#------------------------------------------------------------------------------
#$Date: 2016-03-21 19:19:44 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178845 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/99/4109914.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4109914
loop_
_publ_author_name
'María L. Buil'
'Miguel A. Esteruelas'
'Karin Garcés'
'Montserrat Oliván'
'Enrique Oñate'
_publ_contact_author
;
  Dr. Enrique Oñate
  Departamento de Química Inorgánica - I.C.M.A.
  Universidad de Zaragoza - C.S.I.C.
  50009 Zaragoza, Spain
;
_publ_contact_author_email       enriqueo@unizar.es
_publ_section_title
;
 Understanding the Formation of N-H Tautomers from α-Substituted
 Pyridines: Tautomerization of 2-Ethylpyridine Promoted by Osmium
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10998
_journal_page_last               10999
_journal_paper_doi               10.1021/ja073673r
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C38 H62 B F4 N O Os P2'
_chemical_formula_weight         887.84
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 125.574(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.589(2)
_cell_length_b                   20.399(2)
_cell_length_c                   19.951(2)
_cell_measurement_reflns_used    5720
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      2
_cell_volume                     7808.5(13)
_computing_cell_refinement       'SAINT+ v. 6.1 (Bruker AXS, 2000)'
_computing_data_collection       'SMART v. 5.625 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ v. 6.1 (Bruker AXS, 2000)'
_computing_molecular_graphics    'XP, SHELXTL v. 6.1 (Bruker, 2000)'
_computing_publication_material  'XCIF, SHELXTL v. 6.1 (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       'ω rotations with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0640
_diffrn_reflns_av_sigmaI/netI    0.0937
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            47097
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         2.00
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    3.397
_exptl_absorpt_correction_T_max  0.779
_exptl_absorpt_correction_T_min  0.684
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Absorption correction performed with SADABS program. This is based on the
method of Blessing: Blessing, R. H., Acta Crystallogr., Sect. A 1995, 51, 33.

SADABS: Area-Detector Absorption Correction. Bruker-AXS 
within SAINT+ package, v. 6.1 (2000).
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_description       prism
_exptl_crystal_F_000             3616
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.396
_refine_diff_density_min         -1.110
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.820
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         9748
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      0.843
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0293P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0700
_refine_ls_wR_factor_ref         0.0756
_reflns_number_gt                6594
_reflns_number_total             9748
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja073673rsi20070717_033926_2.cif
_cod_data_source_block           mae240as
_cod_original_cell_volume        7808.3(15)
_cod_database_code               4109914
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Os Os 0.261103(9) 0.565801(9) 0.769553(11) 0.02301(6) Uani 1 1 d D . .
H01 H 0.228(3) 0.4966(13) 0.763(3) 0.074(18) Uiso 1 1 d D . .
H02 H 0.284(3) 0.529(2) 0.851(2) 0.09(2) Uiso 1 1 d D . .
P1 P 0.35087(7) 0.50648(6) 0.77550(7) 0.0268(3) Uani 1 1 d . B .
P2 P 0.17203(7) 0.59899(7) 0.78461(8) 0.0342(3) Uani 1 1 d . D .
O O 0.26275(15) 0.65160(14) 0.71014(17) 0.0257(7) Uani 1 1 d . . .
C1 C 0.1865(2) 0.5484(2) 0.6444(3) 0.0269(11) Uani 1 1 d . . .
C2 C 0.1434(2) 0.4934(2) 0.6034(3) 0.0344(12) Uani 1 1 d . . .
H2 H 0.1486 0.4569 0.6345 0.041 Uiso 1 1 calc R . .
C3 C 0.0940(3) 0.4912(3) 0.5193(3) 0.0399(13) Uani 1 1 d . . .
H3 H 0.0660 0.4543 0.4956 0.048 Uiso 1 1 calc R . .
C4 C 0.0855(3) 0.5433(3) 0.4695(3) 0.0372(13) Uani 1 1 d . . .
H4 H 0.0523 0.5412 0.4128 0.045 Uiso 1 1 calc R . .
C5 C 0.1263(2) 0.5980(2) 0.5048(3) 0.0304(11) Uani 1 1 d . . .
H5 H 0.1219 0.6327 0.4718 0.036 Uiso 1 1 calc R . .
C6 C 0.1747(2) 0.6016(2) 0.5902(3) 0.0266(11) Uani 1 1 d . . .
C7 C 0.2190(2) 0.6572(2) 0.6328(3) 0.0261(10) Uani 1 1 d . . .
C8 C 0.2198(2) 0.7196(2) 0.5957(3) 0.0252(10) Uani 1 1 d . . .
C9 C 0.2834(3) 0.7500(2) 0.6286(3) 0.0325(12) Uani 1 1 d . . .
