#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:43:06 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178664 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/75/4077563.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_4077563
loop_
_publ_author_name
'Rickard, Clifton E. F.'
'Roper, Warren R.'
'Williamson, Alex'
'Wright, L. James'
_publ_section_title
;
 Reactions ofcisandtransBcat, Aryl Osmium Complexes (cat = 1,2-O2C6H4).
 Bis(Bcat) Complexes of Osmium and Ruthenium and a Structural Comparison
 ofcisandtransIsomers of Os(Bcat)I(CO)2(PPh3)2
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              4344
_journal_paper_doi               10.1021/om0004601
_journal_volume                  19
_journal_year                    2000
_chemical_formula_moiety         'C40 H30 Cl4 O2 Os P2'
_chemical_formula_sum            'C40 H30 Cl4 O2 Os P2'
_chemical_formula_weight         936.58
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.07120(10)
_cell_length_b                   17.26220(10)
_cell_length_c                   34.63010(10)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     7216.06(8)
_computing_cell_refinement       'Siemens SMART'
_computing_data_collection       'Siemens SMART (Siemens, 1995)'
_computing_data_reduction        'Siemens SAINT  (Siemens, 1995)'
_computing_molecular_graphics    'Siemens SHELXTL (Siemens, 1994)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 Sheldrick, (1997)'
_computing_structure_solution    'SHELXS Sheldrick, (1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.896
_diffrn_measured_fraction_theta_max 0.896
_diffrn_measurement_device_type  'Siemens SMART'
_diffrn_measurement_method       'Area detector ω scans'
_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  0.0255
_diffrn_reflns_av_sigmaI/netI    0.0186
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            43497
_diffrn_reflns_theta_full        27.15
_diffrn_reflns_theta_max         27.15
_diffrn_reflns_theta_min         2.06
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    3.955
_exptl_absorpt_correction_T_max  0.6274
_exptl_absorpt_correction_T_min  0.2874
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.724
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             3680
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.468
_refine_diff_density_min         -2.150
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.393
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         7861
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.393
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0434
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0000P)²+49.2765P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0902
_refine_ls_wR_factor_ref         0.0914
_reflns_number_gt                7319
_reflns_number_total             7861
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0004601.cif
_cod_data_source_block           '[12]'
_cod_depositor_comments
;
The following automatic conversions were performed:

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

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' 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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+49.2765P] 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^)+(0.0000P)^2^+49.2765P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P bca'
_cod_database_code               4077563
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, 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 0.727082(16) 0.381867(12) 0.116673(6) 0.01886(6) Uani 1 d .
P1 P 0.52567(11) 0.37778(8) 0.12459(4) 0.0220(3) Uani 1 d .
P2 P 0.92831(11) 0.38663(8) 0.10980(4) 0.0209(3) Uani 1 d .
Cl1 Cl 0.72420(13) 0.42493(10) 0.04849(5) 0.0372(4) Uani 1 d .
Cl2 Cl 0.81532(15) 0.48369(10) 0.20535(5) 0.0409(4) Uani 1 d .
Cl4 Cl 0.64611(14) 0.56739(9) 0.10547(5) 0.0394(4) Uani 1 d .
Cl3 Cl 0.72200(17) 0.62975(10) 0.18275(7) 0.0566(5) Uani 1 d .
O1 O 0.7323(4) 0.3081(2) 0.19294(14) 0.0322(10) Uani 1 d .
O2 O 0.7285(4) 0.2266(3) 0.07365(14) 0.0370(11) Uani 1 d .
C1 C 0.7317(5) 0.3369(4) 0.1668(2) 0.0302(13) Uani 1 d .
C2 C 0.7282(5) 0.2817(3) 0.09114(17) 0.0259(12) Uani 1 d .
C3 C 0.7486(6) 0.5327(4) 0.1694(2) 0.0377(15) Uani 1 d .
C4 C 0.7193(5) 0.4991(3) 0.13762(19) 0.0302(13) Uani 1 d .
C11 C 0.4428(5) 0.3741(3) 0.08065(17) 0.0260(12) Uani 1 d .
