#------------------------------------------------------------------------------
#$Date: 2017-03-05 20:59:09 +0100 (dom 05 de mar de 2017) $
#$Revision: 193981 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/74/7027468.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_7027468
loop_
_publ_author_name
'Lehtonen, Ari'
'Jokela, Jukka'
'Edwards, Peter G.'
'Sillanpää, Reijo'
_publ_section_title
;
 Preparation and crystal structures of oxoosmium(VI) diolato complexes
;
_journal_issue                   16
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2785
_journal_paper_doi               10.1039/a903042e
_journal_year                    1999
_chemical_formula_sum            'C54 H77 O8 Os P'
_chemical_formula_weight         1075.33
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                107.08(4)
_cell_angle_beta                 96.18(3)
_cell_angle_gamma                112.90(3)
_cell_formula_units_Z            2
_cell_length_a                   15.055(5)
_cell_length_b                   15.899(8)
_cell_length_c                   12.677(5)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      6.9
_cell_measurement_theta_min      5.9
_cell_volume                     2586(2)
_computing_cell_refinement
;
MSC/AFC5S Control Program (Molecular Structure Corporation, 1995)
;
_computing_data_collection
; 
MSC/AFC Control Program (Molecular Structure Corporation, 1995)
;
_computing_data_reduction
;
TEXSAN for WINDOWS(Molecular Structure Corporation, 1997)
;
_computing_molecular_graphics    'ORTEP-3 for WINDOWS (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Altomare, 1994)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku AFC5S'
_diffrn_measurement_method       ω--2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_sigmaI/netI    0.0661
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9491
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.59
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.548
_exptl_absorpt_correction_T_max  0.7011
_exptl_absorpt_correction_T_min  0.5683
_exptl_absorpt_correction_type
;
empirical via \y scans (North, Phillips & Mathews, 1968)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.817
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     585
_refine_ls_number_reflns         9113
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0287P)²+0.2500P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0697
_refine_ls_wR_factor_ref         0.0768
_reflns_number_gt                7148
_reflns_number_total             9113
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            903042esup1.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0287P)^2^+0.2500P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0287P)^2^+0.2500P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

The following automatic conversions were performed:
data name '_gmom_hbond_distance_dh' replaced with
'_geom_hbond_distance_DH' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 5005 2017-03-03 11:38:54Z antanas 
;
_cod_original_cell_volume        2585.4(19)
_cod_database_code               7027468
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_refinement_flags
Os Os 0.761757(15) 0.603246(14) 0.786013(18) 0.03769(7) Uani 1 d .
P P 0.53653(10) 0.79586(9) 0.23360(11) 0.0448(3) Uani 1 d .
O1 O 0.6379(3) 0.5428(2) 0.7595(3) 0.0562(10) Uani 1 d .
O2 O 0.7973(2) 0.7325(2) 0.7930(3) 0.0392(8) Uani 1 d .
O3 O 0.8197(2) 0.6684(2) 0.9455(3) 0.0459(8) Uani 1 d .
O4 O 0.8250(2) 0.5233(2) 0.8022(3) 0.0417(8) Uani 1 d .
O5 O 0.7977(2) 0.5826(2) 0.6455(3) 0.0415(8) Uani 1 d .
O6 O 0.7065(3) 1.0135(3) 0.1091(3) 0.0589(11) Uani 1 d .
O7 O 0.7702(4) 1.0524(3) 0.3507(4) 0.0738(14) Uani 1 d .
O8 O 0.6084(3) 0.8696(2) 0.1964(3) 0.0602(10) Uani 1 d .
C1 C 0.7992(4) 0.7978(3) 0.9040(4) 0.0433(12) Uani 1 d .
C2 C 0.6910(4) 0.7737(4) 0.9083(5) 0.0534(14) Uani 1 d .
H2A H 0.6580 0.7073 0.9069 0.080 Uiso 1 calc R
H2B H 0.6907 0.8177 0.9798 0.080 Uiso 1 calc R
C3 C 0.6326(4) 0.7825(4) 0.8110(5) 0.0682(17) Uani 1 d .
H3A H 0.5652 0.7672 0.8187 0.102 Uiso 1 calc R
H3B H 0.6290 0.7359 0.7393 0.102 Uiso 1 calc R
C4 C 0.6825(5) 0.8868(5) 0.8107(6) 0.0770(19) Uani 1 d .
H4A H 0.6477 0.8901 0.7442 0.115 Uiso 1 calc R
H4B H 0.6787 0.9325 0.8781 0.115 Uiso 1 calc R
C5 C 0.7917(5) 0.9154(4) 0.8089(5) 0.0637(16) Uani 1 d .
H5A H 0.7942 0.8760 0.7357 0.096 Uiso 1 calc R
H5B H 0.8233 0.9836 0.8160 0.096 Uiso 1 calc R
C6 C 0.8511(4) 0.9023(3) 0.9033(5) 0.0535(14) Uani 1 d .
H6A H 0.8585 0.9495 0.9765 0.080 Uiso 1 calc R
H6B H 0.9172 0.9151 0.8920 0.080 Uiso 1 calc R
C7 C 0.8551(4) 0.7745(3) 0.9927(4) 0.0418(12) Uani 1 d .
C8 C 0.9679(4) 0.8201(4) 1.0069(4) 0.0537(14) Uani 1 d .