H9 H 0.3240 0.7308 0.6728 0.039 Uiso 1 1 calc R . .
C10 C 0.2875(3) 0.8082(2) 0.5970(3) 0.0355(12) Uani 1 1 d . . .
H10 H 0.3305 0.8278 0.6188 0.043 Uiso 1 1 calc R . .
C11 C 0.2267(3) 0.8376(2) 0.5322(3) 0.0419(14) Uani 1 1 d . . .
H11 H 0.2290 0.8770 0.5105 0.050 Uiso 1 1 calc R . .
C12 C 0.1633(3) 0.8088(2) 0.5000(3) 0.0389(13) Uani 1 1 d . . .
H12 H 0.1228 0.8290 0.4571 0.047 Uiso 1 1 calc R . .
C13 C 0.1594(3) 0.7497(2) 0.5312(3) 0.0333(12) Uani 1 1 d . . .
H13 H 0.1163 0.7302 0.5089 0.040 Uiso 1 1 calc R . .
C14 C 0.3703(3) 0.4271(2) 0.8307(3) 0.0322(11) Uani 1 1 d . . .
H14 H 0.4023 0.4032 0.8233 0.039 Uiso 1 1 calc R . .
C15 C 0.4071(3) 0.4349(2) 0.9233(3) 0.0387(12) Uani 1 1 d . . .
H15A H 0.3760 0.4551 0.9334 0.058 Uiso 1 1 calc R . .
H15B H 0.4476 0.4620 0.9456 0.058 Uiso 1 1 calc R . .
H15C H 0.4209 0.3926 0.9492 0.058 Uiso 1 1 calc R . .
C16 C 0.3065(3) 0.3835(2) 0.7964(3) 0.0411(13) Uani 1 1 d . . .
H16A H 0.3212 0.3393 0.8154 0.062 Uiso 1 1 calc R . .
H16B H 0.2785 0.3843 0.7373 0.062 Uiso 1 1 calc R . .
H16C H 0.2795 0.3993 0.8150 0.062 Uiso 1 1 calc R . .
C17 C 0.4373(2) 0.5479(2) 0.8363(3) 0.0326(12) Uani 1 1 d . . .
H17 H 0.4451 0.5611 0.8883 0.039 Uiso 1 1 calc R . .
C18 C 0.5003(3) 0.5062(3) 0.8600(3) 0.0498(16) Uani 1 1 d . . .
H18A H 0.4960 0.4930 0.8111 0.075 Uiso 1 1 calc R . .
H18B H 0.5022 0.4680 0.8894 0.075 Uiso 1 1 calc R . .
H18C H 0.5421 0.5314 0.8945 0.075 Uiso 1 1 calc R . .
C19 C 0.4393(3) 0.6108(3) 0.7967(4) 0.0580(18) Uani 1 1 d . . .
H19A H 0.4786 0.6367 0.8373 0.087 Uiso 1 1 calc R . .
H19B H 0.3972 0.6351 0.7749 0.087 Uiso 1 1 calc R . .
H19C H 0.4435 0.6001 0.7529 0.087 Uiso 1 1 calc R . .
C20 C 0.3427(4) 0.4828(3) 0.6807(3) 0.0612(18) Uani 1 1 d D . .
H20 H 0.3912 0.4748 0.7013 0.073 Uiso 1 1 calc R A 1
C21 C 0.3224(3) 0.5373(3) 0.6207(3) 0.0478(15) Uani 1 1 d . B .
H21A H 0.3343 0.5257 0.5837 0.072 Uiso 1 1 calc R . .
H21B H 0.3467 0.5765 0.6500 0.072 Uiso 1 1 calc R . .
H21C H 0.2731 0.5446 0.5899 0.072 Uiso 1 1 calc R . .
C22A C 0.3083(4) 0.4195(3) 0.6393(4) 0.040(2) Uiso 0.70 1 d PD B 1
H22A H 0.2598 0.4215 0.6176 0.060 Uiso 0.70 1 calc PR B 1
H22B H 0.3301 0.3844 0.6785 0.060 Uiso 0.70 1 calc PR B 1
H22C H 0.3129 0.4118 0.5951 0.060 Uiso 0.70 1 calc PR B 1
C22B C 0.3505(11) 0.4154(6) 0.6579(13) 0.057(6) Uiso 0.30 1 d PD B 2
H22D H 0.3314 0.4142 0.6003 0.085 Uiso 0.30 1 calc PR B 2
H22E H 0.3261 0.3847 0.6691 0.085 Uiso 0.30 1 calc PR B 2
H22F H 0.3990 0.4040 0.6897 0.085 Uiso 0.30 1 calc PR B 2
C23 C 0.1408(3) 0.5309(3) 0.8162(3) 0.0441(14) Uani 1 1 d . . .
