 C39 123.9(6) . . ?
C311 C316 C315 120.3(6) . . ?
C39 C38 C37 119.2(6) . . ?
Cl1A C1S Cl1B 113.0(5) . . ?
C33 C32 C31 119.9(6) . . ?
F3 B1 F4 111.3(7) . . ?
F3 B1 F2 108.7(8) . . ?
F2 B1 F4 109.0(7) . . ?
F1 B1 F4 109.6(8) . . ?
F1 B1 F3 109.6(8) . . ?
F1 B1 F2 108.7(10) . . ?
Cl2A C2S Cl2B 112.6(5) . . ?

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

data_1
_database_code_depnum_ccdc_archive 'CCDC 1038537'
_audit_update_record             
;
2015-02-11 deposited with the CCDC.
2015-03-26 downloaded from the CCDC.
;
_audit_creation_date             2015-02-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.12.26 svn.r3119 for OlexSys, GUI svn.r4975)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C51 H53 Cl2 N3 Os P, C H2 Cl2, B F4'
_chemical_formula_sum            'C52 H55 B Cl4 F4 N3 Os P'
_chemical_formula_weight         1171.77
_chemical_absolute_configuration ad
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 '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'
Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        'C 1 c 1'
_space_group_name_Hall           'C -2yc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 'x, -y, z+1/2'
3 'x+1/2, y+1/2, z'
4 'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   19.3445(9)
_cell_length_b                   16.8974(6)
_cell_length_c                   16.1902(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 111.0040(10)
_cell_angle_gamma                90.00
_cell_volume                     4940.5(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      ?
_cell_measurement_theta_min      ?
_exptl_absorpt_coefficient_mu    2.884
_exptl_absorpt_correction_T_max  0.315
_exptl_absorpt_correction_T_min  0.137
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2352
_exptl_crystal_size_max          1.0
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.4
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_unetI/netI     0.0763
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18915
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         3.25
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                6954
_reflns_number_total             7754
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         1.433
_refine_diff_density_min         -1.148
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.005(7)
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     596
_refine_ls_number_reflns         7754
_refine_ls_number_restraints     47
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0344
_refine_ls_restrained_S_all      1.115
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0304P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0737
_refine_ls_wR_factor_ref         0.0858
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C35-C36
 1.54 with sigma of 0.02
 C32-C33
 1.54 with sigma of 0.02
 C32-N3
 1.47 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C37) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C34)
\\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C36) \\sim Ueq, Uanis(C35) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C45) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Ternary CH refined with riding coordinates:
 C42(H42), C32(H32)
4.b Secondary CH2 refined with riding coordinates:
 C100(H10A,H10B), C46(H46A,H46B), C47(H47A,H47B), C43(H43A,H43B), C44(H44A,
 H44B), C45(H45A,H45B), C37(H37A,H37B), C34(H34A,H34B), C35(H35A,H35B),
 C33(H33A,H33B), C36(H36A,H36B)
4.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C14(H14), C322(H322), C6(H6), C26(H26), C312(H312), C12(H12),
 C303(H303), C304(H304), C16(H16), C1(H1), C324(H324), C306(H306), C316(H316),
 C326(H326), C302(H302), C314(H314), C25(H25), C323(H323), C315(H315), C13(H13),
  C305(H305), C24(H24), C22(H22), C23(H23), C325(H325), N1(H1A), C313(H313)
4.d Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
C15 C 0.0747(5) 0.5100(5) 0.2361(6) 0.050(3) Uani 1 d . . . .
H15 H 0.1163 0.5339 0.2311 0.060 Uiso 1 calc . . R .
C14 C 0.0119(6) 0.5541(5) 0.2230(5) 0.052(3) Uani 1 d . . . .
H14 H 0.0115 0.6081 0.2119 0.062 Uiso 1 calc . . R .
C42 C -0.0827(5) 0.0008(4) 0.4487(5) 0.038(2) Uani 1 d . . . .
H42 H -0.0545 0.0079 0.5119 0.045 Uiso 1 calc . . R .
C3 C 0.0120(4) 0.3071(4) 0.2906(4) 0.0246(16) Uani 1 d . . . .
C322 C 0.0684(4) 0.4767(4) 0.4631(4) 0.0300(17) Uani 1 d . . . .
