#------------------------------------------------------------------------------
#$Date: 2016-02-19 16:29:56 +0200 (Fri, 19 Feb 2016) $
#$Revision: 176759 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/59/2005969.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_2005969
loop_
_publ_author_name
'Herlinger, A. W.'
'Rheingold, A. L.'
_publ_section_title
;Tetracarbonyl-1κ²C,2κ²C-μ-diphenylphosphido-P:P-μ-iodo-bis(triphenylphosphine)-1κP,2κP-diosmium(Os---Os)
 Benzene Solvate
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              285
_journal_page_last               287
_journal_paper_doi               10.1107/S0108270196013911
_journal_volume                  53
_journal_year                    1997
_chemical_formula_iupac
'[Os2 I(C12 H10 P)(C18 H15 P)2 (C O)4], C6 H6'
_chemical_formula_sum            'C58 H46 I O4 Os2 P3'
_chemical_formula_weight         1407.16
_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_type_scat_source           'SHELXTL (Sheldrick, 1985)'
_cell_angle_alpha                79.13(2)
_cell_angle_beta                 81.39(2)
_cell_angle_gamma                69.45(2)
_cell_formula_units_Z            2
_cell_length_a                   10.788(2)
_cell_length_b                   13.754(4)
_cell_length_c                   19.164(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      10
_cell_volume                     2604.0(12)
_diffrn_measurement_device
'Nicolet R3m diffractometer with graphite monochromator'
_diffrn_measurement_method       ω/2θ
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.022
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9167
_diffrn_reflns_theta_max         25
_diffrn_standards_decay_%        <1.0
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.61
_exptl_absorpt_correction_T_max  0.246
_exptl_absorpt_correction_T_min  0.153
_exptl_absorpt_correction_type   'semi-empirical (SHELXTL; Sheldrick, 1985)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.79
_exptl_crystal_density_method    none
_exptl_crystal_description       plate
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.84
_refine_diff_density_min         -0.59
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.0
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     673
_refine_ls_number_reflns         6810
_refine_ls_R_factor_obs          0.029
_refine_ls_shift/esd_max         0.12
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/σ²(Fₒ)+0.001Fₒ²'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.032
_reflns_number_observed          6810
_reflns_number_total             7071
_reflns_observed_criterion       F~o~>=5\s(F~o~)
_cod_data_source_file            bk1268.cif
_cod_data_source_block           bk1268a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value ' 1/\s^2^(F~o~)+0.001F~o~^2^' 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^(F~o~)+0.001F~o~^2^'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2604.0(10)
_cod_database_code               2005969
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
Os(1) .74421(2) -.12925(2) .79593(1) .031(1)
Os(2) .70288(2) .04570(2) .69083(1) .033(1)
I .90488(2) -.14037(4) .66935(2) .045(1)
P(1) .8231(2) .0147(1) .7930(1) .034(1)
P(2) .8521(2) -.2728(1) .8788(1) .033(1)
P(3) .7556(2) .1792(1) .6080(1) .034(1)
C(1) .6018(7) -.0829(6) .8618(4) .047(3)
O(1) .5099(5) -.0540(5) .9012(3) .079(3)
C(2) .6546(7) -.2031(6) .7590(4) .053(3)
O(2) .6011(7) -.2458(5) .7368(4) .088(3)
