#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:45:02 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179126 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/88/4308865.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_4308865
loop_
_publ_author_name
'Jing Zhang'
'Jiang-Lin Liang'
'Xian-Ru Sun'
'Hai-Bing Zhou'
'Nian-Yong Zhu'
'Zhong-Yuan Zhou'
'Philip Wai Hong Chan'
'Chi-Ming Che'
_publ_section_title
;
Chiral Osmium Complexes with Sterically Bulky Schiff-Base Ligands. Crystal
Structures of Os(IV) Derivatives and the Reactivity and Catalytic
Cyclopropanation of Alkenes with EDA
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3942
_journal_page_last               3954
_journal_paper_doi               10.1021/ic0481935
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C36 H52 Cl2 N2 O2 Os'
_chemical_formula_weight         805.90
_chemical_name_systematic
; 
 ? 
;
_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_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                69.723(2)
_cell_angle_beta                 81.066(2)
_cell_angle_gamma                71.178(2)
_cell_formula_units_Z            2
_cell_length_a                   12.1571(11)
_cell_length_b                   13.3553(12)
_cell_length_c                   13.3721(12)
_cell_measurement_reflns_used    CCD
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     1925.4(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        Shelxtl
_computing_molecular_graphics    Shelxtl
_computing_publication_material  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 0.983
_diffrn_measured_fraction_theta_max 0.983
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_sigmaI/netI    0.0585
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13050
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    3.481
_exptl_absorpt_correction_T_max  0.6801
_exptl_absorpt_correction_T_min  0.5428
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PRISM
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.059
_refine_diff_density_min         -0.933
_refine_diff_density_rms         0.177
_refine_ls_extinction_coef       0.0036(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.812
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         8735
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.812
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0445
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1095
_refine_ls_wR_factor_ref         0.1183
_reflns_number_gt                7327
_reflns_number_total             8735
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0481935si20041222_032230.cif
_cod_data_source_block           sxr6
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 
;
_cod_original_sg_symbol_H-M      'P 1'
_cod_database_code               4308865
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Os1 Os 0.285209(10) 0.359930(10) 0.598913(9) 0.02960(3) Uani 1 1 d . . .
Cl1 Cl 0.33366(8) 0.43612(8) 0.71430(7) 0.0436(2) Uani 1 1 d . . .
Cl2 Cl 0.23525(8) 0.28177(7) 0.48613(7) 0.0436(2) Uani 1 1 d . . .
O1 O 0.19077(19) 0.28652(19) 0.71851(17) 0.0343(6) Uani 1 1 d . . .
O2 O 0.4289(2) 0.2360(2) 0.63058(18) 0.0389(7) Uani 1 1 d . . .
N1 N 0.1500(2) 0.4954(2) 0.5555(2) 0.0325(7) Uani 1 1 d . . .
N2 N 0.3654(2) 0.4477(2) 0.4740(2) 0.0313(7) Uani 1 1 d . . .
C1 C 0.2967(3) 0.5676(3) 0.4348(3) 0.0354(8) Uani 1 1 d . . .
H1A H 0.3073 0.6037 0.4837 0.042 Uiso 1 1 calc R . .
C2 C 0.3307(3) 0.6326(3) 0.3230(3) 0.0448(10) Uani 1 1 d . . .
H2A H 0.3272 0.5956 0.2732 0.054 Uiso 1 1 calc R . .
H2B H 0.4098 0.6353 0.3207 0.054 Uiso 1 1 calc R . .
C3 C 0.2477(4) 0.7514(3) 0.2908(4) 0.0541(12) Uani 1 1 d . . .
H3A H 0.2594 0.7910 0.3350 0.065 Uiso 1 1 calc R . .
H3B H 0.2663 0.7902 0.2172 0.065 Uiso 1 1 calc R . .
C4 C 0.1227(3) 0.7534(3) 0.3020(3) 0.0477(11) Uani 1 1 d . . .
H4A H 0.1088 0.7219 0.2515 0.057 Uiso 1 1 calc R . .
H4B H 0.0741 0.8301 0.2848 0.057 Uiso 1 1 calc R . .
C5 C 0.0887(3) 0.6880(3) 0.4146(3) 0.0420(10) Uani 1 1 d . . .
H5A H 0.0940 0.7241 0.4646 0.050 Uiso 1 1 calc R . .
H5B H 0.0089 0.6869 0.4174 0.050 Uiso 1 1 calc R . .
C6 C 0.1681(3) 0.5703(3) 0.4458(3) 0.0326(8) Uani 1 1 d . . .
H6A H 0.1576 0.5358 0.3955 0.039 Uiso 1 1 calc R . .