H8A H 0.9816 0.7986 0.9332 0.081 Uiso 1 calc R
H8B H 0.9939 0.8910 1.0340 0.081 Uiso 1 calc R
C9 C 1.0216(4) 0.7927(4) 1.0898(5) 0.0639(16) Uani 1 d .
H9A H 1.0928 0.8256 1.0983 0.096 Uiso 1 calc R
H9B H 1.0006 0.7225 1.0597 0.096 Uiso 1 calc R
C10 C 0.9990(5) 0.8224(5) 1.2075(5) 0.0772(19) Uani 1 d .
H10A H 1.0317 0.8021 1.2583 0.116 Uiso 1 calc R
H10B H 1.0246 0.8932 1.2405 0.116 Uiso 1 calc R
C11 C 0.8874(5) 0.7743(5) 1.1945(5) 0.0719(18) Uani 1 d .
H11A H 0.8739 0.7961 1.2683 0.108 Uiso 1 calc R
H11B H 0.8636 0.7038 1.1689 0.108 Uiso 1 calc R
C12 C 0.8305(5) 0.7987(4) 1.1096(4) 0.0593(15) Uani 1 d .
H12A H 0.8470 0.8679 1.1407 0.089 Uiso 1 calc R
H12B H 0.7595 0.7618 1.0994 0.089 Uiso 1 calc R
C13 C 0.8633(4) 0.4854(3) 0.7061(4) 0.0413(12) Uani 1 d .
C14 C 0.9761(4) 0.5522(4) 0.7397(4) 0.0494(13) Uani 1 d .
H14A H 1.0041 0.5310 0.6774 0.074 Uiso 1 calc R
H14B H 0.9869 0.6188 0.7510 0.074 Uiso 1 calc R
C15 C 1.0309(4) 0.5518(4) 0.8478(5) 0.0616(15) Uani 1 d .
H15A H 1.0080 0.5793 0.9120 0.092 Uiso 1 calc R
H15B H 1.1017 0.5927 0.8625 0.092 Uiso 1 calc R
C16 C 1.0129(4) 0.4475(4) 0.8362(5) 0.0666(17) Uani 1 d .
H16A H 1.0414 0.4220 0.7767 0.100 Uiso 1 calc R
H16B H 1.0452 0.4484 0.9072 0.100 Uiso 1 calc R
C17 C 0.9014(4) 0.3816(4) 0.8067(5) 0.0574(15) Uani 1 d .
H17A H 0.8750 0.4035 0.8702 0.086 Uiso 1 calc R
H17B H 0.8907 0.3150 0.7956 0.086 Uiso 1 calc R
C18 C 0.8449(4) 0.3817(3) 0.6994(4) 0.0478(13) Uani 1 d .
H18A H 0.7741 0.3424 0.6876 0.072 Uiso 1 calc R
H18B H 0.8650 0.3516 0.6341 0.072 Uiso 1 calc R
C19 C 0.8067(4) 0.4898(3) 0.6018(4) 0.0429(12) Uani 1 d .
C20 C 0.7004(4) 0.4052(4) 0.5506(4) 0.0545(14) Uani 1 d .
H20A H 0.7046 0.3438 0.5197 0.082 Uiso 1 calc R
H20B H 0.6660 0.4018 0.6108 0.082 Uiso 1 calc R
C21 C 0.6924(6) 0.4234(5) 0.3615(5) 0.093(2) Uani 1 d .
H21A H 0.6554 0.4356 0.3050 0.140 Uiso 1 calc R
H21B H 0.6938 0.3613 0.3247 0.140 Uiso 1 calc R
C22 C 0.6401(5) 0.4172(4) 0.4573(5) 0.0741(19) Uani 1 d .
H22A H 0.6318 0.4763 0.4885 0.111 Uiso 1 calc R
H22B H 0.5745 0.3617 0.4273 0.111 Uiso 1 calc R
C23 C 0.7990(5) 0.5055(5) 0.4072(5) 0.0748(19) Uani 1 d .
H23A H 0.8325 0.5031 0.3459 0.112 Uiso 1 calc R
H23B H 0.7968 0.5683 0.4325 0.112 Uiso 1 calc R
C24 C 0.8590(5) 0.4981(4) 0.5059(4) 0.0600(15) Uani 1 d .
H24A H 0.9229 0.5558 0.5366 0.090 Uiso 1 calc R
H24B H 0.8714 0.4412 0.4773 0.090 Uiso 1 calc R
C25 C 0.7429(4) 1.1095(3) 0.1965(4) 0.0448(12) Uani 1 d .
C26 C 0.6552(4) 1.1233(4) 0.2368(4) 0.0647(16) Uani 1 d .
H26A H 0.6236 1.0747 0.2695 0.097 Uiso 1 calc R
H26B H 0.6803 1.1877 0.2961 0.097 Uiso 1 calc R
C27 C 0.5786(5) 1.1140(6) 0.1417(6) 0.098(3) Uani 1 d .
H27A H 0.5275 1.1279 0.1726 0.147 Uiso 1 calc R
H27B H 0.5471 1.0470 0.0870 0.147 Uiso 1 calc R
C28 C 0.6245(7) 1.1835(6) 0.0814(6) 0.104(3) Uani 1 d .
H28A H 0.6477 1.2505 0.1334 0.155 Uiso 1 calc R
H28B H 0.5739 1.1714 0.0171 0.155 Uiso 1 calc R
C29 C 0.7112(6) 1.1713(5) 0.0391(5) 0.080(2) Uani 1 d .
