#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/75/4077515.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_4077515
loop_
_publ_author_name
'Wen, Ting Bin'
'Yang, Sheng-Yong'
'Zhou, Zhong Yuan'
'Lin, Zhenyang'
'Lau, Chak-Po'
'Jia, Guochen'
_publ_section_title
;
 Unexpected Formation of Osmium Carbyne and Vinylidene Complexes from the
 Reaction of OsCl2(PPh3)3with HC⋮CCMe3
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              3757
_journal_paper_doi               10.1021/om000306e
_journal_volume                  19
_journal_year                    2000
_chemical_formula_moiety         'C42 H41 Cl3 Os P2.1/2CH2Cl2'
_chemical_formula_sum            'C42.5 H42 Cl4 Os P2'
_chemical_formula_weight         946.70
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 104.406(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.9208(13)
_cell_length_b                   20.381(2)
_cell_length_c                   16.6709(16)
_cell_measurement_reflns_used    CCD
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     4252.1(7)
_computing_cell_refinement       'Bruker Smart'
_computing_data_collection       'Bruker Smart'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'BRUKER Smart CCD Area Detector'
_diffrn_measurement_method       ω
_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  0.0479
_diffrn_reflns_av_sigmaI/netI    0.0549
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            27942
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    3.353
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.718
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1884
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.347
_refine_diff_density_min         -0.749
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.960
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         9696
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0477P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0848
_refine_ls_wR_factor_ref         0.0915
_reflns_number_gt                7146
_reflns_number_total             9696
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om000306e.cif
_cod_data_source_block           Complex2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        4252.0(7)
_cod_original_sg_symbol_H-M      'P2(1)/c (No.14)'
_cod_original_formula_sum        'C42.50 H42 Cl4 Os P2'
_cod_database_code               4077515
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Os1 Os 0.379088(9) 0.595383(5) 0.307123(7) 0.02443(3) Uani 1 1 d .
P1 P 0.54781(6) 0.59236(4) 0.26550(5) 0.02799(18) Uani 1 1 d .
P2 P 0.21260(6) 0.61952(4) 0.34533(5) 0.02840(18) Uani 1 1 d .
Cl1 Cl 0.39051(6) 0.71568(4) 0.29013(5) 0.0395(2) Uani 1 1 d .
Cl2 Cl 0.47485(6) 0.60288(4) 0.45112(5) 0.0381(2) Uani 1 1 d .
Cl3 Cl 0.28252(6) 0.59605(4) 0.16515(5) 0.0390(2) Uani 1 1 d .
C1 C 0.3677(2) 0.51132(16) 0.31527(18) 0.0313(8) Uani 1 1 d .
C2 C 0.3619(3) 0.44109(16) 0.3267(2) 0.0445(10) Uani 1 1 d .
H2A H 0.3255 0.4333 0.3701 0.053 Uiso 1 1 calc R
H2B H 0.4342 0.4246 0.3463 0.053 Uiso 1 1 calc R
C3 C 0.3049(3) 0.39993(18) 0.2496(3) 0.0572(12) Uani 1 1 d .
C4 C 0.3638(4) 0.4066(3) 0.1834(3) 0.0893(17) Uani 1 1 d .
H4A H 0.3609 0.4514 0.1651 0.134 Uiso 1 1 calc R
H4B H 0.3314 0.3788 0.1375 0.134 Uiso 1 1 calc R
H4C H 0.4370 0.3938 0.2050 0.134 Uiso 1 1 calc R
C5 C 0.3105(5) 0.3285(2) 0.2814(4) 0.110(2) Uani 1 1 d .
H5A H 0.2763 0.2999 0.2369 0.165 Uiso 1 1 calc R
H5B H 0.2749 0.3253 0.3253 0.165 Uiso 1 1 calc R
H5C H 0.3840 0.3157 0.3016 0.165 Uiso 1 1 calc R
C6 C 0.1899(4) 0.4209(2) 0.2209(3) 0.0848(17) Uani 1 1 d .
H6A H 0.1866 0.4654 0.2014 0.127 Uiso 1 1 calc R
H6B H 0.1566 0.4181 0.2663 0.127 Uiso 1 1 calc R
H6C H 0.1532 0.3927 0.1769 0.127 Uiso 1 1 calc R
C7 C 0.5361(2) 0.61742(16) 0.15839(18) 0.0319(8) Uani 1 1 d .
C8 C 0.4868(3) 0.57736(18) 0.0923(2) 0.0426(9) Uani 1 1 d .