C12 C 0.3648(5) 0.3159(4) 0.0740(2) 0.0346(14) Uani 1 d .
H12A H 0.3553 0.2753 0.0922 0.042 Uiso 1 calc R
C13 C 0.3006(6) 0.3179(4) 0.0403(2) 0.0440(18) Uani 1 d .
H13A H 0.2478 0.2782 0.0357 0.053 Uiso 1 calc R
C14 C 0.3133(6) 0.3767(5) 0.0140(2) 0.0456(18) Uani 1 d .
H14A H 0.2685 0.3777 -0.0085 0.055 Uiso 1 calc R
C15 C 0.3901(5) 0.4340(4) 0.02010(19) 0.0381(15) Uani 1 d .
H15A H 0.3989 0.4743 0.0017 0.046 Uiso 1 calc R
C16 C 0.4550(5) 0.4330(4) 0.05330(17) 0.0297(13) Uani 1 d .
H16A H 0.5082 0.4727 0.0574 0.036 Uiso 1 calc R
C21 C 0.4666(5) 0.4586(3) 0.15191(17) 0.0241(12) Uani 1 d .
C22 C 0.3811(5) 0.5056(4) 0.13779(19) 0.0321(14) Uani 1 d .
H22A H 0.3505 0.4957 0.1130 0.038 Uiso 1 calc R
C23 C 0.3410(6) 0.5664(4) 0.1598(2) 0.0419(17) Uani 1 d .
H23A H 0.2839 0.5987 0.1499 0.050 Uiso 1 calc R
C24 C 0.3842(6) 0.5802(4) 0.1964(2) 0.0429(17) Uani 1 d .
H24A H 0.3568 0.6221 0.2114 0.051 Uiso 1 calc R
C25 C 0.4670(6) 0.5332(4) 0.2108(2) 0.0396(16) Uani 1 d .
H25A H 0.4958 0.5423 0.2360 0.047 Uiso 1 calc R
C26 C 0.5083(5) 0.4727(4) 0.18869(18) 0.0303(13) Uani 1 d .
H26A H 0.5654 0.4406 0.1987 0.036 Uiso 1 calc R
C31 C 0.4762(5) 0.2947(3) 0.15326(18) 0.0266(12) Uani 1 d .
C32 C 0.5246(6) 0.2230(4) 0.1503(2) 0.0442(18) Uani 1 d .
H32A H 0.5852 0.2159 0.1332 0.053 Uiso 1 calc R
C33 C 0.4868(6) 0.1604(4) 0.1721(3) 0.052(2) Uani 1 d .
H33A H 0.5214 0.1112 0.1694 0.062 Uiso 1 calc R
C34 C 0.4005(6) 0.1693(4) 0.1971(2) 0.0461(18) Uani 1 d .
H34A H 0.3753 0.1269 0.2122 0.055 Uiso 1 calc R
C35 C 0.3506(7) 0.2405(5) 0.1999(2) 0.053(2) Uani 1 d .
H35A H 0.2896 0.2470 0.2170 0.064 Uiso 1 calc R
C36 C 0.3871(6) 0.3025(4) 0.1786(2) 0.0443(18) Uani 1 d .
H36A H 0.3513 0.3513 0.1812 0.053 Uiso 1 calc R
C41 C 0.9906(5) 0.4705(3) 0.08568(15) 0.0220(11) Uani 1 d .
C42 C 1.1011(5) 0.4651(4) 0.0736(2) 0.0357(15) Uani 1 d .
H42A H 1.1410 0.4181 0.0769 0.043 Uiso 1 calc R
C43 C 1.1521(5) 0.5288(4) 0.0567(2) 0.0390(16) Uani 1 d .
H43A H 1.2270 0.5249 0.0484 0.047 Uiso 1 calc R
C44 C 1.0960(5) 0.5968(4) 0.05173(19) 0.0342(14) Uani 1 d .
H44A H 1.1318 0.6401 0.0402 0.041 Uiso 1 calc R
C45 C 0.9877(6) 0.6023(4) 0.0635(3) 0.052(2) Uani 1 d .