H29A H 0.7423 1.2211 0.0077 0.121 Uiso 1 calc R
H29B H 0.6864 1.1075 -0.0213 0.121 Uiso 1 calc R
C30 C 0.7887(5) 1.1802(4) 0.1355(5) 0.0641(16) Uani 1 d .
H30A H 0.8201 1.2470 0.1905 0.096 Uiso 1 calc R
H30B H 0.8399 1.1667 0.1045 0.096 Uiso 1 calc R
C31 C 0.8203(4) 1.1186(3) 0.2961(4) 0.0442(12) Uani 1 d .
C32 C 0.9032(5) 1.0954(5) 0.2540(5) 0.0710(18) Uani 1 d .
H32A H 0.8736 1.0307 0.1945 0.107 Uiso 1 calc R
H32B H 0.9394 1.1427 0.2216 0.107 Uiso 1 calc R
C33 C 0.9757(6) 1.0986(6) 0.3504(6) 0.095(2) Uani 1 d .
H33A H 0.9405 1.0490 0.3804 0.143 Uiso 1 calc R
H33B H 1.0271 1.0840 0.3212 0.143 Uiso 1 calc R
C34 C 1.0232(5) 1.1989(5) 0.4451(6) 0.088(2) Uani 1 d .
H34A H 1.0672 1.1989 0.5070 0.132 Uiso 1 calc R
H34B H 1.0629 1.2478 0.4166 0.132 Uiso 1 calc R
C35 C 0.9442(5) 1.2251(5) 0.4893(5) 0.0732(18) Uani 1 d .
H35A H 0.9758 1.2911 0.5462 0.110 Uiso 1 calc R
H35B H 0.9096 1.1805 0.5255 0.110 Uiso 1 calc R
C36 C 0.8688(4) 1.2191(4) 0.3926(4) 0.0538(14) Uani 1 d .
H36A H 0.8174 1.2328 0.4231 0.081 Uiso 1 calc R
H36B H 0.9024 1.2690 0.3623 0.081 Uiso 1 calc R
C37 C 0.5992(4) 0.7616(4) 0.3296(4) 0.0484(13) Uani 1 d .
C38 C 0.6900(4) 0.8313(4) 0.4062(5) 0.0638(16) Uani 1 d .
H38 H 0.7188 0.8938 0.4035 0.096 Uiso 1 calc R
C39 C 0.7376(5) 0.8099(5) 0.4853(5) 0.0744(18) Uani 1 d .
H39 H 0.7982 0.8576 0.5355 0.112 Uiso 1 calc R
C40 C 0.6954(5) 0.7170(5) 0.4904(6) 0.0774(19) Uani 1 d .
H40 H 0.7272 0.7018 0.5440 0.116 Uiso 1 calc R
C41 C 0.6061(5) 0.6477(5) 0.4152(6) 0.084(2) Uani 1 d .
H41 H 0.5775 0.5855 0.4187 0.126 Uiso 1 calc R
C42 C 0.5582(5) 0.6683(4) 0.3352(5) 0.0678(17) Uani 1 d .
H42 H 0.4981 0.6199 0.2845 0.102 Uiso 1 calc R
C43 C 0.4560(4) 0.6845(3) 0.1139(4) 0.0432(12) Uani 1 d .
C44 C 0.4978(5) 0.6512(5) 0.0300(5) 0.082(2) Uani 1 d .
H44 H 0.5653 0.6868 0.0366 0.122 Uiso 1 calc R
C45 C 0.4425(6) 0.5661(6) -0.0639(6) 0.100(3) Uani 1 d .
H45 H 0.4719 0.5454 -0.1206 0.150 Uiso 1 calc R
C46 C 0.3442(5) 0.5127(4) -0.0723(5) 0.0748(19) Uani 1 d .
H46 H 0.3064 0.4548 -0.1348 0.112 Uiso 1 calc R
C47 C 0.3010(4) 0.5434(4) 0.0096(5) 0.0681(17) Uani 1 d .
H47 H 0.2338 0.5066 0.0029 0.102 Uiso 1 calc R
C48 C 0.3564(4) 0.6291(4) 0.1033(5) 0.0593(15) Uani 1 d .
H48 H 0.3264 0.6494 0.1595 0.089 Uiso 1 calc R
C49 C 0.4570(4) 0.8395(4) 0.3061(4) 0.0480(13) Uani 1 d .
C50 C 0.4467(5) 0.8385(4) 0.4129(5) 0.0671(17) Uani 1 d .
H50 H 0.4813 0.8144 0.4511 0.101 Uiso 1 calc R
C51 C 0.3836(6) 0.8742(5) 0.4631(6) 0.083(2) Uani 1 d .
H51 H 0.3758 0.8729 0.5344 0.125 Uiso 1 calc R
C52 C 0.3346(6) 0.9102(5) 0.4090(7) 0.089(2) Uani 1 d .
H52 H 0.2931 0.9337 0.4433 0.134 Uiso 1 calc R
C53 C 0.3447(6) 0.9126(6) 0.3047(8) 0.106(3) Uani 1 d .
H53 H 0.3099 0.9373 0.2676 0.160 Uiso 1 calc R
C54 C 0.4066(6) 0.8785(5) 0.2540(5) 0.084(2) Uani 1 d .