C(3) .5469(7) .1382(5) .7249(4) .045(3)
O(3) .4457(5) .1957(5) .7430(3) .081(3)
C(4) .6052(7) .0044(6) .6339(4) .054(3)
O(4) .5492(7) -.0237(5) .6005(4) .089(3)
C(11) .8585(3) .1022(4) .9073(5) .052(3)
C(12) .8143 .1523 .9676 .064(4)
C(13) .6784 .1946 .9871 .066(4)
C(14) .5867 .1867 .9461 .066(4)
C(15) .6309 .1366 .8857 .051(3)
C(16) .7668 .0943 .8663 .038(2)
C(21) 1.0950(4) -.0985(3) .8058(3) .057(3)
C(22) 1.2296 -.1092 .7977 .072(4)
C(23) 1.2704 -.0247 .7646 .069(4)
C(24) 1.1767 .0705 .7396 .060(4)
C(25) 1.0421 .0812 .7477 .051(3)
C(26) 1.0012 -.0033 .7808 .037(2)
C(31) .8187(5) -.3242(3) 1.0284(2) .050(3)
C(32) .7980 -.3014 1.0980 .064(4)
C(33) .7883 -.2020 1.1102 .066(4)
C(34) .7993 -.1254 1.0528 .066(4)
C(35) .8200 -.1482 .9832 .048(3)
C(36) .8297 -.2476 .9710 .037(2)
C(41) .6515(4) -.3584(3) .9070(3) .054(3)
C(42) .5949 -.4375 .9169 .074(5)
C(43) .6747 -.5401 .9088 .075(5)
C(44) .8112 -.5636 .8908 .074(4)
C(45) .8678 -.4845 .8810 .054(3)
C(46) .7879 -.3819 .8890 .039(3)
C(51) 1.1137(4) -.3653(4) .9189(2) .051(3)
C(52) 1.2495 -.4183 .9065 .075(4)
C(53) 1.3030 -.4454 .8392 .070(4)
C(54) 1.2206 -.4195 .7841 .060(3)
C(55) 1.0847 -.3665 .7965 .045(3)
C(56) 1.0313 -.3394 .8638 .035(2)
C(61) .6828(5) .3191(3) .7065(2) .053(3)
C(62) .6320 .4180 .7283 .068(4)
C(63) .5778 .5069 .6794 .081(4)
C(64) .5743 .4969 .6086 .078(4)
C(65) .6251 .3981 .5869 .059(3)
C(66) .6793 .3092 .6358 .038(2)
C(71) .7751(3) .2078(4) .4571(2) .046(3)
C(72) .7262 .2189 .3916 .065(4)
C(73) .5953 .2242 .3892 .055(3)
C(74) .5134 .2184 .4524 .056(3)
C(75) .5623 .2072 .5179 .048(3)
C(76) .6932 .2019 .5202 .036(2)
C(81) 1.0195(4) .0762(3) .5650(3) .047(3)
C(82) 1.1527 .0663 .5455 .058(3)
C(83) 1.1960 .1509 .5447 .062(4)
C(84) 1.1061 .2453 .5635 .064(4)
C(85) .9729 .2552 .5831 .051(3)
C(86) .9295 .1706 .5838 .036(2)
C(91) .856(2) .610(2) .3038(13) .101(9)
C(92) .979(2) .574(2) .2982(13) .138(8)
C(93) 1.042(2) .487(2) .3394(14) .135(8)
C(94) 1.017(3) .452(2) .3839(17) .143(10)
C(95) .911(2) .450(2) .4087(13) .142(8)
C(96) .813(2) .502(2) .3923(11) .110(7)
C(97) .7799(17) .574(1) .3486(10) .091(5)
C(91') .939(3) .584(2) .2943(15) .079(8)
C(92') 1.055(3) .528(4) .308(3) .114(14)
C(93') 1.095(7) .452(6) .334(5) .026(3)
C(94') .970(5) .425(4) .390(3) .152(18)
C(95') .867(4) .472(4) .432(3) .158(16)
C(96') .750(5) .556(4) .391(3) .173(18)
C(97') .812(4) .608(3) .318(2) .090(12)
H(11) .9521 .0731 .8939 .080
H(12) .8775 .1577 .9958 .080
H(13) .6480 .2290 1.0286 .080
H(14) .4932 .2158 .9595 .080
H(15) .5678 .1312 .8575 .080
H(21) 1.0669 -.1567 .8286 .080
H(22) 1.2941 -.1747 .8149 .080
H(23) 1.3631 -.0320 .7590 .080
H(24) 1.2048 .1287 .7168 .080
H(25) .9775 .1467 .7305 .080
H(31) .8254 -.3926 1.0200 .080
H(32) .7904 -.3541 1.1375 .080
H(33) .7740 -.1863 1.1581 .080
H(34) .7926 -.0570 1.0611 .080
H(35) .8275 -.0955 .9437 .080
H(41) .5965 -.2878 .9126 .080
H(42) .5010 -.4213 .9293 .080
H(43) .6358 -.5945 .9156 .080
H(44) .8661 -.6342 .8853 .080
H(45) .9617 -.5007 .8686 .080
H(51) 1.0769 -.3467 .9652 .080
H(52) 1.3062 -.4362 .9444 .080
H(53) 1.3964 -.4819 .8307 .080
H(54) 1.2573 -.4382 .7378 .080
H(55) 1.0280 -.3487 .7586 .080
H(61) .7202 .2580 .7402 .080
H(62) .6344 .4248 .7770 .080
H(63) .5428 .5749 .6944 .080
H(64) .5369 .5581 .5750 .080
H(65) .6227 .3912 .5382 .080
H(71) .8652 .2042 .4587 .080
H(72) .7826 .2230 .3481 .080
H(73) .5617 .2319 .3442 .080
H(74) .4233 .2220 .4508 .080
H(75) .5059 .2032 .5614 .080
H(81) .9896 .0180 .5655 .080
H(82) 1.2146 .0013 .5326 .080