C7 C 0.0571(3) 0.5198(3) 0.6163(3) 0.0341(8) Uani 1 1 d . . .
H7A H 0.0015 0.5879 0.5893 0.041 Uiso 1 1 calc R . .
C9 C -0.0677(3) 0.4989(3) 0.7767(3) 0.0425(10) Uani 1 1 d . . .
H9A H -0.1126 0.5713 0.7437 0.051 Uiso 1 1 calc R . .
C8 C 0.0338(3) 0.4505(3) 0.7211(3) 0.0337(8) Uani 1 1 d . . .
C10 C -0.1010(3) 0.4422(3) 0.8771(3) 0.0429(10) Uani 1 1 d . . .
C11 C -0.0296(3) 0.3332(3) 0.9247(3) 0.0445(10) Uani 1 1 d . . .
H11A H -0.0510 0.2948 0.9937 0.053 Uiso 1 1 calc R . .
C12 C 0.0695(3) 0.2793(3) 0.8766(3) 0.0356(8) Uani 1 1 d . . .
C13 C 0.1013(3) 0.3386(3) 0.7702(2) 0.0329(8) Uani 1 1 d . . .
C14 C -0.2086(4) 0.4928(4) 0.9391(3) 0.0617(14) Uani 1 1 d . . .
C15 C -0.1740(6) 0.4905(6) 1.0442(4) 0.111(2) Uani 1 1 d . . .
H15A H -0.1241 0.5372 1.0305 0.167 Uiso 1 1 calc R . .
H15B H -0.1335 0.4154 1.0836 0.167 Uiso 1 1 calc R . .
H15C H -0.2426 0.5174 1.0849 0.167 Uiso 1 1 calc R . .
C16 C -0.2742(7) 0.6064(6) 0.8755(6) 0.170(4) Uani 1 1 d . . .
H16A H -0.2253 0.6547 0.8565 0.255 Uiso 1 1 calc R . .
H16B H -0.3414 0.6346 0.9170 0.255 Uiso 1 1 calc R . .
H16C H -0.2985 0.6035 0.8119 0.255 Uiso 1 1 calc R . .
C17 C -0.2915(5) 0.4172(6) 0.9683(5) 0.101(2) Uani 1 1 d . . .
H17A H -0.3178 0.4175 0.9040 0.152 Uiso 1 1 calc R . .
H17B H -0.3573 0.4453 1.0111 0.152 Uiso 1 1 calc R . .
H17C H -0.2503 0.3423 1.0076 0.152 Uiso 1 1 calc R . .
C18 C 0.1452(4) 0.1616(3) 0.9336(3) 0.0462(10) Uani 1 1 d . . .
C19 C 0.0990(5) 0.1156(4) 1.0491(3) 0.0706(17) Uani 1 1 d . . .
H19A H 0.0212 0.1127 1.0486 0.106 Uiso 1 1 calc R . .
H19B H 0.0988 0.1634 1.0887 0.106 Uiso 1 1 calc R . .
H19C H 0.1482 0.0419 1.0820 0.106 Uiso 1 1 calc R . .
C20 C 0.1469(5) 0.0800(3) 0.8750(4) 0.0636(14) Uani 1 1 d . . .
H20A H 0.1753 0.1062 0.8025 0.095 Uiso 1 1 calc R . .
H20B H 0.0694 0.0756 0.8759 0.095 Uiso 1 1 calc R . .
H20C H 0.1968 0.0075 0.9101 0.095 Uiso 1 1 calc R . .
C21 C 0.2687(4) 0.1641(4) 0.9390(4) 0.0641(15) Uani 1 1 d . . .
H21A H 0.3003 0.1923 0.8680 0.096 Uiso 1 1 calc R . .
H21B H 0.3163 0.0899 0.9729 0.096 Uiso 1 1 calc R . .
H21C H 0.2673 0.2115 0.9794 0.096 Uiso 1 1 calc R . .
C22 C 0.4646(3) 0.4071(3) 0.4287(3) 0.0366(9) Uani 1 1 d . . .
H22A H 0.4907 0.4553 0.3679 0.044 Uiso 1 1 calc R . .
C23 C 0.5367(3) 0.2942(3) 0.4651(3) 0.0338(8) Uani 1 1 d . . .
C24 C 0.6350(3) 0.2670(3) 0.3974(3) 0.0412(9) Uani 1 1 d . . .
H24A H 0.6476 0.3214 0.3346 0.049 Uiso 1 1 calc R . .
C25 C 0.7129(3) 0.1615(3) 0.4223(3) 0.0436(9) Uani 1 1 d . . .