H54 H 0.4145 0.8818 0.1833 0.126 Uiso 1 calc R
H1 H 0.669(4) 0.973(4) 0.131(5) 0.07(2) Uiso 1 d .
H2 H 0.722(4) 1.005(4) 0.300(5) 0.08(2) Uiso 1 d .
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'
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
O1 Os O2 109.39(15) y
O1 Os O5 108.51(17) y
O2 Os O5 85.56(13) y
O1 Os O3 110.56(16) y
O2 Os O3 82.14(14) y
O5 Os O3 140.93(14) y
O1 Os O4 111.86(15) y
O2 Os O4 138.75(14) y
O5 Os O4 82.32(13) y
O3 Os O4 82.95(14) y
O8 P C37 111.6(2) ?
O8 P C43 111.4(2) ?
C37 P C43 106.7(2) ?
O8 P C49 113.0(2) ?
C37 P C49 106.8(2) ?
C43 P C49 107.1(2) ?
C1 O2 Os 112.8(3) y
C7 O3 Os 117.5(3) y
C13 O4 Os 116.9(3) y
C19 O5 Os 113.2(3) y
C25 O6 H1 109(4) ?
C31 O7 H2 106(4) ?
O2 C1 C2 107.6(4) ?
O2 C1 C6 105.3(4) ?
C2 C1 C6 109.1(4) ?
O2 C1 C7 104.4(3) ?
C2 C1 C7 113.7(4) ?
C6 C1 C7 116.0(4) ?
C3 C2 C1 113.4(4) ?
C3 C2 H2A 108.9 ?
C1 C2 H2A 108.9 ?
C3 C2 H2B 108.9 ?
C1 C2 H2B 108.9 ?
H2A C2 H2B 107.7 ?
C2 C3 C4 110.3(5) ?
C2 C3 H3A 109.6 ?
C4 C3 H3A 109.6 ?
C2 C3 H3B 109.6 ?
C4 C3 H3B 109.6 ?
H3A C3 H3B 108.1 ?
C5 C4 C3 110.3(5) ?
C5 C4 H4A 109.6 ?
C3 C4 H4A 109.6 ?
C5 C4 H4B 109.6 ?
C3 C4 H4B 109.6 ?
H4A C4 H4B 108.1 ?
C6 C5 C4 114.0(5) ?
C6 C5 H5A 108.7 ?
C4 C5 H5A 108.7 ?
C6 C5 H5B 108.7 ?
C4 C5 H5B 108.7 ?
H5A C5 H5B 107.6 ?
C5 C6 C1 111.4(4) ?
C5 C6 H6A 109.3 ?
C1 C6 H6A 109.3 ?
C5 C6 H6B 109.3 ?
C1 C6 H6B 109.3 ?
H6A C6 H6B 108.0 ?
O3 C7 C8 106.5(4) ?
O3 C7 C12 106.5(4) ?
C8 C7 C12 110.6(4) ?
O3 C7 C1 105.2(4) ?
C8 C7 C1 113.2(4) ?
C12 C7 C1 114.2(4) ?
C9 C8 C7 112.7(4) ?
C9 C8 H8A 109.0 ?
C7 C8 H8A 109.0 ?
C9 C8 H8B 109.0 ?
C7 C8 H8B 109.0 ?
H8A C8 H8B 107.8 ?
C8 C9 C10 110.8(5) ?
C8 C9 H9A 109.5 ?
C10 C9 H9A 109.5 ?
C8 C9 H9B 109.5 ?
C10 C9 H9B 109.5 ?
H9A C9 H9B 108.1 ?
C11 C10 C9 109.9(5) ?
C11 C10 H10A 109.7 ?
C9 C10 H10A 109.7 ?
C11 C10 H10B 109.7 ?
C9 C10 H10B 109.7 ?
H10A C10 H10B 108.2 ?
C10 C11 C12 112.4(5) ?
C10 C11 H11A 109.1 ?
C12 C11 H11A 109.1 ?
C10 C11 H11B 109.1 ?
C12 C11 H11B 109.1 ?
H11A C11 H11B 107.9 ?
C11 C12 C7 112.4(4) ?
C11 C12 H12A 109.1 ?
C7 C12 H12A 109.1 ?
C11 C12 H12B 109.1 ?
C7 C12 H12B 109.1 ?
H12A C12 H12B 107.9 ?
O4 C13 C19 106.1(4) ?
O4 C13 C18 105.6(4) ?
C19 C13 C18 115.0(4) ?
O4 C13 C14 106.1(4) ?
C19 C13 C14 113.7(4) ?
C18 C13 C14 109.6(4) ?
C15 C14 C13 113.3(4) ?
C15 C14 H14A 108.9 ?
C13 C14 H14A 108.9 ?
C15 C14 H14B 108.9 ?
C13 C14 H14B 108.9 ?
H14A C14 H14B 107.7 ?
C14 C15 C16 111.0(5) ?
C14 C15 H15A 109.4 ?
C16 C15 H15A 109.4 ?
C14 C15 H15B 109.4 ?
C16 C15 H15B 109.4 ?
H15A C15 H15B 108.0 ?
C17 C16 C15 109.7(4) ?
C17 C16 H16A 109.7 ?
C15 C16 H16A 109.7 ?
C17 C16 H16B 109.7 ?
C15 C16 H16B 109.7 ?