H23 H 0.1032 0.5486 0.8182 0.053 Uiso 1 1 calc R . .
C24 C 0.1970(3) 0.5059(3) 0.9027(3) 0.0578(17) Uani 1 1 d . . .
H24A H 0.1771 0.4740 0.9188 0.087 Uiso 1 1 calc R . .
H24B H 0.2151 0.5419 0.9408 0.087 Uiso 1 1 calc R . .
H24C H 0.2339 0.4861 0.9028 0.087 Uiso 1 1 calc R . .
C25 C 0.1097(3) 0.4741(3) 0.7548(4) 0.0606(18) Uani 1 1 d . . .
H25A H 0.1464 0.4500 0.7588 0.091 Uiso 1 1 calc R . .
H25B H 0.0785 0.4910 0.7000 0.091 Uiso 1 1 calc R . .
H25C H 0.0845 0.4456 0.7673 0.091 Uiso 1 1 calc R . .
C26 C 0.0902(3) 0.6279(3) 0.6874(4) 0.083(2) Uani 1 1 d D . .
H26 H 0.0855 0.6018 0.6432 0.099 Uiso 1 1 calc R C 1
C27 C 0.0247(3) 0.6222(4) 0.6763(4) 0.092(3) Uani 1 1 d . D .
H27A H 0.0244 0.6508 0.7144 0.139 Uiso 1 1 calc R . .
H27B H 0.0182 0.5778 0.6863 0.139 Uiso 1 1 calc R . .
H27C H -0.0123 0.6343 0.6210 0.139 Uiso 1 1 calc R . .
C28A C 0.1099(8) 0.7012(5) 0.6763(9) 0.056(4) Uiso 0.50 1 d PD D 1
H28A H 0.0923 0.7081 0.6197 0.084 Uiso 0.50 1 calc PR D 1
H28B H 0.1596 0.7064 0.7104 0.084 Uiso 0.50 1 calc PR D 1
H28C H 0.0895 0.7327 0.6921 0.084 Uiso 0.50 1 calc PR D 1
C28B C 0.0910(9) 0.6904(6) 0.6469(9) 0.062(5) Uiso 0.50 1 d PD D 2
H28D H 0.0470 0.6955 0.5942 0.093 Uiso 0.50 1 calc PR D 2
H28E H 0.1276 0.6881 0.6394 0.093 Uiso 0.50 1 calc PR D 2
H28F H 0.0988 0.7272 0.6813 0.093 Uiso 0.50 1 calc PR D 2
C29 C 0.1989(3) 0.6592(3) 0.8668(4) 0.0591(17) Uani 1 1 d D . .
H29 H 0.2434 0.6463 0.9176 0.071 Uiso 1 1 calc R D 1
C30A C 0.1466(6) 0.6782(6) 0.8853(8) 0.047(3) Uiso 0.50 1 d PD D 1
H30A H 0.1693 0.7051 0.9338 0.070 Uiso 0.50 1 calc PR D 1
H30B H 0.1289 0.6393 0.8941 0.070 Uiso 0.50 1 calc PR D 1
H30C H 0.1088 0.7022 0.8395 0.070 Uiso 0.50 1 calc PR D 1
C30B C 0.1581(7) 0.6568(7) 0.9079(8) 0.060(4) Uiso 0.50 1 d PD D 2
H30D H 0.1777 0.6884 0.9516 0.090 Uiso 0.50 1 calc PR D 2
H30E H 0.1621 0.6138 0.9297 0.090 Uiso 0.50 1 calc PR D 2
H30F H 0.1098 0.6668 0.8672 0.090 Uiso 0.50 1 calc PR D 2
C31A C 0.2070(8) 0.7290(6) 0.8332(10) 0.065(5) Uiso 0.50 1 d P D 1
H31A H 0.2372 0.7574 0.8791 0.098 Uiso 0.50 1 calc PR D 1
H31B H 0.1621 0.7491 0.7976 0.098 Uiso 0.50 1 calc PR D 1
H31C H 0.2266 0.7215 0.8030 0.098 Uiso 0.50 1 calc PR D 1
C31B C 0.2296(8) 0.7256(5) 0.8681(10) 0.074(5) Uiso 0.50 1 d PD D 2
H31D H 0.1927 0.7568 0.8369 0.112 Uiso 0.50 1 calc PR D 2
H31E H 0.2549 0.7212 0.8442 0.112 Uiso 0.50 1 calc PR D 2
H31F H 0.2606 0.7405 0.9240 0.112 Uiso 0.50 1 calc PR D 2
C32 C 0.3366(2) 0.6179(2) 0.8769(3) 0.0288(11) Uani 1 1 d . . .