H322 H 0.0282 0.4979 0.4175 0.036 Uiso 1 calc . . R .
C4 C 0.0863(4) 0.2659(4) 0.3422(4) 0.0268(16) Uani 1 d . . . .
C6 C -0.0904(4) 0.2132(4) 0.2352(4) 0.0254(16) Uani 1 d . . . .
H6 H -0.1242 0.1760 0.2015 0.031 Uiso 1 calc . . R .
C11 C 0.0143(4) 0.3935(4) 0.2629(6) 0.0269(19) Uani 1 d . . . .
C26 C -0.1151(5) 0.2643(4) 0.0526(4) 0.0313(18) Uani 1 d . . . .
H26 H -0.1549 0.2454 0.0662 0.038 Uiso 1 calc . . R .
C41 C -0.0355(4) 0.0869(5) 0.3472(4) 0.0272(17) Uani 1 d . . . .
C312 C -0.0838(5) 0.2776(4) 0.5675(4) 0.038(2) Uani 1 d . . . .
H312 H -0.1154 0.3210 0.5567 0.046 Uiso 1 calc . . R .
C12 C -0.0493(5) 0.4379(5) 0.2458(5) 0.034(2) Uani 1 d . . . .
H12 H -0.0919 0.4135 0.2473 0.041 Uiso 1 calc . . R .
C303 C -0.2288(4) 0.4498(5) 0.3665(5) 0.041(2) Uani 1 d . . . .
H303 H -0.2743 0.4439 0.3209 0.050 Uiso 1 calc . . R .
C304 C -0.2200(5) 0.5062(4) 0.4336(5) 0.035(2) Uani 1 d . . . .
H304 H -0.2609 0.5353 0.4334 0.042 Uiso 1 calc . . R .
C5 C 0.1570(4) 0.3062(4) 0.3998(4) 0.0319(17) Uani 1 d . . . .
H5A H 0.1926 0.3041 0.3711 0.048 Uiso 1 calc . . GR .
H5B H 0.1764 0.2796 0.4558 0.048 Uiso 1 calc . . GR .
H5C H 0.1467 0.3604 0.4089 0.048 Uiso 1 calc . . GR .
C2 C -0.0325(4) 0.2988(4) 0.3531(4) 0.0245(15) Uani 1 d . . . .
C16 C 0.0764(5) 0.4285(5) 0.2572(5) 0.035(2) Uani 1 d . . . .
H16 H 0.1192 0.3990 0.2671 0.042 Uiso 1 calc . . R .
C1 C -0.0863(4) 0.2432(4) 0.3210(4) 0.0223(15) Uani 1 d . . . .
H1 H -0.1169 0.2262 0.3505 0.027 Uiso 1 calc . . R .
C324 C 0.1933(5) 0.4847(6) 0.5618(6) 0.048(3) Uani 1 d . . . .
H324 H 0.2386 0.5109 0.5821 0.057 Uiso 1 calc . . R .
C21 C -0.0458(5) 0.2730(4) 0.1186(4) 0.0301(18) Uani 1 d . . . .
C311 C -0.0301(4) 0.2736(4) 0.5293(4) 0.0233(15) Uani 1 d . . . .
C306 C -0.0921(4) 0.4742(4) 0.5007(4) 0.0289(17) Uani 1 d . . . .
H306 H -0.0461 0.4835 0.5442 0.035 Uiso 1 calc . . R .
C316 C 0.0170(4) 0.2079(4) 0.5457(4) 0.0301(17) Uani 1 d . . . .
H316 H 0.0515 0.2039 0.5182 0.036 Uiso 1 calc . . R .
C326 C 0.1189(4) 0.3744(4) 0.5696(5) 0.0303(18) Uani 1 d . . . .
H326 H 0.1136 0.3267 0.5955 0.036 Uiso 1 calc . . R .
C302 C -0.1697(4) 0.4037(4) 0.3690(4) 0.0309(18) Uani 1 d . . . .
H302 H -0.1750 0.3650 0.3262 0.037 Uiso 1 calc . . R .
C301 C -0.1008(4) 0.4158(4) 0.4373(4) 0.0242(15) Uani 1 d . . . .
C314 C -0.0407(5) 0.1538(5) 0.6412(5) 0.046(2) Uani 1 d . . . .