H16A C16 H16B 108.2 ?
C16 C17 C18 112.5(5) ?
C16 C17 H17A 109.1 ?
C18 C17 H17A 109.1 ?
C16 C17 H17B 109.1 ?
C18 C17 H17B 109.1 ?
H17A C17 H17B 107.8 ?
C17 C18 C13 112.7(4) ?
C17 C18 H18A 109.0 ?
C13 C18 H18A 109.0 ?
C17 C18 H18B 109.0 ?
C13 C18 H18B 109.0 ?
H18A C18 H18B 107.8 ?
O5 C19 C24 105.0(4) ?
O5 C19 C13 104.7(4) ?
C24 C19 C13 116.6(4) ?
O5 C19 C20 107.7(4) ?
C24 C19 C20 108.9(4) ?
C13 C19 C20 113.2(4) ?
C22 C20 C19 112.9(5) ?
C22 C20 H20A 109.0 ?
C19 C20 H20A 109.0 ?
C22 C20 H20B 109.0 ?
C19 C20 H20B 109.0 ?
H20A C20 H20B 107.8 ?
C22 C21 C23 111.0(5) ?
C22 C21 H21A 109.4 ?
C23 C21 H21A 109.4 ?
C22 C21 H21B 109.4 ?
C23 C21 H21B 109.4 ?
H21A C21 H21B 108.0 ?
C20 C22 C21 110.3(6) ?
C20 C22 H22A 109.6 ?
C21 C22 H22A 109.6 ?
C20 C22 H22B 109.6 ?
C21 C22 H22B 109.6 ?
H22A C22 H22B 108.1 ?
C24 C23 C21 112.8(5) ?
C24 C23 H23A 109.0 ?
C21 C23 H23A 109.0 ?
C24 C23 H23B 109.0 ?
C21 C23 H23B 109.0 ?
H23A C23 H23B 107.8 ?
C23 C24 C19 113.1(5) ?
C23 C24 H24A 109.0 ?
C19 C24 H24A 109.0 ?
C23 C24 H24B 109.0 ?
C19 C24 H24B 109.0 ?
H24A C24 H24B 107.8 ?
O6 C25 C30 103.9(4) ?
O6 C25 C26 109.5(4) ?
C30 C25 C26 109.9(5) ?
O6 C25 C31 108.5(4) ?
C30 C25 C31 113.2(4) ?
C26 C25 C31 111.5(4) ?
C27 C26 C25 112.7(5) ?
C27 C26 H26A 109.1 ?
C25 C26 H26A 109.1 ?
C27 C26 H26B 109.1 ?
C25 C26 H26B 109.1 ?
H26A C26 H26B 107.8 ?
C26 C27 C28 111.8(6) ?
C26 C27 H27A 109.2 ?
C28 C27 H27A 109.2 ?
C26 C27 H27B 109.2 ?
C28 C27 H27B 109.2 ?
H27A C27 H27B 107.9 ?
C27 C28 C29 112.0(6) ?
C27 C28 H28A 109.2 ?
C29 C28 H28A 109.2 ?
C27 C28 H28B 109.2 ?
C29 C28 H28B 109.2 ?
H28A C28 H28B 107.9 ?
C28 C29 C30 111.3(5) ?
C28 C29 H29A 109.4 ?
C30 C29 H29A 109.4 ?
C28 C29 H29B 109.4 ?
C30 C29 H29B 109.4 ?
H29A C29 H29B 108.0 ?
C29 C30 C25 112.4(5) ?
C29 C30 H30A 109.1 ?
C25 C30 H30A 109.1 ?
C29 C30 H30B 109.1 ?
C25 C30 H30B 109.1 ?
H30A C30 H30B 107.9 ?
O7 C31 C36 103.6(4) ?
O7 C31 C32 109.6(4) ?
C36 C31 C32 108.3(4) ?
O7 C31 C25 109.3(4) ?
C36 C31 C25 114.0(4) ?
C32 C31 C25 111.6(4) ?
C33 C32 C31 111.6(5) ?
C33 C32 H32A 109.3 ?
C31 C32 H32A 109.3 ?
C33 C32 H32B 109.3 ?
C31 C32 H32B 109.3 ?
H32A C32 H32B 108.0 ?
C34 C33 C32 110.6(6) ?
C34 C33 H33A 109.5 ?
C32 C33 H33A 109.5 ?
C34 C33 H33B 109.5 ?
C32 C33 H33B 109.5 ?
H33A C33 H33B 108.1 ?
C35 C34 C33 110.6(6) ?
C35 C34 H34A 109.5 ?
C33 C34 H34A 109.5 ?
C35 C34 H34B 109.5 ?
C33 C34 H34B 109.5 ?
H34A C34 H34B 108.1 ?
C34 C35 C36 111.3(5) ?
C34 C35 H35A 109.4 ?
C36 C35 H35A 109.4 ?
C34 C35 H35B 109.4 ?
C36 C35 H35B 109.4 ?
H35A C35 H35B 108.0 ?
C31 C36 C35 112.4(4) ?
C31 C36 H36A 109.1 ?
C35 C36 H36A 109.1 ?
C31 C36 H36B 109.1 ?
C35 C36 H36B 109.1 ?
H36A C36 H36B 107.9 ?
C38 C37 C42 117.9(5) ?
C38 C37 P 119.6(4) ?
C42 C37 P 122.5(4) ?