H45A H 0.9486 0.6496 0.0602 0.063 Uiso 1 calc R
C46 C 0.9344(6) 0.5388(4) 0.0804(2) 0.0383(16) Uani 1 d .
H46A H 0.8593 0.5430 0.0883 0.046 Uiso 1 calc R
C51 C 1.0047(5) 0.3803(4) 0.15549(16) 0.0269(12) Uani 1 d .
C52 C 1.0798(5) 0.4371(4) 0.16655(18) 0.0337(14) Uani 1 d .
H52A H 1.0933 0.4799 0.1500 0.040 Uiso 1 calc R
C53 C 1.1355(6) 0.4321(5) 0.2016(2) 0.0446(18) Uani 1 d .
H53A H 1.1859 0.4716 0.2091 0.054 Uiso 1 calc R
C54 C 1.1173(7) 0.3701(5) 0.2252(2) 0.053(2) Uani 1 d .
H54A H 1.1560 0.3663 0.2490 0.063 Uiso 1 calc R
C55 C 1.0436(7) 0.3131(5) 0.2149(2) 0.052(2) Uani 1 d .
H55A H 1.0312 0.2705 0.2318 0.063 Uiso 1 calc R
C56 C 0.9866(6) 0.3172(4) 0.17977(18) 0.0363(15) Uani 1 d .
H56A H 0.9363 0.2775 0.1726 0.044 Uiso 1 calc R
C61 C 0.9847(5) 0.3064(3) 0.08094(17) 0.0245(12) Uani 1 d .
C62 C 0.9709(5) 0.3091(4) 0.04103(19) 0.0364(15) Uani 1 d .
H62A H 0.9333 0.3517 0.0296 0.044 Uiso 1 calc R
C63 C 1.0114(6) 0.2505(5) 0.0179(2) 0.0431(17) Uani 1 d .
H63A H 1.0021 0.2536 -0.0092 0.052 Uiso 1 calc R
C64 C 1.0652(6) 0.1878(4) 0.0337(2) 0.0404(16) Uani 1 d .
H64A H 1.0936 0.1481 0.0175 0.049 Uiso 1 calc R
C65 C 1.0771(7) 0.1833(4) 0.0727(2) 0.051(2) Uani 1 d .
H65A H 1.1123 0.1393 0.0837 0.061 Uiso 1 calc R
C66 C 1.0382(7) 0.2426(4) 0.0968(2) 0.0437(18) Uani 1 d .
H66A H 1.0485 0.2392 0.1240 0.052 Uiso 1 calc R
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'
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'
Cl Cl 0.1484 0.1585 '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
C1 Os C2 93.0(2) y
C1 Os C4 94.4(2) y
C2 Os C4 172.3(3) y
C1 Os P2 94.22(18) y
C2 Os P2 88.78(17) y
C4 Os P2 92.57(16) y
C1 Os P1 85.13(18) y
C2 Os P1 91.84(17) y
C4 Os P1 86.89(16) y
P2 Os P1 179.12(5) y
C1 Os Cl1 173.31(18) y
C2 Os Cl1 80.39(18) y
C4 Os Cl1 92.22(18) y
P2 Os Cl1 84.89(5) y
P1 Os Cl1 95.83(5) y
C11 P1 C21 104.2(3) ?
C11 P1 C31 104.1(3) ?
C21 P1 C31 100.9(3) ?
C11 P1 Os 116.92(19) ?
C21 P1 Os 115.00(19) ?
C31 P1 Os 113.87(19) ?
C41 P2 C51 103.5(3) ?
C41 P2 C61 101.3(2) ?
C51 P2 C61 103.8(3) ?
C41 P2 Os 118.61(18) ?
C51 P2 Os 114.43(19) ?
C61 P2 Os 113.33(19) ?
O1 C1 Os 175.2(6) y
O2 C2 Os 174.6(5) y
C4 C3 Cl2 121.9(5) y
C4 C3 Cl3 126.7(6) y
Cl2 C3 Cl3 111.3(4) y
C3 C4 Cl4 110.9(5) y
C3 C4 Os 134.2(5) y
Cl4 C4 Os 114.7(3) y
C12 C11 C16 118.9(6) ?
C12 C11 P1 122.3(5) ?