H8A H 0.4594 0.5369 0.1026 0.051 Uiso 1 1 calc R
C9 C 0.4782(3) 0.5971(2) 0.0113(2) 0.0538(11) Uani 1 1 d .
H9A H 0.4467 0.5696 -0.0325 0.065 Uiso 1 1 calc R
C10 C 0.5166(3) 0.6578(2) -0.0042(2) 0.0593(12) Uani 1 1 d .
H10A H 0.5115 0.6710 -0.0585 0.071 Uiso 1 1 calc R
C11 C 0.5622(3) 0.6985(2) 0.0602(2) 0.0629(12) Uani 1 1 d .
H11A H 0.5854 0.7401 0.0497 0.075 Uiso 1 1 calc R
C12 C 0.5738(3) 0.67772(19) 0.1412(2) 0.0466(10) Uani 1 1 d .
H12A H 0.6075 0.7050 0.1846 0.056 Uiso 1 1 calc R
C13 C 0.6077(2) 0.51050(15) 0.2742(2) 0.0345(8) Uani 1 1 d .
C14 C 0.6182(3) 0.47671(17) 0.3493(2) 0.0422(9) Uani 1 1 d .
H14A H 0.5978 0.4966 0.3931 0.051 Uiso 1 1 calc R
C15 C 0.6589(3) 0.41390(18) 0.3577(2) 0.0542(11) Uani 1 1 d .
H15A H 0.6643 0.3914 0.4070 0.065 Uiso 1 1 calc R
C16 C 0.6912(3) 0.3844(2) 0.2951(3) 0.0612(12) Uani 1 1 d .
H16A H 0.7164 0.3415 0.3012 0.073 Uiso 1 1 calc R
C17 C 0.6867(4) 0.4175(2) 0.2233(3) 0.0677(13) Uani 1 1 d .
H17A H 0.7116 0.3979 0.1814 0.081 Uiso 1 1 calc R
C18 C 0.6450(3) 0.4807(2) 0.2128(2) 0.0529(11) Uani 1 1 d .
H18A H 0.6421 0.5030 0.1637 0.063 Uiso 1 1 calc R
C19 C 0.6609(2) 0.64179(15) 0.32341(19) 0.0333(8) Uani 1 1 d .
C20 C 0.7590(3) 0.6324(2) 0.3066(2) 0.0476(10) Uani 1 1 d .
H20A H 0.7660 0.6010 0.2679 0.057 Uiso 1 1 calc R
C21 C 0.8468(3) 0.6687(2) 0.3460(3) 0.0544(11) Uani 1 1 d .
H21A H 0.9122 0.6616 0.3336 0.065 Uiso 1 1 calc R
C22 C 0.8380(3) 0.71564(19) 0.4040(2) 0.0507(11) Uani 1 1 d .
H22A H 0.8971 0.7404 0.4305 0.061 Uiso 1 1 calc R
C23 C 0.7415(3) 0.72508(19) 0.4219(2) 0.0479(10) Uani 1 1 d .
H23A H 0.7355 0.7558 0.4617 0.057 Uiso 1 1 calc R
C24 C 0.6516(2) 0.68893(16) 0.3810(2) 0.0384(9) Uani 1 1 d .
H24A H 0.5858 0.6966 0.3925 0.046 Uiso 1 1 calc R
C25 C 0.2168(2) 0.67114(15) 0.43614(18) 0.0299(7) Uani 1 1 d .
C26 C 0.2945(3) 0.71735(17) 0.4671(2) 0.0413(9) Uani 1 1 d .
H26A H 0.3521 0.7222 0.4434 0.050 Uiso 1 1 calc R
C27 C 0.2870(3) 0.75667(18) 0.5333(2) 0.0471(10) Uani 1 1 d .
H27A H 0.3400 0.7875 0.5539 0.057 Uiso 1 1 calc R
C28 C 0.2028(3) 0.75060(18) 0.5686(2) 0.0462(10) Uani 1 1 d .
H28A H 0.1984 0.7772 0.6129 0.055 Uiso 1 1 calc R
C29 C 0.1245(3) 0.70514(18) 0.5384(2) 0.0452(9) Uani 1 1 d .
H29A H 0.0667 0.7014 0.5619 0.054 Uiso 1 1 calc R
C30 C 0.1312(3) 0.66469(17) 0.4731(2) 0.0408(9) Uani 1 1 d .