H314 H -0.0433 0.1146 0.6803 0.056 Uiso 1 calc . . R .
C25 C -0.1241(5) 0.2843(4) -0.0339(5) 0.043(2) Uani 1 d . . . .
H25 H -0.1702 0.2772 -0.0781 0.051 Uiso 1 calc . . R .
C323 C 0.1339(4) 0.5169(5) 0.4921(5) 0.035(2) Uani 1 d . . . .
H323 H 0.1391 0.5645 0.4661 0.042 Uiso 1 calc . . R .
C315 C 0.0123(5) 0.1493(5) 0.6024(5) 0.042(2) Uani 1 d . . . .
H315 H 0.0448 0.1067 0.6147 0.051 Uiso 1 calc . . R .
C13 C -0.0508(5) 0.5173(5) 0.2267(5) 0.046(2) Uani 1 d . . . .
H13 H -0.0940 0.5462 0.2162 0.056 Uiso 1 calc . . R .
C305 C -0.1540(5) 0.5190(4) 0.4980(5) 0.035(2) Uani 1 d . . . .
H305 H -0.1493 0.5575 0.5407 0.041 Uiso 1 calc . . R .
C31 C 0.0468(5) 0.1324(4) 0.1631(6) 0.040(3) Uani 1 d . . . .
C24 C -0.0678(6) 0.3139(5) -0.0556(5) 0.047(2) Uani 1 d . . . .
H24 H -0.0756 0.3275 -0.1139 0.057 Uiso 1 calc . . R .
C22 C 0.0101(5) 0.3038(4) 0.0931(5) 0.041(2) Uani 1 d . . . .
H22 H 0.0567 0.3113 0.1363 0.049 Uiso 1 calc . . R .
C321 C 0.0605(4) 0.4041(4) 0.5006(4) 0.0257(16) Uani 1 d . . . .
C7 C -0.0346(4) 0.2499(4) 0.2113(4) 0.0252(16) Uani 1 d . . . .
C23 C 0.0002(6) 0.3236(5) 0.0082(6) 0.049(2) Uani 1 d . . . .
H23 H 0.0394 0.3435 -0.0060 0.059 Uiso 1 calc . . R .
C325 C 0.1851(4) 0.4140(5) 0.6010(5) 0.0374(19) Uani 1 d . . . .
H325 H 0.2243 0.3935 0.6483 0.045 Uiso 1 calc . . R .
N1 N 0.0836(3) 0.1903(3) 0.3358(4) 0.0280(14) Uani 1 d . . . .
H1A H 0.1210 0.1643 0.3703 0.034 Uiso 1 calc . . R .
N2 N -0.0532(4) 0.0543(4) 0.3976(4) 0.0350(15) Uani 1 d . . . .
N3 N 0.0788(5) 0.1294(5) 0.1133(5) 0.069(3) Uani 1 d . . D .
P1 P -0.02432(11) 0.34892(11) 0.45331(12) 0.0227(4) Uani 1 d . . . .
Cl1 Cl 0.07716(11) 0.01066(11) 0.29474(14) 0.0404(5) Uani 1 d . . . .
Cl2 Cl -0.10025(11) 0.04838(11) 0.14914(11) 0.0327(4) Uani 1 d . . . .
Os1 Os -0.00112(3) 0.127082(12) 0.25187(3) 0.02354(8) Uani 1 d . . . .
C313 C -0.0901(5) 0.2168(5) 0.6218(6) 0.050(2) Uani 1 d . . . .
H313 H -0.1275 0.2182 0.6453 0.060 Uiso 1 calc . . R .
Cl3 Cl 0.0699(2) 0.7431(2) 0.3382(2) 0.1082(13) Uani 1 d . . . .
Cl4 Cl 0.2253(3) 0.7180(3) 0.3767(4) 0.171(2) Uani 1 d . . . .
C100 C 0.1472(9) 0.7726(9) 0.3164(9) 0.121(6) Uani 1 d . . . .
H10A H 0.1566 0.8282 0.3309 0.145 Uiso 1 calc . . R .
H10B H 0.1378 0.7663 0.2538 0.145 Uiso 1 calc . . R .
F1 F 0.2899(3) 0.1225(3) 0.6433(4) 0.0575(15) Uani 1 d . . . .
