#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:43:06 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178664 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/75/4077559.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_4077559
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         'C38 H30 O2 Os P2'
_chemical_formula_sum            'C38 H30 O2 Os P2'
_chemical_formula_weight         770.76
_chemical_name_systematic
; 
 ? 
;
_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'
_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                 97.35
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.35510(10)
_cell_length_b                   10.99250(10)
_cell_length_c                   17.71080(10)
_cell_measurement_reflns_used    8107
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     3157.95(4)
_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 0.927
_diffrn_measured_fraction_theta_max 0.927
_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  0.0189
_diffrn_reflns_av_sigmaI/netI    0.0216
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            18839
_diffrn_reflns_theta_full        27.06
_diffrn_reflns_theta_max         27.06
_diffrn_reflns_theta_min         1.60
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    4.172
_exptl_absorpt_correction_T_max  0.4101
_exptl_absorpt_correction_T_min  0.2861
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Irregular ragment'
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.26
_refine_diff_density_max         1.762
_refine_diff_density_min         -0.906
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         6764
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0251
_refine_ls_R_factor_gt           0.0222
_refine_ls_shift/su_max          0.182
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0230P)²+5.2423P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0545
_refine_ls_wR_factor_ref         0.0565
_reflns_number_gt                6248
_reflns_number_total             6764
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0004601.cif
_cod_data_source_block           '[5]'
_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.

'_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^)+(0.0230P)^2^+5.2423P] 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^)+(0.0230P)^2^+5.2423P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3157.92(4)
_cod_original_sg_symbol_H-M      ' P 21/n'
_cod_database_code               4077559
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_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 0.499575(6) 0.643998(10) 0.277246(6) 0.02259(4) Uani 1 d .
H1 H 0.5622(19) 0.573(3) 0.2236(18) 0.027 Uiso 1 d .
P1 P 0.39475(4) 0.61778(6) 0.17463(4) 0.02284(14) Uani 1 d .
P2 P 0.62204(4) 0.71513(7) 0.34902(4) 0.02439(14) Uani 1 d .
O1 O 0.37194(15) 0.7731(2) 0.36307(14) 0.0440(6) Uani 1 d .
O2 O 0.50560(15) 0.4042(2) 0.36553(15) 0.0447(6) Uani 1 d .
C1 C 0.42214(18) 0.7278(3) 0.33366(16) 0.0278(6) Uani 1 d .
C2 C 0.50219(17) 0.4953(3) 0.33310(18) 0.0307(6) Uani 1 d .
C11 C 0.42468(17) 0.7626(3) 0.13895(15) 0.0246(5) Uani 1 d .
C12 C 0.49380(17) 0.7885(3) 0.19365(15) 0.0246(5) Uani 1 d .
C13 C 0.53848(19) 0.8944(3) 0.18145(17) 0.0308(6) Uani 1 d .
H13A H 0.5865 0.9143 0.2152 0.037 Uiso 1 calc R
C14 C 0.5125(2) 0.9703(3) 0.11981(18) 0.0351(7) Uani 1 d .
H14A H 0.5432 1.0418 0.1125 0.042 Uiso 1 calc R
C15 C 0.4430(2) 0.9440(3) 0.06904(18) 0.0366(7) Uani 1 d .
H15A H 0.4259 0.9983 0.0283 0.044 Uiso 1 calc R
C16 C 0.39835(19) 0.8386(3) 0.07750(17) 0.0311(6) Uani 1 d .
H16A H 0.3513 0.8188 0.0425 0.037 Uiso 1 calc R
C21 C 0.39983(17) 0.5006(3) 0.10259(17) 0.0294(6) Uani 1 d .
C22 C 0.3907(2) 0.5289(4) 0.0249(2) 0.0459(8) Uani 1 d .
H22A H 0.3802 0.6103 0.0085 0.055 Uiso 1 calc R
C23 C 0.3973(3) 0.4373(4) -0.0283(2) 0.0540(10) Uani 1 d .
H23A H 0.3910 0.4567 -0.0810 0.065 Uiso 1 calc R
C24 C 0.4126(2) 0.3199(4) -0.0057(2) 0.0514(10) Uani 1 d .
H24A H 0.4176 0.2582 -0.0424 0.062 Uiso 1 calc R
C25 C 0.4207(4) 0.2916(4) 0.0695(3) 0.0748(15) Uani 1 d .
H25A H 0.4304 0.2096 0.0852 0.090 Uiso 1 calc R
C26 C 0.4149(3) 0.3819(4) 0.1242(2) 0.0607(12) Uani 1 d .
H26A H 0.4214 0.3610 0.1767 0.073 Uiso 1 calc R
C31 C 0.28754(17) 0.6186(3) 0.19250(16) 0.0259(6) Uani 1 d .