C33 C 0.3671(2) 0.6032(2) 0.9601(3) 0.0307(12) Uani 1 1 d . . .
H33 H 0.3556 0.5637 0.9727 0.037 Uiso 1 1 calc R . .
C34 C 0.4128(3) 0.6443(3) 1.0234(3) 0.0404(13) Uani 1 1 d . . .
H34 H 0.4304 0.6330 1.0774 0.049 Uiso 1 1 calc R . .
C35 C 0.4327(4) 0.7016(3) 1.0078(4) 0.084(3) Uani 1 1 d . E .
H35 H 0.4625 0.7303 1.0504 0.100 Uiso 1 1 calc R . .
C36 C 0.4082(4) 0.7155(3) 0.9298(4) 0.093(3) Uani 1 1 d D . .
C37A C 0.4392(4) 0.7688(4) 0.9038(5) 0.050(2) Uiso 0.70 1 d PD E 1
H37A H 0.4807 0.7881 0.9519 0.060 Uiso 0.70 1 calc PR E 1
H37B H 0.4511 0.7500 0.8688 0.060 Uiso 0.70 1 calc PR E 1
C38A C 0.3821(4) 0.8198(4) 0.8571(5) 0.062(3) Uiso 0.70 1 d PD E 1
H38A H 0.3454 0.8025 0.8043 0.093 Uiso 0.70 1 calc PR E 1
H38B H 0.4010 0.8584 0.8495 0.093 Uiso 0.70 1 calc PR E 1
H38C H 0.3639 0.8306 0.8879 0.093 Uiso 0.70 1 calc PR E 1
C37B C 0.3874(8) 0.7897(6) 0.8993(12) 0.059(6) Uiso 0.30 1 d PD E 2
H37C H 0.3494 0.7907 0.8411 0.071 Uiso 0.30 1 calc PR E 2
H37D H 0.3721 0.8115 0.9295 0.071 Uiso 0.30 1 calc PR E 2
C38B C 0.4513(9) 0.8252(7) 0.9141(12) 0.060(6) Uiso 0.30 1 d PD E 2
H38D H 0.4849 0.7934 0.9226 0.091 Uiso 0.30 1 calc PR E 2
H38E H 0.4717 0.8526 0.9619 0.091 Uiso 0.30 1 calc PR E 2
H38F H 0.4371 0.8517 0.8670 0.091 Uiso 0.30 1 calc PR E 2
N N 0.3593(3) 0.6761(2) 0.8684(3) 0.0615(18) Uani 1 1 d . E .
H1 H 0.341(2) 0.687(2) 0.824(3) 0.030(15) Uiso 1 1 d . . .
B1A B 0.5000 0.8026(3) 0.7500 0.0340(19) Uiso 1 2 d SD . .
F1A F 0.4646(4) 0.8476(4) 0.6863(4) 0.040(2) Uiso 0.50 1 d PD F 1
F2A F 0.4572(4) 0.7547(4) 0.7437(5) 0.056(2) Uiso 0.50 1 d PD F 1
F1B F 0.4702(5) 0.8333(4) 0.6756(4) 0.061(3) Uiso 0.50 1 d PD F 2
F2B F 0.4466(4) 0.7742(4) 0.7519(5) 0.055(2) Uiso 0.50 1 d PD F 2
B1B B 0.0000 0.8168(4) 0.7500 0.049(2) Uiso 1 2 d SD . .
F3A F -0.0143(4) 0.7728(3) 0.6920(4) 0.0582(18) Uiso 0.50 1 d PD . .
F4A F 0.0080(5) 0.8796(3) 0.7325(5) 0.092(3) Uiso 0.50 1 d PD . .
F3B F 0.0331(3) 0.8122(3) 0.7138(3) 0.0474(16) Uiso 0.50 1 d PD . .
F4B F -0.0731(3) 0.8009(4) 0.6828(4) 0.098(3) Uiso 0.50 1 d PD . .
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'
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'
F F 0.0171 0.0103 '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'
Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
C1 Os C32 158.11(17) . .
C1 Os O 75.49(14) . .
C32 Os O 82.69(15) . .
C1 Os P1 94.58(13) . .
C32 Os P1 90.24(13) . .
O Os P1 98.15(9) . .
C1 Os P2 90.41(13) . .
C32 Os P2 90.84(13) . .
O Os P2 98.03(9) . .
P1 Os P2 163.79(4) . .
C1 Os H01 73.7(19) . .
C32 Os H01 128.0(18) . .
O Os H01 149.2(19) . .
P1 Os H01 86.2(19) . .
P2 Os H01 80.4(19) . .
C1 Os H02 134(2) . .