F3 F 0.1830(4) 0.1456(4) 0.5302(4) 0.0801(19) Uani 1 d . . . .
F4 F 0.1841(4) 0.1384(4) 0.6705(5) 0.079(2) Uani 1 d . . . .
F5 F 0.2347(3) 0.2407(3) 0.6259(5) 0.092(2) Uani 1 d . . . .
B1 B 0.2229(5) 0.1616(6) 0.6165(6) 0.039(2) Uani 1 d . . . .
C46 C -0.2098(6) 0.0045(10) 0.3353(8) 0.106(6) Uani 1 d . . . .
H46A H -0.2614 0.0140 0.3269 0.127 Uiso 1 calc . . R .
H46B H -0.1969 0.0394 0.2955 0.127 Uiso 1 calc . . R .
C47 C -0.1630(6) 0.0253(8) 0.4289(6) 0.078(4) Uani 1 d . . . .
H47A H -0.1819 -0.0014 0.4694 0.094 Uiso 1 calc . . R .
H47B H -0.1654 0.0819 0.4377 0.094 Uiso 1 calc . . R .
C43 C -0.0749(6) -0.0824(5) 0.4234(5) 0.054(3) Uani 1 d . . . .
H43A H -0.0892 -0.1177 0.4618 0.064 Uiso 1 calc . . R .
H43B H -0.0232 -0.0925 0.4330 0.064 Uiso 1 calc . . R .
C44 C -0.1220(8) -0.1015(6) 0.3262(7) 0.080(4) Uani 1 d . . . .
H44A H -0.1038 -0.0722 0.2867 0.097 Uiso 1 calc . . R .
H44B H -0.1194 -0.1575 0.3149 0.097 Uiso 1 calc . . R .
C45 C -0.2018(9) -0.0778(10) 0.3110(9) 0.110(5) Uani 1 d . . . U
H45A H -0.2316 -0.0854 0.2490 0.131 Uiso 1 calc . . R .
H45B H -0.2211 -0.1126 0.3452 0.131 Uiso 1 calc . . R .
C37 C 0.1891(8) 0.2172(7) 0.1020(10) 0.098(5) Uani 1 d . . . U
H37A H 0.2183 0.2258 0.0650 0.118 Uiso 1 calc . . R .
H37B H 0.1620 0.2657 0.1009 0.118 Uiso 1 calc . . R .
C34 C 0.2173(8) 0.0600(7) 0.1636(10) 0.092(4) Uani 1 d . . . U
H34A H 0.2480 0.0168 0.1571 0.110 Uiso 1 calc . . R .
H34B H 0.1940 0.0428 0.2046 0.110 Uiso 1 calc . . R .
C35 C 0.2673(10) 0.1310(9) 0.2041(11) 0.132(6) Uani 1 d . . D U
H35A H 0.2865 0.1242 0.2678 0.158 Uiso 1 calc . . R .
H35B H 0.3092 0.1288 0.1847 0.158 Uiso 1 calc . . R .
C32 C 0.1307(9) 0.1510(10) 0.0569(8) 0.135(7) Uani 1 d . . D U
H32 H 0.1040 0.1582 -0.0067 0.162 Uiso 1 calc . . R .
C33 C 0.1620(11) 0.0746(9) 0.0816(12) 0.138(7) Uani 1 d . . D U
H33A H 0.1214 0.0390 0.0768 0.165 Uiso 1 calc . . R .
H33B H 0.1817 0.0583 0.0369 0.165 Uiso 1 calc . . R .
C36 C 0.2368(11) 0.2067(10) 0.1858(13) 0.156(7) Uani 1 d . . D U
H36A H 0.2111 0.2181 0.2261 0.187 Uiso 1 calc . . R .
H36B H 0.2768 0.2447 0.1975 0.187 Uiso 1 calc . . R .


_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
C15 C14 1.375(13) . ?
C15 C16 1.417(11) . ?
C14 C13 1.382(13) . ?
C42 N2 1.471(10) . ?
C42 C47 1.525(12) . ?
C42 C43 1.487(11) . ?
C3 C4 1.546(10) . ?
C3 C11 1.533(9) . ?
C3 C2 1.552(10) . ?
C3 C7 1.602(9) . ?
C322 C323 1.364(10) . ?
C322 C321 1.402(10) . ?