H(83) 1.2878 .1441 .5313 .080
H(84) 1.1360 .3036 .5630 .080
H(85) .9110 .3203 .5960 .080
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
Os(2) Os(1) I 60.00(10) yes
I Os(1) P(1) 79.20(10) yes
I Os(1) P(2) 107.50(10) yes
Os(2) Os(1) C(1) 101.4(2) yes
P(1) Os(1) C(1) 94.6(3) yes
Os(2) Os(1) C(2) 99.1(2) yes
P(1) Os(1) C(2) 153.7(2) yes
C(1) Os(1) C(2) 91.2(3) yes
Os(1) Os(2) P(1) 54.70(10) yes
Os(1) Os(2) P(3) 157.60(10) yes
P(1) Os(2) P(3) 107.90(10) yes
I Os(2) C(3) 161.1(2) yes
P(3) Os(2) C(3) 92.5(2) yes
I Os(2) C(4) 85.7(2) yes
P(3) Os(2) C(4) 99.7(2) yes
Os(1) I Os(2) 60.40(10) yes
Os(1) P(1) C(16) 119.4(2) yes
Os(1) P(1) C(26) 121.3(2) yes
Os(1) P(2) C(36) 115.40(10) yes
Os(1) P(2) C(56) 119.70(10) yes
Os(2) P(3) C(76) 114.9(2) yes
Os(1) C(1) O(1) 177.5(7) yes
Os(2) C(3) O(3) 176.1(7) yes
Os(2) Os(1) P(1) 54.60(10) yes
Os(2) Os(1) P(2) 160.40(10) yes
P(1) Os(1) P(2) 110.50(10) yes
I Os(1) C(1) 160.6(2) yes
P(2) Os(1) C(1) 91.8(2) yes
I Os(1) C(2) 86.9(2) yes
P(2) Os(1) C(2) 94.9(2) yes
Os(1) Os(2) I 59.60(10) yes
I Os(2) P(1) 79.00(10) yes
I Os(2) P(3) 106.40(10) yes
Os(1) Os(2) C(3) 103.1(2) yes
P(1) Os(2) C(3) 97.4(2) yes
Os(1) Os(2) C(4) 96.6(2) yes
P(1) Os(2) C(4) 151.3(2) yes
C(3) Os(2) C(4) 89.3(3) yes
Os(1) P(1) Os(2) 70.80(10) yes
Os(2) P(1) C(16) 124.00(10) yes
Os(2) P(1) C(26) 119.8(2) yes
Os(1) P(2) C(46) 113.0(2) yes
Os(2) P(3) C(66) 113.00(10) yes
Os(2) P(3) C(86) 120.00(10) yes
Os(1) C(2) O(2) 179.3(5) yes
Os(2) C(4) O(4) 177.7(6) yes
P(1) C(16) C(11) 120.50(10) no
P(1) C(26) C(21) 121.10(10) no
P(2) C(36) C(31) 121.50(10) no
P(2) C(46) C(41) 116.40(10) no
P(2) C(56) C(51) 121.10(10) no
P(3) C(66) C(61) 118.70(10) no
P(3) C(76) C(71) 121.70(10) no
P(3) C(86) C(81) 118.00(10) no
C(92) C(91) C(97) 126.(2) no
C(91) C(92) C(93) 121.(3) no
C(92) C(93) C(95) 107.2(18) no
P(1) C(16) C(15) 119.10(10) no
P(1) C(26) C(25) 118.80(10) no
P(2) C(36) C(35) 118.50(10) no
P(2) C(46) C(45) 123.60(10) no
P(2) C(56) C(55) 118.90(10) no
P(3) C(66) C(65) 121.20(10) no
P(3) C(76) C(75) 118.20(10) no
P(3) C(86) C(85) 122.00(10) no
C(92) C(93) C(94) 133.(3) no
C(93) C(94) C(95) 129.(4) no
C(93) C(95) C(96) 107.(2) no
C(95) C(96) C(97) 133.(3) no
C(97) C(96) C(94') 120.(3) no
C(94) C(95) C(96) 129.(3) no
C(92') C(91') C(97') 144.(3) no
C(91') C(92') C(93') 133.(7) no
C(92') C(93') C(94') 107.(6) no
C(93') C(94') C(95') 140.(6) no
C(94') C(95') C(96') 115.(5) no
C(95') C(96') C(97') 108.(4) no
C(91') C(97') C(96') 127.(3) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Os(1) . Os(2) . 2.781(1) yes
Os(1) . I . 2.758(1) yes
Os(1) . P(1) . 2.403(2) yes
Os(1) . P(2) . 2.352(1) yes
Os(1) . C(1) . 1.843(6) yes
Os(1) . C(2) . 1.907(10) yes
Os(2) . I . 2.771(1) yes
Os(2) . P(1) . 2.399(2) yes
Os(2) . P(3) . 2.362(2) yes
Os(2) . C(3) . 1.833(6) yes
Os(2) . C(4) . 1.902(10) yes
P(1) . C(26) . 1.833(5) no
P(2) . C(46) . 1.830(5) no
P(3) . C(66) . 1.830(4) no
P(3) . C(86) . 1.831(5) no
C(2) . O(2) . 1.125(13) no
C(4) . O(4) . 1.139(13) no
C(91) . C(97) . 1.26(3) no
C(93) . C(94) . 0.950(40) no
C(94) . C(95) . 1.177(41) no
P(1) . C(16) . 1.844(5) no
P(2) . C(36) . 1.828(5) no
P(2) . C(56) . 1.830(4) no
P(3) . C(76) . 1.838(5) no
C(1) . O(1) . 1.151(8) no
C(3) . O(3) . 1.150(8) no
C(91) . C(92) . 1.24(3) no
C(92) . C(93) . 1.325(30) no
(93) . C(95) . 1.926(36) no
C(95) . C(96) . 1.10(3) no
C(96) . C(97) . 1.16(3) no
C(91') . C(92') . 1.25(5) no
C(94') . C(95') . 1.31(7) no
C(96') . C(97') . 1.610(7) no