C39 C38 C37 121.6(6) ?
C39 C38 H38 119.2 ?
C37 C38 H38 119.2 ?
C38 C39 C40 119.9(6) ?
C38 C39 H39 120.1 ?
C40 C39 H39 120.1 ?
C41 C40 C39 119.1(6) ?
C41 C40 H40 120.5 ?
C39 C40 H40 120.5 ?
C42 C41 C40 121.5(6) ?
C42 C41 H41 119.3 ?
C40 C41 H41 119.3 ?
C41 C42 C37 120.2(6) ?
C41 C42 H42 119.9 ?
C37 C42 H42 119.9 ?
C44 C43 C48 118.0(5) ?
C44 C43 P 117.6(4) ?
C48 C43 P 124.4(4) ?
C43 C44 C45 121.7(6) ?
C43 C44 H44 119.1 ?
C45 C44 H44 119.1 ?
C46 C45 C44 119.1(6) ?
C46 C45 H45 120.4 ?
C44 C45 H45 120.4 ?
C47 C46 C45 120.5(6) ?
C47 C46 H46 119.8 ?
C45 C46 H46 119.8 ?
C46 C47 C48 120.4(5) ?
C46 C47 H47 119.8 ?
C48 C47 H47 119.8 ?
C43 C48 C47 120.3(5) ?
C43 C48 H48 119.8 ?
C47 C48 H48 119.8 ?
C54 C49 C50 118.3(6) ?
C54 C49 P 118.4(4) ?
C50 C49 P 123.3(4) ?
C49 C50 C51 119.5(6) ?
C49 C50 H50 120.2 ?
C51 C50 H50 120.2 ?
C52 C51 C50 120.5(6) ?
C52 C51 H51 119.8 ?
C50 C51 H51 119.8 ?
C51 C52 C53 120.8(7) ?
C51 C52 H52 119.6 ?
C53 C52 H52 119.6 ?
C52 C53 C54 119.8(7) ?
C52 C53 H53 120.1 ?
C54 C53 H53 120.1 ?
C53 C54 C49 121.1(6) ?
C53 C54 H54 119.5 ?
C49 C54 H54 119.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Os O1 1.672(3) y
Os O2 1.882(3) y
Os O5 1.892(3) y
Os O3 1.899(3) y
Os O4 1.902(3) y
P O8 1.488(3) y
P C37 1.791(5) y
P C43 1.806(5) y
P C49 1.808(5) y
O2 C1 1.473(5) y
O3 C7 1.458(5) y
O4 C13 1.472(5) y
O5 C19 1.481(5) y
O6 C25 1.443(5) y
O6 H1 0.81(5) y
O7 C31 1.441(6) y
O7 H2 0.83(6) y
C1 C2 1.533(7) ?
C1 C6 1.540(6) ?
C1 C7 1.546(7) y
C2 C3 1.509(7) ?
C2 H2A 0.9700 ?
C2 H2B 0.9700 ?
C3 C4 1.532(8) ?
C3 H3A 0.9700 ?
C3 H3B 0.9700 ?
C4 C5 1.530(8) ?
C4 H4A 0.9700 ?
C4 H4B 0.9700 ?
C5 C6 1.528(7) ?
C5 H5A 0.9700 ?
C5 H5B 0.9700 ?
C6 H6A 0.9700 ?
C6 H6B 0.9700 ?
C7 C8 1.531(7) ?
C7 C12 1.542(6) ?
C8 C9 1.518(7) ?
C8 H8A 0.9700 ?
C8 H8B 0.9700 ?
C9 C10 1.544(8) ?
C9 H9A 0.9700 ?
C9 H9B 0.9700 ?
C10 C11 1.516(9) ?
C10 H10A 0.9700 ?
C10 H10B 0.9700 ?
C11 C12 1.532(7) ?
C11 H11A 0.9700 ?
C11 H11B 0.9700 ?
C12 H12A 0.9700 ?
C12 H12B 0.9700 ?
C13 C19 1.529(7) ?
C13 C18 1.535(6) ?
C13 C14 1.539(7) ?
C14 C15 1.524(7) ?
C14 H14A 0.9700 ?
C14 H14B 0.9700 ?
C15 C16 1.531(7) ?
C15 H15A 0.9700 ?
C15 H15B 0.9700 ?
C16 C17 1.524(8) ?
C16 H16A 0.9700 ?
C16 H16B 0.9700 ?
C17 C18 1.526(7) ?
C17 H17A 0.9700 ?
C17 H17B 0.9700 ?
C18 H18A 0.9700 ?
C18 H18B 0.9700 ?
C19 C24 1.528(7) ?
C19 C20 1.542(7) ?
C20 C22 1.514(7) ?
C20 H20A 0.9700 ?
C20 H20B 0.9700 ?
C21 C22 1.523(9) ?
C21 C23 1.529(9) ?
C21 H21A 0.9700 ?
C21 H21B 0.9700 ?
C22 H22A 0.9700 ?
C22 H22B 0.9700 ?
C23 C24 1.523(7) ?
C23 H23A 0.9700 ?
C23 H23B 0.9700 ?
C24 H24A 0.9700 ?
C24 H24B 0.9700 ?
C25 C30 1.536(7) ?
C25 C26 1.536(7) ?
C25 C31 1.553(7) y
C26 C27 1.505(8) ?
C26 H26A 0.9700 ?