C32 C 0.23370(19) 0.7123(3) 0.1679(2) 0.0371(7) Uani 1 d .
H32A H 0.2515 0.7767 0.1381 0.045 Uiso 1 calc R
C33 C 0.1537(2) 0.7121(4) 0.1869(2) 0.0478(9) Uani 1 d .
H33A H 0.1169 0.7758 0.1692 0.057 Uiso 1 calc R
C34 C 0.1273(2) 0.6205(4) 0.2312(2) 0.0420(8) Uani 1 d .
H34A H 0.0731 0.6224 0.2451 0.050 Uiso 1 calc R
C35 C 0.1794(2) 0.5267(4) 0.2549(2) 0.0491(9) Uani 1 d .
H35A H 0.1610 0.4626 0.2845 0.059 Uiso 1 calc R
C36 C 0.2595(2) 0.5251(4) 0.2356(2) 0.0449(9) Uani 1 d .
H36A H 0.2953 0.4596 0.2520 0.054 Uiso 1 calc R
C41 C 0.66583(17) 0.6056(3) 0.42120(16) 0.0275(6) Uani 1 d .
C42 C 0.7275(2) 0.5258(3) 0.40629(19) 0.0386(7) Uani 1 d .
H42A H 0.7518 0.5338 0.3606 0.046 Uiso 1 calc R
C43 C 0.7541(2) 0.4340(4) 0.4580(2) 0.0486(9) Uani 1 d .
H43A H 0.7955 0.3788 0.4467 0.058 Uiso 1 calc R
C44 C 0.7210(2) 0.4227(4) 0.5253(2) 0.0481(9) Uani 1 d .
H44A H 0.7400 0.3608 0.5607 0.058 Uiso 1 calc R
C45 C 0.6603(2) 0.5018(4) 0.5407(2) 0.0498(9) Uani 1 d .
H45A H 0.6377 0.4948 0.5873 0.060 Uiso 1 calc R
C46 C 0.6315(2) 0.5922(3) 0.4890(2) 0.0406(8) Uani 1 d .
H46A H 0.5884 0.6448 0.4998 0.049 Uiso 1 calc R
C51 C 0.61392(18) 0.8572(3) 0.40245(17) 0.0281(6) Uani 1 d .
C52 C 0.6673(2) 0.8852(3) 0.4684(2) 0.0431(8) Uani 1 d .
H52A H 0.7075 0.8274 0.4885 0.052 Uiso 1 calc R
C53 C 0.6623(2) 0.9957(4) 0.5046(2) 0.0492(9) Uani 1 d .
H53A H 0.6992 1.0133 0.5492 0.059 Uiso 1 calc R
C54 C 0.6041(2) 1.0810(3) 0.47634(19) 0.0421(8) Uani 1 d .
H54A H 0.6015 1.1576 0.5008 0.051 Uiso 1 calc R
C55 C 0.5494(2) 1.0539(3) 0.41208(18) 0.0357(7) Uani 1 d .
H55A H 0.5087 1.1115 0.3929 0.043 Uiso 1 calc R
C56 C 0.55415(18) 0.9429(3) 0.37576(16) 0.0294(6) Uani 1 d .
H56A H 0.5161 0.9248 0.3320 0.035 Uiso 1 calc R
C61 C 0.71001(18) 0.7408(3) 0.29618(18) 0.0336(7) Uani 1 d .
C62 C 0.7756(3) 0.8138(4) 0.3246(3) 0.0722(15) Uani 1 d .
H62A H 0.7725 0.8610 0.3690 0.087 Uiso 1 calc R
C63 C 0.8459(3) 0.8187(5) 0.2884(4) 0.099(2) Uani 1 d .
H63A H 0.8913 0.8671 0.3094 0.119 Uiso 1 calc R
C64 C 0.8506(3) 0.7543(5) 0.2227(3) 0.0726(15) Uani 1 d .
H64A H 0.8986 0.7589 0.1978 0.087 Uiso 1 calc R
C65 C 0.7864(3) 0.6845(6) 0.1939(3) 0.0768(16) Uani 1 d .
H65A H 0.7894 0.6390 0.1488 0.092 Uiso 1 calc R
C66 C 0.7161(3) 0.6788(5) 0.2297(2) 0.0680(14) Uani 1 d .
H66A H 0.6708 0.6309 0.2078 0.082 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'
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
H1 Os C2 85.4(11) y
H1 Os C1 176.4(11) y
C2 Os C1 96.47(13) y
H1 Os C12 86.1(11) y
C2 Os C12 168.24(12) y
C1 Os C12 91.68(11) y
H1 Os P1 86.7(11) y
C2 Os P1 105.15(9) y
C1 Os P1 89.82(8) y
C12 Os P1 66.28(8) y
H1 Os P2 85.5(11) y
C2 Os P2 92.49(9) y
C1 Os P2 97.46(8) y
C12 Os P2 94.86(8) y
P1 Os P2 160.07(3) y
C11 P1 C31 111.53(13) y
C11 P1 C21 109.88(14) y
C31 P1 C21 104.86(13) y
C11 P1 Os 87.64(9) y
C31 P1 Os 119.21(9) y
C21 P1 Os 122.26(10) y
C41 P2 C61 101.21(14) ?