C32 Os H02 67(2) . .
O Os H02 150(2) . .
P1 Os H02 86(2) . .
P2 Os H02 79(2) . .
H01 Os H02 61(2) . .
C20 P1 C14 102.8(2) . .
C20 P1 C17 102.0(3) . .
C14 P1 C17 102.1(2) . .
C20 P1 Os 121.4(2) . .
C14 P1 Os 112.18(16) . .
C17 P1 Os 114.03(16) . .
C29 P2 C23 101.3(3) . .
C29 P2 C26 109.1(3) . .
C23 P2 C26 102.5(3) . .
C29 P2 Os 115.40(18) . .
C23 P2 Os 112.66(18) . .
C26 P2 Os 114.4(2) . .
C7 O Os 119.1(3) . .
C2 C1 C6 113.8(4) . .
C2 C1 Os 130.7(3) . .
C6 C1 Os 115.5(3) . .
C3 C2 C1 123.0(5) . .
C3 C2 H2 118.5 . .
C1 C2 H2 118.5 . .
C2 C3 C4 121.0(5) . .
C2 C3 H3 119.5 . .
C4 C3 H3 119.5 . .
C5 C4 C3 119.3(5) . .
C5 C4 H4 120.3 . .
C3 C4 H4 120.3 . .
C4 C5 C6 120.0(5) . .
C4 C5 H5 120.0 . .
C6 C5 H5 120.0 . .
C5 C6 C7 124.0(4) . .
C5 C6 C1 122.7(4) . .
C7 C6 C1 113.2(4) . .
O C7 C6 116.5(4) . .
O C7 C8 116.6(4) . .
C6 C7 C8 126.9(4) . .
C9 C8 C13 119.1(4) . .
C9 C8 C7 118.3(4) . .
C13 C8 C7 122.6(4) . .
C10 C9 C8 121.0(5) . .
C10 C9 H9 119.5 . .
C8 C9 H9 119.5 . .
C9 C10 C11 119.3(5) . .
C9 C10 H10 120.3 . .
C11 C10 H10 120.3 . .
C12 C11 C10 120.4(5) . .
C12 C11 H11 119.8 . .
C10 C11 H11 119.8 . .
C11 C12 C13 120.2(5) . .
C11 C12 H12 119.9 . .
C13 C12 H12 119.9 . .
C12 C13 C8 120.0(5) . .
C12 C13 H13 120.0 . .
C8 C13 H13 120.0 . .
C15 C14 C16 108.8(4) . .
C15 C14 P1 113.4(3) . .
C16 C14 P1 113.8(3) . .
C15 C14 H14 106.8 . .
C16 C14 H14 106.8 . .
P1 C14 H14 106.8 . .
C14 C15 H15A 109.5 . .
C14 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
C14 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
C14 C16 H16A 109.5 . .
C14 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C14 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
C19 C17 C18 108.1(4) . .
C19 C17 P1 113.5(3) . .
C18 C17 P1 116.7(4) . .
C19 C17 H17 105.9 . .
C18 C17 H17 105.9 . .
P1 C17 H17 105.9 . .
C17 C18 H18A 109.5 . .
C17 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
C17 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
C17 C19 H19A 109.5 . .
C17 C19 H19B 109.5 . .
H19A C19 H19B 109.5 . .
C17 C19 H19C 109.5 . .
H19A C19 H19C 109.5 . .
H19B C19 H19C 109.5 . .
C21 C20 C22B 118.7(9) . .
C21 C20 C22A 112.5(5) . .
C22B C20 C22A 32.7(8) . .
C21 C20 P1 114.8(4) . .
C22B C20 P1 126.4(9) . .
C22A C20 P1 119.4(5) . .
C21 C20 H20 102.3 . .
C22B C20 H20 69.6 . .
C22A C20 H20 102.3 . .
P1 C20 H20 102.3 . .
C20 C21 H21A 109.5 . .
C20 C21 H21B 109.5 . .
H21A C21 H21B 109.5 . .
C20 C21 H21C 109.5 . .
H21A C21 H21C 109.5 . .
H21B C21 H21C 109.5 . .
C20 C22A H22A 109.5 . .
C20 C22A H22B 109.5 . .
C20 C22A H22C 109.5 . .
C20 C22B H22D 109.5 . .
C20 C22B H22E 109.5 . .
H22D C22B H22E 109.5 . .
C20 C22B H22F 109.5 . .
H22D C22B H22F 109.5 . .
H22E C22B H22F 109.5 . .
C24 C23 C25 110.4(5) . .
C24 C23 P2 112.4(4) . .
C25 C23 P2 113.5(4) . .
C24 C23 H23 106.7 . .
C25 C23 H23 106.7 . .