C26 H26B 0.9700 ?
C27 C28 1.516(10) ?
C27 H27A 0.9700 ?
C27 H27B 0.9700 ?
C28 C29 1.522(10) ?
C28 H28A 0.9700 ?
C28 H28B 0.9700 ?
C29 C30 1.530(8) ?
C29 H29A 0.9700 ?
C29 H29B 0.9700 ?
C30 H30A 0.9700 ?
C30 H30B 0.9700 ?
C31 C36 1.528(6) ?
C31 C32 1.539(7) ?
C32 C33 1.522(8) ?
C32 H32A 0.9700 ?
C32 H32B 0.9700 ?
C33 C34 1.516(9) ?
C33 H33A 0.9700 ?
C33 H33B 0.9700 ?
C34 C35 1.515(8) ?
C34 H34A 0.9700 ?
C34 H34B 0.9700 ?
C35 C36 1.531(7) ?
C35 H35A 0.9700 ?
C35 H35B 0.9700 ?
C36 H36A 0.9700 ?
C36 H36B 0.9700 ?
C37 C38 1.394(7) ?
C37 C42 1.396(7) ?
C38 C39 1.367(7) ?
C38 H38 0.9300 ?
C39 C40 1.388(8) ?
C39 H39 0.9300 ?
C40 C41 1.372(9) ?
C40 H40 0.9300 ?
C41 C42 1.370(8) ?
C41 H41 0.9300 ?
C42 H42 0.9300 ?
C43 C44 1.371(7) ?
C43 C48 1.379(7) ?
C44 C45 1.380(8) ?
C44 H44 0.9300 ?
C45 C46 1.363(9) ?
C45 H45 0.9300 ?
C46 C47 1.353(8) ?
C46 H46 0.9300 ?
C47 C48 1.384(7) ?
C47 H47 0.9300 ?
C48 H48 0.9300 ?
C49 C54 1.377(7) ?
C49 C50 1.383(7) ?
C50 C51 1.402(8) ?
C50 H50 0.9300 ?
C51 C52 1.338(9) ?
C51 H51 0.9300 ?
C52 C53 1.358(10) ?
C52 H52 0.9300 ?
C53 C54 1.376(9) ?
C53 H53 0.9300 ?
C54 H54 0.9300 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O6 H1 O8 0.81(5) 2.01(5) 2.802(5) 166(6)
O7 H2 O8 0.83(6) 2.07(6) 2.886(6) 167(6)
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_publ_flag
O1 Os O2 C1 80.8(3) ?
O5 Os O2 C1 -171.1(3) ?
O3 Os O2 C1 -28.3(3) ?
O4 Os O2 C1 -98.1(3) ?
O1 Os O3 C7 -104.9(3) ?
O2 Os O3 C7 2.9(3) ?
O5 Os O3 C7 75.8(4) ?
O4 Os O3 C7 144.4(3) ?
O1 Os O4 C13 104.8(3) ?
O2 Os O4 C13 -76.4(4) ?
O5 Os O4 C13 -2.2(3) ?
O3 Os O4 C13 -145.9(3) ?
O1 Os O5 C19 -83.8(3) ?
O2 Os O5 C19 167.2(3) ?
O3 Os O5 C19 95.5(3) ?
O4 Os O5 C19 26.7(3) ?
Os O2 C1 C2 -75.8(4) ?
Os O2 C1 C6 167.9(3) ?
Os O2 C1 C7 45.3(4) ?
O2 C1 C2 C3 -56.5(5) ?
C6 C1 C2 C3 57.2(6) ?
C7 C1 C2 C3 -171.6(4) ?
C1 C2 C3 C4 -58.7(6) ?
C2 C3 C4 C5 54.4(6) ?
C3 C4 C5 C6 -53.1(7) ?
C4 C5 C6 C1 53.0(6) ?
O2 C1 C6 C5 62.6(5) ?
C2 C1 C6 C5 -52.7(6) ?
C7 C1 C6 C5 177.3(4) ?
Os O3 C7 C8 -99.7(4) ?
Os O3 C7 C12 142.2(3) ?
Os O3 C7 C1 20.6(4) ?
O2 C1 C7 O3 -39.4(4) y
C2 C1 C7 O3 77.6(5) ?
C6 C1 C7 O3 -154.7(4) ?
O2 C1 C7 C8 76.4(4) ?
C2 C1 C7 C8 -166.6(4) ?
C6 C1 C7 C8 -38.9(6) ?
O2 C1 C7 C12 -155.8(4) ?
C2 C1 C7 C12 -38.8(6) ?
C6 C1 C7 C12 88.9(5) ?
O3 C7 C8 C9 -62.1(5) ?
C12 C7 C8 C9 53.2(5) ?
C1 C7 C8 C9 -177.2(4) ?
C7 C8 C9 C10 -56.8(6) ?
C8 C9 C10 C11 57.1(6) ?
C9 C10 C11 C12 -56.0(6) ?
C10 C11 C12 C7 53.9(6) ?
O3 C7 C12 C11 64.3(6) ?
C8 C7 C12 C11 -51.0(6) ?
C1 C7 C12 C11 179.9(4) ?
Os O4 C13 C19 -21.0(4) ?
Os O4 C13 C18 -143.4(3) ?
Os O4 C13 C14 100.3(4) ?
O4 C13 C14 C15 60.4(5) ?