C16 C11 P1 118.8(5) ?
C11 C12 C13 119.6(7) ?
C14 C13 C12 120.6(7) ?
C13 C14 C15 120.5(6) ?
C14 C15 C16 119.8(7) ?
C15 C16 C11 120.6(6) ?
C26 C21 C22 119.0(6) ?
C26 C21 P1 117.7(4) ?
C22 C21 P1 123.2(5) ?
C23 C22 C21 120.3(6) ?
C22 C23 C24 120.0(7) ?
C25 C24 C23 120.1(6) ?
C24 C25 C26 120.1(7) ?
C25 C26 C21 120.4(6) ?
C32 C31 C36 117.5(6) ?
C32 C31 P1 121.6(5) ?
C36 C31 P1 120.9(5) ?
C31 C32 C33 121.3(7) ?
C34 C33 C32 120.4(7) ?
C33 C34 C35 118.8(7) ?
C36 C35 C34 121.2(7) ?
C35 C36 C31 120.7(7) ?
C46 C41 C42 119.2(6) ?
C46 C41 P2 122.5(4) ?
C42 C41 P2 118.2(4) ?
C43 C42 C41 119.6(6) ?
C44 C43 C42 120.9(6) ?
C43 C44 C45 119.6(6) ?
C44 C45 C46 120.5(6) ?
C41 C46 C45 120.1(6) ?
C52 C51 C56 119.2(6) ?
C52 C51 P2 121.6(5) ?
C56 C51 P2 119.2(5) ?
C51 C52 C53 120.8(7) ?
C54 C53 C52 119.6(7) ?
C53 C54 C55 120.7(7) ?
C54 C55 C56 120.5(7) ?
C51 C56 C55 119.2(7) ?
C66 C61 C62 118.4(6) ?
C66 C61 P2 123.6(5) ?
C62 C61 P2 118.0(5) ?
C63 C62 C61 120.5(6) ?
C64 C63 C62 121.1(7) ?
C65 C64 C63 119.2(6) ?
C64 C65 C66 120.9(7) ?
C61 C66 C65 119.8(7) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Os C1 1.901(8) y
Os C2 1.941(6) y
Os C4 2.151(6) y
Os P2 2.4421(14) y
Os P1 2.4477(14) y
Os Cl1 2.4757(16) y
P1 C11 1.822(6) ?
P1 C21 1.831(6) ?
P1 C31 1.844(6) ?
P2 C41 1.833(6) ?
P2 C51 1.834(6) ?
P2 C61 1.839(6) ?
Cl2 C3 1.707(8) y
Cl4 C4 1.847(7) y
Cl3 C3 1.768(7) y
O1 C1 1.034(8) y
O2 C2 1.128(7) y
C3 C4 1.293(9) y
C11 C12 1.395(8) ?
C11 C16 1.398(8) ?
C12 C13 1.400(10) ?
C13 C14 1.371(11) ?
C14 C15 1.373(11) ?
C15 C16 1.392(9) ?
C21 C26 1.391(8) ?
C21 C22 1.401(8) ?
C22 C23 1.385(9) ?
C23 C24 1.389(11) ?
C24 C25 1.382(10) ?
C25 C26 1.389(9) ?
C31 C32 1.374(9) ?
C31 C36 1.395(9) ?
C32 C33 1.394(9) ?
C33 C34 1.363(11) ?
C34 C35 1.373(11) ?
C35 C36 1.372(10) ?
C41 C46 1.372(8) ?
C41 C42 1.402(8) ?
C42 C43 1.389(9) ?
C43 C44 1.367(9) ?
C44 C45 1.374(9) ?
C45 C46 1.399(9) ?
C51 C52 1.389(9) ?
C51 C56 1.394(9) ?
C52 C53 1.391(9) ?
C53 C54 1.364(12) ?
C54 C55 1.374(12) ?
C55 C56 1.399(10) ?
C61 C66 1.389(9) ?
C61 C62 1.393(9) ?
C62 C63 1.379(9) ?
C63 C64 1.374(10) ?
C64 C65 1.361(11) ?
C65 C66 1.403(9) ?