P2 C23 H23 106.7 . .
C23 C24 H24A 109.5 . .
C23 C24 H24B 109.5 . .
H24A C24 H24B 109.5 . .
C23 C24 H24C 109.5 . .
H24A C24 H24C 109.5 . .
H24B C24 H24C 109.5 . .
C23 C25 H25A 109.5 . .
C23 C25 H25B 109.5 . .
H25A C25 H25B 109.5 . .
C23 C25 H25C 109.5 . .
H25A C25 H25C 109.5 . .
H25B C25 H25C 109.5 . .
C27 C26 C28B 109.5(8) . .
C27 C26 C28A 115.1(8) . .
C28B C26 C28A 19.3(8) . .
C27 C26 P2 120.3(5) . .
C28B C26 P2 119.6(8) . .
C28A C26 P2 103.2(6) . .
C27 C26 H26 105.7 . .
C28B C26 H26 90.4 . .
C28A C26 H26 105.7 . .
P2 C26 H26 105.7 . .
C26 C27 H27A 109.5 . .
C26 C27 H27B 109.5 . .
H27A C27 H27B 109.5 . .
C26 C27 H27C 109.5 . .
H27A C27 H27C 109.5 . .
H27B C27 H27C 109.5 . .
C26 C28A H28A 109.5 . .
C26 C28A H28B 109.5 . .
C26 C28A H28C 109.5 . .
C26 C28B H28D 109.5 . .
C26 C28B H28E 109.5 . .
H28D C28B H28E 109.5 . .
C26 C28B H28F 109.5 . .
H28D C28B H28F 109.5 . .
H28E C28B H28F 109.5 . .
C30A C29 C31B 102.3(9) . .
C30A C29 C30B 21.0(7) . .
C31B C29 C30B 116.3(9) . .
C30A C29 C31A 100.5(8) . .
C31B C29 C31A 21.0(9) . .
C30B C29 C31A 119.4(9) . .
C30A C29 P2 118.4(6) . .
C31B C29 P2 121.3(7) . .
C30B C29 P2 116.2(6) . .
C31A C29 P2 106.1(6) . .
C30A C29 H29 110.4 . .
C31B C29 H29 90.5 . .
C30B C29 H29 93.7 . .
C31A C29 H29 110.4 . .
P2 C29 H29 110.4 . .
C29 C30A H30A 109.5 . .
C29 C30A H30B 109.5 . .
C29 C30A H30C 109.5 . .
C29 C30B H30D 109.5 . .
C29 C30B H30E 109.5 . .
H30D C30B H30E 109.5 . .
C29 C30B H30F 109.5 . .
H30D C30B H30F 109.5 . .
H30E C30B H30F 109.5 . .
C29 C31A H31A 109.5 . .
C29 C31A H31B 109.5 . .
C29 C31A H31C 109.5 . .
C29 C31B H31D 109.5 . .
C29 C31B H31E 109.5 . .
H31D C31B H31E 109.5 . .
C29 C31B H31F 109.5 . .
H31D C31B H31F 109.5 . .
H31E C31B H31F 109.5 . .
N C32 C33 111.6(4) . .
N C32 Os 118.5(3) . .
C33 C32 Os 129.9(4) . .
C34 C33 C32 123.1(5) . .
C34 C33 H33 118.5 . .
C32 C33 H33 118.5 . .
C35 C34 C33 120.4(5) . .
C35 C34 H34 119.8 . .
C33 C34 H34 119.8 . .
C36 C35 C34 118.4(5) . .
C36 C35 H35 120.8 . .
C34 C35 H35 120.8 . .
C35 C36 N 119.4(5) . .
C35 C36 C37A 124.5(6) . .
N C36 C37A 115.5(6) . .
C35 C36 C37B 118.2(10) . .
N C36 C37B 107.8(8) . .
C37A C36 C37B 46.5(6) . .
C38A C37A C36 105.1(6) . .
C38A C37A H37A 110.7 . .
C36 C37A H37A 110.7 . .
C38A C37A H37B 110.7 . .
C36 C37A H37B 110.7 . .
H37A C37A H37B 108.8 . .
C38B C37B C36 108.9(8) . .
C38B C37B H37C 109.9 . .
C36 C37B H37C 109.9 . .
C38B C37B H37D 109.9 . .
C36 C37B H37D 109.9 . .
H37C C37B H37D 108.3 . .
C37B C38B H38D 109.5 . .
C37B C38B H38E 109.5 . .
H38D C38B H38E 109.5 . .
C37B C38B H38F 109.5 . .
H38D C38B H38F 109.5 . .
H38E C38B H38F 109.5 . .
C32 N C36 126.7(5) . .
C32 N H1 114(4) . .
C36 N H1 120(4) . .