H30A H 0.0788 0.6332 0.4537 0.049 Uiso 1 1 calc R
C31 C 0.1095(2) 0.66098(17) 0.26547(19) 0.0365(8) Uani 1 1 d .
C32 C 0.0888(3) 0.7273(2) 0.2762(2) 0.0505(11) Uani 1 1 d .
H32A H 0.1291 0.7503 0.3214 0.061 Uiso 1 1 calc R
C33 C 0.0070(3) 0.7587(2) 0.2183(2) 0.0631(12) Uani 1 1 d .
H33A H -0.0068 0.8029 0.2245 0.076 Uiso 1 1 calc R
C34 C -0.0517(3) 0.7250(3) 0.1535(3) 0.0716(14) Uani 1 1 d .
H34A H -0.1078 0.7459 0.1166 0.086 Uiso 1 1 calc R
C35 C -0.0312(3) 0.6619(3) 0.1409(3) 0.0708(15) Uani 1 1 d .
H35A H -0.0716 0.6399 0.0948 0.085 Uiso 1 1 calc R
C36 C 0.0511(3) 0.6291(2) 0.1971(2) 0.0520(11) Uani 1 1 d .
H36A H 0.0659 0.5855 0.1879 0.062 Uiso 1 1 calc R
C37 C 0.1500(2) 0.54547(16) 0.37477(19) 0.0354(8) Uani 1 1 d .
C38 C 0.2140(3) 0.51095(18) 0.4399(2) 0.0481(10) Uani 1 1 d .
H38A H 0.2837 0.5249 0.4627 0.058 Uiso 1 1 calc R
C39 C 0.1752(3) 0.4555(2) 0.4718(2) 0.0639(12) Uani 1 1 d .
H39A H 0.2188 0.4327 0.5159 0.077 Uiso 1 1 calc R
C40 C 0.0735(4) 0.4346(2) 0.4384(3) 0.0754(14) Uani 1 1 d .
H40A H 0.0481 0.3971 0.4588 0.091 Uiso 1 1 calc R
C41 C 0.0088(3) 0.4689(2) 0.3748(3) 0.0784(14) Uani 1 1 d .
H41A H -0.0612 0.4550 0.3530 0.094 Uiso 1 1 calc R
C42 C 0.0469(3) 0.52535(19) 0.3418(2) 0.0533(11) Uani 1 1 d .
H42A H 0.0028 0.5484 0.2984 0.064 Uiso 1 1 calc R
C43 C 0.1522(5) 0.5506(4) -0.0310(4) 0.215(9) Uani 0.50 1 d PD
Cl4 Cl 0.2294(2) 0.48547(18) -0.03958(18) 0.1252(12) Uani 0.50 1 d PD
Cl5 Cl 0.0872(4) 0.5965(4) -0.1161(3) 0.161(3) Uani 0.25 1 d PD
Cl6 Cl 0.0450(5) 0.5174(5) 0.0000(5) 0.177(4) Uani 0.25 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'
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'
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
C1 Os1 Cl3 92.86(9) .
C1 Os1 Cl2 90.99(9) .
Cl3 Os1 Cl2 175.99(3) .
C1 Os1 P2 94.67(10) .
Cl3 Os1 P2 88.87(3) .
Cl2 Os1 P2 89.70(3) .
C1 Os1 P1 95.56(10) .
Cl3 Os1 P1 90.10(3) .
Cl2 Os1 P1 90.64(3) .
P2 Os1 P1 169.77(3) .
C1 Os1 Cl1 177.79(9) .
Cl3 Os1 Cl1 84.96(3) .
Cl2 Os1 Cl1 91.19(3) .
P2 Os1 Cl1 84.94(3) .
P1 Os1 Cl1 84.83(3) .
C7 P1 C13 105.26(15) .
C7 P1 C19 102.82(14) .
C13 P1 C19 101.10(14) .
C7 P1 Os1 114.01(10) .
C13 P1 Os1 112.93(11) .
C19 P1 Os1 119.01(11) .
C25 P2 C37 100.10(15) .
C25 P2 C31 101.62(14) .
C37 P2 C31 106.48(15) .
C25 P2 Os1 118.98(10) .
C37 P2 Os1 112.29(11) .
C31 P2 Os1 115.51(11) .
C2 C1 Os1 176.8(2) .
C1 C2 C3 117.0(3) .
C4 C3 C6 112.5(4) .
C4 C3 C5 110.4(4) .
C6 C3 C5 109.6(4) .
C4 C3 C2 109.7(3) .