C4 C5 1.512(9) . ?
C4 N1 1.280(9) . ?
C6 C1 1.454(9) . ?
C6 C7 1.412(10) . ?
C6 Os1 2.199(7) . ?
C11 C12 1.381(11) . ?
C11 C16 1.370(11) . ?
C26 C21 1.390(10) . ?
C26 C25 1.388(10) . ?
C41 N2 1.135(9) . ?
C41 Os1 2.006(7) . ?
C312 C311 1.387(11) . ?
C312 C313 1.386(11) . ?
C12 C13 1.375(11) . ?
C303 C304 1.409(11) . ?
C303 C302 1.373(10) . ?
C304 C305 1.346(11) . ?
C2 C1 1.360(10) . ?
C2 P1 1.786(7) . ?
C324 C323 1.401(12) . ?
C324 C325 1.388(13) . ?
C21 C22 1.391(11) . ?
C21 C7 1.490(9) . ?
C311 C316 1.400(9) . ?
C311 P1 1.801(7) . ?
C306 C301 1.391(9) . ?
C306 C305 1.403(10) . ?
C316 C315 1.374(11) . ?
C326 C321 1.367(10) . ?
C326 C325 1.371(11) . ?
C302 C301 1.408(9) . ?
C301 P1 1.804(7) . ?
C314 C315 1.383(13) . ?
C314 C313 1.389(12) . ?
C25 C24 1.355(13) . ?
C31 N3 1.181(12) . ?
C31 Os1 1.971(11) . ?
C24 C23 1.360(13) . ?
C22 C23 1.360(11) . ?
C321 P1 1.802(7) . ?
C7 Os1 2.202(7) . ?
N1 Os1 2.020(6) . ?
N3 C32 1.622(16) . ?
Cl1 Os1 2.4272(18) . ?
Cl2 Os1 2.4343(17) . ?
Cl3 C100 1.729(15) . ?
Cl4 C100 1.740(15) . ?
F1 B1 1.379(10) . ?
F3 B1 1.360(11) . ?
F4 B1 1.395(12) . ?
F5 B1 1.357(11) . ?
C46 C47 1.503(16) . ?
C46 C45 1.468(19) . ?
C43 C44 1.544(13) . ?
C44 C45 1.527(19) . ?
C37 C32 1.571(18) . ?
C37 C36 1.35(2) . ?
C34 C35 1.533(19) . ?
C34 C33 1.396(18) . ?
C35 C36 1.395(15) . ?
C32 C33 1.421(14) . ?

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
C14 C15 C16 120.4(9) . . ?
C15 C14 C13 119.3(8) . . ?
N2 C42 C47 106.6(6) . . ?
N2 C42 C43 109.1(7) . . ?
C43 C42 C47 113.3(9) . . ?
C4 C3 C2 103.4(5) . . ?
C4 C3 C7 108.0(6) . . ?
C11 C3 C4 117.9(6) . . ?
C11 C3 C2 111.0(6) . . ?
C11 C3 C7 114.1(5) . . ?
C2 C3 C7 100.6(5) . . ?
C323 C322 C321 121.2(7) . . ?
C5 C4 C3 126.2(6) . . ?
N1 C4 C3 113.7(6) . . ?
N1 C4 C5 120.0(7) . . ?
C1 C6 Os1 110.0(4) . . ?
C7 C6 C1 108.8(6) . . ?
C7 C6 Os1 71.4(4) . . ?
C12 C11 C3 117.2(7) . . ?
C16 C11 C3 123.3(7) . . ?
C16 C11 C12 119.4(7) . . ?
C25 C26 C21 119.3(8) . . ?
N2 C41 Os1 170.7(7) . . ?
C311 C312 C313 119.8(7) . . ?
C13 C12 C11 121.3(9) . . ?
C302 C303 C304 119.6(7) . . ?
C305 C304 C303 121.6(8) . . ?
C3 C2 P1 131.4(5) . . ?
C1 C2 C3 109.9(6) . . ?
C1 C2 P1 118.8(6) . . ?
C11 C16 C15 119.4(9) . . ?
C2 C1 C6 112.3(6) . . ?
C325 C324 C323 120.5(8) . . ?
C26 C21 C7 120.0(7) . . ?
C22 C21 C26 116.7(7) . . ?
