#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/05/2200532.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# 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_2200532
loop_
_publ_author_name
'Li, Zhengkai'
'Zhou, Zhongyuan'
_publ_section_title
;
 trans-Tetrachlorobis(triphenylphosphine)osmium(IV)
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m291
_journal_page_last               m292
_journal_paper_doi               10.1107/S1600536801008698
_journal_volume                  57
_journal_year                    2001
_chemical_formula_moiety         'C36 H30 Cl4 Os P2'
_chemical_formula_sum            'C36 H30 Cl4 Os P2'
_chemical_formula_weight         856.54
_chemical_name_systematic
;
trans-Tetrachloro-bis(triphenylphosphine)osmium(IV)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90
_cell_angle_beta                 117.425(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.3364(9)
_cell_length_b                   20.948(2)
_cell_length_c                   9.6251(9)
_cell_measurement_reflns_used    CCD
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.0
_cell_volume                     1670.9(3)
_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, 1997)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full .997
_diffrn_measured_fraction_theta_max .997
_diffrn_measurement_device_type  'Bruker CCD Area Detector'
_diffrn_measurement_method       'phi and omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .044
_diffrn_reflns_av_sigmaI/netI    .046
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            11100
_diffrn_reflns_theta_full        27.6
_diffrn_reflns_theta_max         27.6
_diffrn_reflns_theta_min         1.9
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.257
_exptl_absorpt_correction_T_max  .676
_exptl_absorpt_correction_T_min  .483
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.702
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             840
_exptl_crystal_size_max          .20
_exptl_crystal_size_mid          .16
_exptl_crystal_size_min          .10
_refine_diff_density_max         .98
_refine_diff_density_min         -.60
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   .98
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         3844
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      .98
_refine_ls_R_factor_all          .046
_refine_ls_R_factor_gt           .032
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0409P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .078
_reflns_number_gt                2867
_reflns_number_total             3844
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            tk6024.cif
_cod_data_source_block           I
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2200532
_cod_database_fobs_code          2200532
loop_
_symmetry_equiv_pos_as_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'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Os1 .0000 .5000 .0000 .02692(8) Uani d S 1 . . Os
Cl1 -.02973(14) .52136(6) -.24674(13) .0406(3) Uani d . 1 . . Cl
Cl2 .23832(14) .55820(6) .11330(14) .0459(3) Uani d . 1 . . Cl
P1 .16725(13) .40280(5) .02986(12) .0292(2) Uani d . 1 . . P
C1 .3804(5) .4102(2) .1714(5) .0343(9) Uani d . 1 . . C
C2 .5065(6) .3981(3) .1369(6) .0509(12) Uani d . 1 . . C
H2A .4798 .3867 .0331 .042 Uiso d . 1 . . H
C3 .6625(7) .4013(3) .2523(8) .0691(17) Uani d . 1 . . C
H3A .7317 .3842 .2281 .062 Uiso d . 1 . . H