C41 P2 C51 104.25(14) ?
C61 P2 C51 104.17(14) ?
C41 P2 Os 112.72(9) ?
C61 P2 Os 116.24(11) ?
C51 P2 Os 116.46(10) ?
O1 C1 Os 174.8(3) y
O2 C2 Os 177.9(3) y
C16 C11 C12 123.4(3) y
C16 C11 P1 137.0(2) y
C12 C11 P1 99.58(19) y
C13 C12 C11 116.5(3) y
C13 C12 Os 137.3(2) y
C11 C12 Os 106.27(19) y
C14 C13 C12 120.2(3) y
C15 C14 C13 121.6(3) y
C16 C15 C14 120.2(3) y
C15 C16 C11 118.0(3) y
C26 C21 C22 118.5(3) ?
C26 C21 P1 119.9(3) ?
C22 C21 P1 121.5(3) ?
C23 C22 C21 119.8(4) ?
C24 C23 C22 120.8(4) ?
C25 C24 C23 119.7(3) ?
C24 C25 C26 120.7(4) ?
C21 C26 C25 120.5(4) ?
C32 C31 C36 118.6(3) ?
C32 C31 P1 122.4(2) ?
C36 C31 P1 118.9(2) ?
C31 C32 C33 120.1(3) ?
C34 C33 C32 120.7(3) ?
C35 C34 C33 119.8(3) ?
C34 C35 C36 120.1(3) ?
C31 C36 C35 120.7(3) ?
C42 C41 C46 118.6(3) ?
C42 C41 P2 120.7(2) ?
C46 C41 P2 120.3(2) ?
C41 C42 C43 120.4(3) ?
C44 C43 C42 120.7(3) ?
C45 C44 C43 119.3(3) ?
C44 C45 C46 120.9(3) ?
C45 C46 C41 120.1(3) ?
C56 C51 C52 118.0(3) ?
C56 C51 P2 119.5(2) ?
C52 C51 P2 122.5(2) ?
C53 C52 C51 120.9(3) ?
C52 C53 C54 120.4(3) ?
C53 C54 C55 119.5(3) ?
C56 C55 C54 120.2(3) ?
C55 C56 C51 121.0(3) ?
C66 C61 C62 117.5(3) ?
C66 C61 P2 120.5(3) ?
C62 C61 P2 121.8(3) ?
C63 C62 C61 120.3(4) ?
C64 C63 C62 120.8(5) ?
C65 C64 C63 119.2(4) ?
C64 C65 C66 120.4(5) ?
C61 C66 C65 121.7(4) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Os H1 1.68(3) y
Os C2 1.908(3) y
Os C1 1.943(3) y
Os C12 2.166(3) y
Os P1 2.3512(7) y
Os P2 2.3637(7) y
P1 C11 1.803(3) ?
P1 C31 1.821(3) ?
P1 C21 1.822(3) ?
P2 C41 1.834(3) ?
P2 C61 1.836(3) ?
P2 C51 1.840(3) ?
O1 C1 1.141(4) y
O2 C2 1.153(4) y
C11 C16 1.396(4) y
C11 C12 1.420(4) y
C12 C13 1.405(4) y
C13 C14 1.397(4) y
C14 C15 1.387(5) y
C15 C16 1.388(5) y
C21 C26 1.373(5) ?
C21 C22 1.400(5) ?
C22 C23 1.393(5) ?
C23 C24 1.365(6) ?
C24 C25 1.358(7) ?
C25 C26 1.398(6) ?
C31 C32 1.389(4) ?
C31 C36 1.392(4) ?
C32 C33 1.392(5) ?
C33 C34 1.379(5) ?
C34 C35 1.369(5) ?
C35 C36 1.396(5) ?
C41 C42 1.388(4) ?
C41 C46 1.396(4) ?
C42 C43 1.394(5) ?
C43 C44 1.375(5) ?
C44 C45 1.374(6) ?
C45 C46 1.392(5) ?
C51 C56 1.396(4) ?
C51 C52 1.399(4) ?
C52 C53 1.382(5) ?
C53 C54 1.384(5) ?
C54 C55 1.387(5) ?
C55 C56 1.386(4) ?
C61 C66 1.374(5) ?
C61 C62 1.382(5) ?
C62 C63 1.387(6) ?
C63 C64 1.373(8) ?
C64 C65 1.347(7) ?
C65 C66 1.384(5) ?