C6 C3 C2 109.6(3) .
C5 C3 C2 104.7(4) .
C12 C7 C8 118.3(3) .
C12 C7 P1 120.3(2) .
C8 C7 P1 121.3(3) .
C9 C8 C7 120.7(3) .
C10 C9 C8 119.8(3) .
C11 C10 C9 120.0(4) .
C10 C11 C12 120.0(4) .
C7 C12 C11 121.1(3) .
C18 C13 C14 118.2(3) .
C18 C13 P1 124.3(3) .
C14 C13 P1 117.6(3) .
C15 C14 C13 119.7(3) .
C16 C15 C14 121.1(4) .
C15 C16 C17 120.1(4) .
C16 C17 C18 120.0(4) .
C13 C18 C17 120.8(4) .
C20 C19 C24 118.7(3) .
C20 C19 P1 118.0(3) .
C24 C19 P1 123.3(2) .
C21 C20 C19 121.3(4) .
C20 C21 C22 120.3(3) .
C23 C22 C21 119.2(3) .
C22 C23 C24 120.7(3) .
C19 C24 C23 119.8(3) .
C26 C25 C30 118.8(3) .
C26 C25 P2 124.7(3) .
C30 C25 P2 116.4(2) .
C25 C26 C27 120.3(3) .
C28 C27 C26 120.7(3) .
C27 C28 C29 119.8(3) .
C28 C29 C30 120.4(3) .
C29 C30 C25 120.0(3) .
C36 C31 C32 118.9(3) .
C36 C31 P2 122.5(3) .
C32 C31 P2 118.6(2) .
C33 C32 C31 119.4(3) .
C34 C33 C32 120.0(4) .
C35 C34 C33 121.5(4) .
C34 C35 C36 120.0(4) .
C31 C36 C35 120.1(4) .
C42 C37 C38 119.6(3) .
C42 C37 P2 125.9(3) .
C38 C37 P2 114.3(2) .
C37 C38 C39 120.7(3) .
C40 C39 C38 119.9(4) .
C39 C40 C41 120.0(4) .
C40 C41 C42 120.8(4) .
C37 C42 C41 119.0(4) .
Cl4 C43 Cl6 104.6(5) .
Cl4 C43 Cl5 122.1(5) .
Cl6 C43 Cl5 101.2(5) .
Cl6 Cl6 C43 161.8(10) 3_565
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Os1 C1 1.728(3) .
Os1 Cl3 2.3852(8) .
Os1 Cl2 2.4164(8) .
Os1 P2 2.4407(8) .
Os1 P1 2.4476(8) .
Os1 Cl1 2.4767(8) .
P1 C7 1.827(3) .
P1 C13 1.830(3) .
P1 C19 1.838(3) .
P2 C25 1.833(3) .
P2 C37 1.836(3) .
P2 C31 1.838(3) .
C1 C2 1.448(4) .
C2 C3 1.557(5) .
C3 C4 1.495(7) .
C3 C6 1.506(6) .
C3 C5 1.545(6) .
C7 C12 1.378(5) .
C7 C8 1.392(4) .
C8 C9 1.388(5) .
C9 C10 1.380(6) .
C10 C11 1.369(6) .
C11 C12 1.387(5) .
C13 C18 1.377(5) .
C13 C14 1.405(5) .
C14 C15 1.378(5) .
C15 C16 1.356(6) .
C16 C17 1.363(6) .
C17 C18 1.389(5) .
C19 C20 1.378(5) .
C19 C24 1.385(5) .
C20 C21 1.375(5) .
C21 C22 1.385(6) .
C22 C23 1.366(5) .
C23 C24 1.402(4) .
C25 C26 1.380(4) .
C25 C30 1.399(5) .
C26 C27 1.387(5) .
C27 C28 1.365(5) .
C28 C29 1.371(5) .
C29 C30 1.385(5) .
C31 C36 1.365(5) .
C31 C32 1.397(5) .
C32 C33 1.396(5) .
C33 C34 1.343(6) .
C34 C35 1.339(7) .
C35 C36 1.400(6) .
C37 C42 1.372(5) .
C37 C38 1.382(5) .
C38 C39 1.395(5) .
C39 C40 1.361(6) .
C40 C41 1.368(6) .
C41 C42 1.416(6) .
C43 Cl4 1.687(7) .
C43 Cl6 1.731(7) .
C43 Cl5 1.733(7) .
Cl6 Cl6 1.363(13) 3_565