C4 .6988(6) .4155(3) .4024(7) .0661(17) Uani d . 1 . . C
H4A .8052 .4218 .4886 .081 Uiso d . 1 . . H
C5 .5765(6) .4273(3) .4389(6) .0650(16) Uani d . 1 . . C
H5A .5996 .4369 .5414 .078 Uiso calc R 1 . . H
C6 .4184(6) .4251(3) .3236(6) .0555(14) Uani d . 1 . . C
H6A .3359 .4339 .3493 .067 Uiso calc R 1 . . H
C7 .1138(5) .32993(19) .0984(5) .0350(10) Uani d . 1 . . C
C8 -.0207(6) .3227(2) .1166(7) .0556(14) Uani d . 1 . . C
H8A -.0932 .3564 .0923 .067 Uiso calc R 1 . . H
C9 -.0518(8) .2658(3) .1709(8) .0722(18) Uani d . 1 . . C
H9A -.1450 .2623 .1826 .087 Uiso calc R 1 . . H
C10 .0460(7) .2166(3) .2065(8) .0685(17) Uani d . 1 . . C
H10A .0247 .1792 .2459 .082 Uiso calc R 1 . . H
C11 .1791(8) .2218(3) .1842(9) .0893(19) Uani d . 1 . . C
H11A .2588 .1883 .2088 .105 Uiso d . 1 . . H
C12 .2146(7) .2783(3) .1329(8) .0730(15) Uani d . 1 . . C
H12A .3101 .2831 .1071 .091 Uiso d . 1 . . H
C13 .1654(5) .3819(2) -.1535(5) .0331(9) Uani d . 1 . . C
C14 .0885(6) .3280(2) -.2372(6) .0487(12) Uani d . 1 . . C
H14A .0412 .2996 -.1963 .058 Uiso calc R 1 . . H
C15 .0816(7) .3160(3) -.3819(6) .0635(15) Uani d . 1 . . C
H15A .0293 .2796 -.4373 .076 Uiso calc R 1 . . H
C16 .1505(7) .3570(3) -.4435(6) .0644(16) Uani d . 1 . . C
H16A .1449 .3486 -.5408 .077 Uiso calc R 1 . . H
C17 .2274(8) .4103(3) -.3629(6) .0604(16) Uani d . 1 . . C
H17A .2790 .4386 -.3868 .071 Uiso d . 1 . . H
C18 .2355(6) .4237(2) -.2182(6) .0483(12) Uani d . 1 . . C
H18A .2875 .4605 -.1644 .058 Uiso calc R 1 . . H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P .1023 .0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl .1484 .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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
Cl1 Os1 Cl1 3_565 . 180.00(6)
Cl1 Os1 Cl2 3_565 3_565 90.95(4)
Cl1 Os1 Cl2 . 3_565 89.05(4)
Cl1 Os1 Cl2 3_565 . 89.05(4)
Cl1 Os1 Cl2 . . 90.95(4)
Cl2 Os1 Cl2 3_565 . 180.00(5)
Cl1 Os1 P1 3_565 3_565 92.81(4)
Cl1 Os1 P1 . 3_565 87.19(4)
Cl2 Os1 P1 3_565 3_565 87.76(4)
Cl2 Os1 P1 . 3_565 92.24(4)
Cl1 Os1 P1 3_565 . 87.19(4)
Cl1 Os1 P1 . . 92.81(4)
Cl2 Os1 P1 3_565 . 92.24(4)
Cl2 Os1 P1 . . 87.76(4)
P1 Os1 P1 3_565 . 180.0
C13 P1 C7 . . 105.6(2)
C13 P1 C1 . . 105.37(19)
C7 P1 C1 . . 100.8(2)
C13 P1 Os1 . . 111.06(13)
C7 P1 Os1 . . 117.60(14)
C1 P1 Os1 . . 115.10(14)
C6 C1 C2 . . 117.8(4)
C6 C1 P1 . . 118.1(3)
C2 C1 P1 . . 124.0(3)
C3 C2 C1 . . 120.1(5)
C4 C3 C2 . . 121.7(5)
C3 C4 C5 . . 119.1(5)
C4 C5 C6 . . 120.0(5)
C1 C6 C5 . . 121.3(5)
C8 C7 C12 . . 117.1(4)
C8 C7 P1 . . 124.4(3)
C12 C7 P1 . . 118.5(4)
C7 C8 C9 . . 120.9(5)
C10 C9 C8 . . 122.2(5)
C9 C10 C11 . . 118.1(5)
C10 C11 C12 . . 120.9(6)
C7 C12 C11 . . 120.8(5)
C14 C13 C18 . . 118.4(4)
C14 C13 P1 . . 122.3(3)
C18 C13 P1 . . 119.1(3)
C13 C14 C15 . . 120.4(5)
C16 C15 C14 . . 120.7(5)
C17 C16 C15 . . 120.0(5)
C16 C17 C18 . . 120.7(5)
C17 C18 C13 . . 119.9(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Os1 Cl1 3_565 2.3044(11) ?
Os1 Cl1 . 2.3044(11) ?
Os1 Cl2 3_565 2.3220(11) ?
Os1 Cl2 . 2.3220(11) ?
Os1 P1 3_565 2.5007(11) ?
Os1 P1 . 2.5007(11) ?
P1 C13 . 1.811(4) ?
P1 C7 . 1.822(4) ?
P1 C1 . 1.829(4) ?
C1 C6 . 1.375(6) ?
C1 C2 . 1.385(6) ?
C2 C3 . 1.367(7) ?
C3 C4 . 1.356(8) ?
C4 C5 . 1.363(7) ?
C5 C6 . 1.380(7) ?
C7 C8 . 1.354(6) ?
C7 C12 . 1.370(7) ?
C8 C9 . 1.385(7) ?
C9 C10 . 1.314(8) ?
C10 C11 . 1.359(8) ?
C11 C12 . 1.381(8) ?
C13 C14 . 1.380(6) ?
C13 C18 . 1.400(6) ?
C14 C15 . 1.387(7) ?
C15 C16 . 1.362(8) ?
C16 C17 . 1.360(8) ?
C17 C18 . 1.388(7) ?