F2A B1A F2A 87.9(8) . 2_656
F2A B1A F1B 108.3(5) . 2_656
F2A B1A F1B 110.1(5) 2_656 2_656
F2A B1A F1B 110.1(5) . .
F2A B1A F1B 108.3(5) 2_656 .
F1B B1A F1B 125.6(10) 2_656 .
F2A B1A F1A 125.5(5) . 2_656
F2A B1A F1A 111.9(5) 2_656 2_656
F1B B1A F1A 17.7(5) 2_656 2_656
F1B B1A F1A 110.3(6) . 2_656
F2A B1A F1A 111.9(5) . .
F2A B1A F1A 125.5(5) 2_656 .
F1B B1A F1A 110.3(6) 2_656 .
F1B B1A F1A 17.7(5) . .
F1A B1A F1A 97.1(8) 2_656 .
F2A B1A F2B 109.3(7) . 2_656
F2A B1A F2B 22.6(4) 2_656 2_656
F1B B1A F2B 108.3(5) 2_656 2_656
F1B B1A F2B 93.6(5) . 2_656
F1A B1A F2B 103.1(5) 2_656 2_656
F1A B1A F2B 108.6(5) . 2_656
F2A B1A F2B 22.6(4) . .
F2A B1A F2B 109.3(7) 2_656 .
F1B B1A F2B 93.6(5) 2_656 .
F1B B1A F2B 108.3(5) . .
F1A B1A F2B 108.6(5) 2_656 .
F1A B1A F2B 103.1(5) . .
F2B B1A F2B 131.3(9) 2_656 .
F3B B1B F3B 171.9(8) . 2_556
F3B B1B F3A 54.7(3) . .
F3B B1B F3A 119.0(6) 2_556 .
F3B B1B F3A 119.0(6) . 2_556
F3B B1B F3A 54.7(3) 2_556 2_556
F3A B1B F3A 96.2(7) . 2_556
F3B B1B F4A 114.4(6) . 2_556
F3B B1B F4A 73.6(4) 2_556 2_556
F3A B1B F4A 147.3(6) . 2_556
F3A B1B F4A 114.1(4) 2_556 2_556
F3B B1B F4A 73.6(4) . .
F3B B1B F4A 114.4(6) 2_556 .
F3A B1B F4A 114.1(4) . .
F3A B1B F4A 147.3(6) 2_556 .
F4A B1B F4A 41.4(6) 2_556 .
F3B B1B F4B 103.6(4) . .
F3B B1B F4B 74.6(4) 2_556 .
F3A B1B F4B 59.8(4) . .
F3A B1B F4B 102.1(6) 2_556 .
F4A B1B F4B 100.1(6) 2_556 .
F4A B1B F4B 103.6(6) . .
F3B B1B F4B 74.6(4) . 2_556
F3B B1B F4B 103.6(4) 2_556 2_556
F3A B1B F4B 102.1(6) . 2_556
F3A B1B F4B 59.8(4) 2_556 2_556
F4A B1B F4B 103.6(6) 2_556 2_556
F4A B1B F4B 100.1(6) . 2_556
F4B B1B F4B 154.6(9) . 2_556
F3B F3A B1B 62.5(3) . .
F3B F3A F4B 113.8(6) . .
B1B F3A F4B 64.9(4) . .
F4A F4A B1B 69.3(3) 2_556 .
F4A F4A F3B 120.8(4) 2_556 .
B1B F4A F3B 52.3(3) . .
F3A F3B B1B 62.8(4) . .
F3A F3B F4A 104.9(5) . .
B1B F3B F4A 54.0(4) . .
F3A F3B F4B 95.1(5) . 2_556
B1B F3B F4B 56.4(3) . 2_556
F4A F3B F4B 81.8(5) . 2_556
F3A F4B B1B 55.3(3) . .
F3A F4B F3B 95.0(5) . 2_556
B1B F4B F3B 49.0(3) . 2_556
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Os C1 2.084(4) .
Os C32 2.110(5) .
Os O 2.127(3) .
Os P1 2.3812(13) .
Os P2 2.3870(14) .
Os H01 1.582(10) .
Os H02 1.576(10) .
P1 C20 1.850(5) .
P1 C14 1.859(4) .
P1 C17 1.860(5) .
P2 C29 1.841(6) .
P2 C23 1.846(5) .
P2 C26 1.866(6) .
O C7 1.267(5) .
C1 C2 1.412(6) .
C1 C6 1.440(6) .
C2 C3 1.378(6) .
C2 H2 0.9300 .
C3 C4 1.387(7) .
C3 H3 0.9300 .
C4 C5 1.371(6) .
C4 H4 0.9300 .
C5 C6 1.396(6) .