C19 C13 C14 C15 176.6(4) ?
C18 C13 C14 C15 -53.1(5) ?
C13 C14 C15 C16 56.4(6) ?
C14 C15 C16 C17 -56.1(6) ?
C15 C16 C17 C18 55.8(6) ?
C16 C17 C18 C13 -54.9(6) ?
O4 C13 C18 C17 -62.2(5) ?
C19 C13 C18 C17 -178.8(4) ?
C14 C13 C18 C17 51.7(6) ?
Os O5 C19 C24 -167.0(3) ?
Os O5 C19 C13 -43.7(4) ?
Os O5 C19 C20 77.0(4) ?
O4 C13 C19 O5 38.7(4) y
C18 C13 C19 O5 154.9(4) ?
C14 C13 C19 O5 -77.6(5) ?
O4 C13 C19 C24 154.2(4) ?
C18 C13 C19 C24 -89.5(5) ?
C14 C13 C19 C24 38.0(6) ?
O4 C13 C19 C20 -78.3(5) ?
C18 C13 C19 C20 38.0(6) ?
C14 C13 C19 C20 165.4(4) ?
O5 C19 C20 C22 57.3(6) ?
C24 C19 C20 C22 -56.1(6) ?
C13 C19 C20 C22 172.5(4) ?
C19 C20 C22 C21 58.4(6) ?
C23 C21 C22 C20 -55.2(7) ?
C22 C21 C23 C24 52.8(7) ?
C21 C23 C24 C19 -52.4(7) ?
O5 C19 C24 C23 -62.8(6) ?
C13 C19 C24 C23 -178.1(4) ?
C20 C19 C24 C23 52.3(6) ?
O6 C25 C26 C27 -59.4(7) ?
C30 C25 C26 C27 54.1(7) ?
C31 C25 C26 C27 -179.5(5) ?
C25 C26 C27 C28 -54.9(8) ?
C26 C27 C28 C29 54.3(8) ?
C27 C28 C29 C30 -53.6(8) ?
C28 C29 C30 C25 54.1(7) ?
O6 C25 C30 C29 63.5(6) ?
C26 C25 C30 C29 -53.7(6) ?
C31 C25 C30 C29 -179.1(5) ?
O6 C25 C31 O7 -67.4(5) y
C30 C25 C31 O7 177.9(4) ?
C26 C25 C31 O7 53.4(5) ?
O6 C25 C31 C36 177.2(4) ?
C30 C25 C31 C36 62.5(6) ?
C26 C25 C31 C36 -62.0(6) ?
O6 C25 C31 C32 54.0(5) ?
C30 C25 C31 C32 -60.7(6) ?
C26 C25 C31 C32 174.8(5) ?
O7 C31 C32 C33 -55.5(7) ?
C36 C31 C32 C33 57.0(7) ?
C25 C31 C32 C33 -176.7(5) ?
C31 C32 C33 C34 -58.9(8) ?
C32 C33 C34 C35 57.0(8) ?
C33 C34 C35 C36 -55.3(8) ?
O7 C31 C36 C35 61.1(6) ?
C32 C31 C36 C35 -55.3(6) ?
C25 C31 C36 C35 179.8(4) ?
C34 C35 C36 C31 55.7(7) ?
O8 P C37 C38 34.5(5) ?
C43 P C37 C38 156.4(5) ?
C49 P C37 C38 -89.4(5) ?
O8 P C37 C42 -148.9(5) ?
C43 P C37 C42 -27.0(5) ?
C49 P C37 C42 87.3(5) ?
C42 C37 C38 C39 -0.5(9) ?
P C37 C38 C39 176.3(5) ?
C37 C38 C39 C40 -0.1(10) ?
C38 C39 C40 C41 0.1(10) ?
C39 C40 C41 C42 0.3(11) ?
C40 C41 C42 C37 -0.9(11) ?
C38 C37 C42 C41 0.9(9) ?
P C37 C42 C41 -175.8(5) ?
O8 P C43 C44 40.0(5) ?
C37 P C43 C44 -82.1(5) ?
C49 P C43 C44 163.9(5) ?
O8 P C43 C48 -142.5(5) ?
C37 P C43 C48 95.5(5) ?
C49 P C43 C48 -18.5(5) ?
C48 C43 C44 C45 1.4(10) ?
P C43 C44 C45 179.1(6) ?
C43 C44 C45 C46 -1.4(12) ?
C44 C45 C46 C47 0.8(12) ?
C45 C46 C47 C48 -0.4(11) ?
C44 C43 C48 C47 -1.0(9) ?
P C43 C48 C47 -178.5(5) ?
C46 C47 C48 C43 0.4(10) ?
O8 P C49 C54 51.5(5) ?
C37 P C49 C54 174.5(5) ?
C43 P C49 C54 -71.5(5) ?
O8 P C49 C50 -126.4(5) ?
C37 P C49 C50 -3.4(5) ?
C43 P C49 C50 110.6(5) ?
C54 C49 C50 C51 1.9(9) ?
P C49 C50 C51 179.7(5) ?
C49 C50 C51 C52 -0.8(10) ?
C50 C51 C52 C53 0.1(12) ?
C51 C52 C53 C54 -0.5(13) ?
C52 C53 C54 C49 1.6(13) ?
C50 C49 C54 C53 -2.3(10) ?
P C49 C54 C53 179.8(6) ?