C22 C21 C7 123.4(7) . . ?
C312 C311 C316 119.6(6) . . ?
C312 C311 P1 120.7(5) . . ?
C316 C311 P1 119.6(6) . . ?
C301 C306 C305 119.0(7) . . ?
C315 C316 C311 120.3(8) . . ?
C321 C326 C325 120.8(7) . . ?
C303 C302 C301 118.9(7) . . ?
C306 C301 C302 120.8(7) . . ?
C306 C301 P1 117.6(5) . . ?
C302 C301 P1 121.2(5) . . ?
C315 C314 C313 120.1(8) . . ?
C24 C25 C26 121.9(8) . . ?
C322 C323 C324 118.5(8) . . ?
C316 C315 C314 120.0(8) . . ?
C12 C13 C14 120.1(9) . . ?
C304 C305 C306 120.0(7) . . ?
N3 C31 Os1 173.9(8) . . ?
C23 C24 C25 119.8(8) . . ?
C23 C22 C21 123.4(8) . . ?
C322 C321 P1 119.5(5) . . ?
C326 C321 C322 119.3(7) . . ?
C326 C321 P1 121.1(6) . . ?
C3 C7 Os1 108.0(4) . . ?
C6 C7 C3 108.2(6) . . ?
C6 C7 C21 122.7(6) . . ?
C6 C7 Os1 71.2(4) . . ?
C21 C7 C3 119.0(6) . . ?
C21 C7 Os1 117.9(5) . . ?
C24 C23 C22 119.0(9) . . ?
C326 C325 C324 119.7(7) . . ?
C4 N1 Os1 125.6(5) . . ?
C41 N2 C42 168.7(7) . . ?
C31 N3 C32 163.0(10) . . ?
C2 P1 C311 106.2(3) . . ?
C2 P1 C301 111.4(3) . . ?
C2 P1 C321 113.7(3) . . ?
C311 P1 C301 107.0(3) . . ?
C311 P1 C321 110.2(3) . . ?
C321 P1 C301 108.2(3) . . ?
C6 Os1 C7 37.4(3) . . ?
C6 Os1 Cl1 162.40(19) . . ?
C6 Os1 Cl2 83.45(19) . . ?
C41 Os1 C6 81.7(3) . . ?
C41 Os1 C7 113.9(3) . . ?
C41 Os1 N1 94.3(3) . . ?
C41 Os1 Cl1 81.4(2) . . ?
C41 Os1 Cl2 86.7(2) . . ?
C31 Os1 C6 115.7(3) . . ?
C31 Os1 C41 161.6(3) . . ?
C31 Os1 C7 84.5(3) . . ?
C31 Os1 N1 89.2(3) . . ?
C31 Os1 Cl1 80.6(2) . . ?
C31 Os1 Cl2 89.3(2) . . ?
C7 Os1 Cl1 159.3(2) . . ?
C7 Os1 Cl2 103.62(19) . . ?
N1 Os1 C6 98.3(2) . . ?
N1 Os1 C7 77.5(2) . . ?
N1 Os1 Cl1 87.94(16) . . ?
N1 Os1 Cl2 178.09(19) . . ?
Cl1 Os1 Cl2 90.60(7) . . ?
C314 C313 C312 120.0(9) . . ?
Cl3 C100 Cl4 111.9(7) . . ?
F1 B1 F4 108.9(7) . . ?
F3 B1 F1 110.6(8) . . ?
F3 B1 F4 110.7(8) . . ?
F3 B1 F5 108.7(8) . . ?
F5 B1 F1 109.6(8) . . ?
F5 B1 F4 108.3(8) . . ?
C45 C46 C47 114.1(11) . . ?
C46 C47 C42 110.4(10) . . ?
C42 C43 C44 113.3(8) . . ?
C45 C44 C43 107.7(11) . . ?
C46 C45 C44 113.7(11) . . ?
C36 C37 C32 119.5(11) . . ?
C33 C34 C35 114.8(11) . . ?
C36 C35 C34 118.2(14) . . ?
C37 C32 N3 112.6(10) . . ?
C33 C32 N3 85.7(12) . . ?
C33 C32 C37 110.7(12) . . ?
C34 C33 C32 122.1(12) . . ?
C37 C36 C35 114.7(15) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