C5 H5 0.9300 .
C6 C7 1.438(6) .
C7 C8 1.480(6) .
C8 C9 1.386(6) .
C8 C13 1.390(6) .
C9 C10 1.373(6) .
C9 H9 0.9300 .
C10 C11 1.390(7) .
C10 H10 0.9300 .
C11 C12 1.369(7) .
C11 H11 0.9300 .
C12 C13 1.383(6) .
C12 H12 0.9300 .
C13 H13 0.9300 .
C14 C15 1.525(6) .
C14 C16 1.526(6) .
C14 H14 0.9800 .
C15 H15A 0.9600 .
C15 H15B 0.9600 .
C15 H15C 0.9600 .
C16 H16A 0.9600 .
C16 H16B 0.9600 .
C16 H16C 0.9600 .
C17 C19 1.523(6) .
C17 C18 1.528(6) .
C17 H17 0.9800 .
C18 H18A 0.9600 .
C18 H18B 0.9600 .
C18 H18C 0.9600 .
C19 H19A 0.9600 .
C19 H19B 0.9600 .
C19 H19C 0.9600 .
C20 C21 1.493(7) .
C20 C22B 1.493(9) .
C20 C22A 1.493(7) .
C20 H20 0.9800 .
C21 H21A 0.9600 .
C21 H21B 0.9600 .
C21 H21C 0.9600 .
C22A H22A 0.9600 .
C22A H22B 0.9600 .
C22A H22C 0.9600 .
C22B H22D 0.9600 .
C22B H22E 0.9600 .
C22B H22F 0.9600 .
C23 C24 1.528(7) .
C23 C25 1.528(7) .
C23 H23 0.9800 .
C24 H24A 0.9600 .
C24 H24B 0.9600 .
C24 H24C 0.9600 .
C25 H25A 0.9600 .
C25 H25B 0.9600 .
C25 H25C 0.9600 .
C26 C27 1.433(8) .
C26 C28B 1.515(9) .
C26 C28A 1.619(9) .
C26 H26 0.9800 .
C27 H27A 0.9600 .
C27 H27B 0.9600 .
C27 H27C 0.9600 .
C28A H28A 0.9600 .
C28A H28B 0.9600 .
C28A H28C 0.9600 .
C28B H28D 0.9600 .
C28B H28E 0.9600 .
C28B H28F 0.9600 .
C29 C30A 1.529(8) .
C29 C31B 1.530(7) .
C29 C30B 1.587(8) .
C29 C31A 1.631(14) .
C29 H29 0.9800 .
C30A H30A 0.9600 .
C30A H30B 0.9600 .
C30A H30C 0.9600 .
C30B H30D 0.9600 .
C30B H30E 0.9600 .
C30B H30F 0.9600 .
C31A H31A 0.9600 .
C31A H31B 0.9600 .
C31A H31C 0.9600 .
C31B H31D 0.9600 .
C31B H31E 0.9600 .
C31B H31F 0.9600 .
C32 N 1.353(6) .
C32 C33 1.404(6) .
C33 C34 1.371(6) .
C33 H33 0.9300 .
C34 C35 1.360(7) .
C34 H34 0.9300 .
C35 C36 1.338(7) .
C35 H35 0.9300 .
C36 N 1.353(7) .
C36 C37A 1.559(7) .
C36 C37B 1.599(9) .
C37A C38A 1.518(7) .
C37A H37A 0.9700 .
C37A H37B 0.9700 .
C38A H38A 0.9600 .
C38A H38B 0.9600 .
C38A H38C 0.9600 .
C37B C38B 1.538(10) .
C37B H37C 0.9700 .
C37B H37D 0.9700 .
C38B H38D 0.9600 .
C38B H38E 0.9600 .
C38B H38F 0.9600 .
N H1 0.76(4) .
B1A F2A 1.358(7) .
B1A F2A 1.358(7) 2_656
B1A F1B 1.369(7) 2_656
B1A F1B 1.369(7) .
B1A F1A 1.386(7) 2_656
B1A F1A 1.386(7) .
B1A F2B 1.407(7) 2_656
B1A F2B 1.407(7) .
B1B F3B 1.339(5) .
B1B F3B 1.339(5) 2_556
B1B F3A 1.343(6) .
B1B F3A 1.343(6) 2_556
B1B F4A 1.370(7) 2_556
B1B F4A 1.370(7) .
B1B F4B 1.479(6) .
B1B F4B 1.479(6) 2_556
F3A F3B 1.231(7) .
F3A F4B 1.411(9) .
F4A F4A 0.969(14) 2_556
F4A F3B 1.623(8) .
F3B F4B 1.712(9) 2_556
F4B F3B 1.712(9) 2_556