C26 C 0.6905(3) 0.0819(3) 0.5164(3) 0.0453(10) Uani 1 1 d . . .
H26A H 0.7416 0.0101 0.5328 0.054 Uiso 1 1 calc R . .
C27 C 0.5972(3) 0.1034(3) 0.5867(3) 0.0389(9) Uani 1 1 d . . .
C28 C 0.5181(3) 0.2118(3) 0.5611(3) 0.0338(8) Uani 1 1 d . . .
C29 C 0.8197(4) 0.1352(4) 0.3452(3) 0.0526(11) Uani 1 1 d . . .
C30 C 0.8997(4) 0.2034(5) 0.3395(5) 0.1104(19) Uani 1 1 d . . .
H30A H 0.9653 0.1868 0.2915 0.166 Uiso 1 1 calc R . .
H30B H 0.9264 0.1855 0.4093 0.166 Uiso 1 1 calc R . .
H30C H 0.8584 0.2813 0.3141 0.166 Uiso 1 1 calc R . .
C31 C 0.7764(5) 0.1687(5) 0.2324(4) 0.0888(18) Uani 1 1 d . . .
H31A H 0.8416 0.1524 0.1840 0.133 Uiso 1 1 calc R . .
H31B H 0.7366 0.2471 0.2089 0.133 Uiso 1 1 calc R . .
H31C H 0.7241 0.1274 0.2342 0.133 Uiso 1 1 calc R . .
C32 C 0.8827(6) 0.0118(5) 0.3772(6) 0.125(3) Uani 1 1 d . . .
H32A H 0.9476 -0.0020 0.3278 0.187 Uiso 1 1 calc R . .
H32B H 0.8304 -0.0285 0.3764 0.187 Uiso 1 1 calc R . .
H32C H 0.9100 -0.0125 0.4478 0.187 Uiso 1 1 calc R . .
C33 C 0.5758(4) 0.0113(3) 0.6889(3) 0.0491(11) Uani 1 1 d . . .
C34 C 0.6727(6) -0.0978(4) 0.7035(5) 0.105(3) Uani 1 1 d . . .
H34A H 0.7453 -0.0861 0.7082 0.157 Uiso 1 1 calc R . .
H34B H 0.6774 -0.1233 0.6437 0.157 Uiso 1 1 calc R . .
H34C H 0.6565 -0.1528 0.7679 0.157 Uiso 1 1 calc R . .
C35 C 0.4603(5) -0.0094(5) 0.6848(5) 0.0889(18) Uani 1 1 d . . .
H35A H 0.3984 0.0588 0.6764 0.133 Uiso 1 1 calc R . .
H35B H 0.4461 -0.0646 0.7500 0.133 Uiso 1 1 calc R . .
H35C H 0.4638 -0.0355 0.6256 0.133 Uiso 1 1 calc R . .
C36 C 0.5711(4) 0.0434(4) 0.7896(3) 0.0640(14) Uani 1 1 d . . .
H36A H 0.6435 0.0555 0.7943 0.096 Uiso 1 1 calc R . .
H36B H 0.5580 -0.0157 0.8515 0.096 Uiso 1 1 calc R . .
H36C H 0.5088 0.1106 0.7858 0.096 Uiso 1 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'
N N 0.0061 0.0033 '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'
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
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Os1 O1 95.15(9) . . ?
O2 Os1 N1 173.71(10) . . ?
O1 Os1 N1 91.04(10) . . ?
O2 Os1 N2 90.92(10) . . ?
O1 Os1 N2 173.93(9) . . ?
N1 Os1 N2 82.90(10) . . ?
O2 Os1 Cl2 89.67(9) . . ?
O1 Os1 Cl2 90.74(8) . . ?
N1 Os1 Cl2 91.36(9) . . ?
N2 Os1 Cl2 89.22(9) . . ?
O2 Os1 Cl1 90.26(9) . . ?
O1 Os1 Cl1 88.26(8) . . ?
N1 Os1 Cl1 88.81(9) . . ?
N2 Os1 Cl1 91.79(9) . . ?
Cl2 Os1 Cl1 178.99(3) . . ?
C13 O1 Os1 125.4(2) . . ?
C28 O2 Os1 126.72(19) . . ?
C7 N1 C6 122.8(3) . . ?
C7 N1 Os1 124.7(2) . . ?
C6 N1 Os1 112.43(19) . . ?
C22 N2 C1 122.6(3) . . ?
C22 N2 Os1 125.3(2) . . ?
C1 N2 Os1 112.14(19) . . ?
N2 C1 C2 115.7(3) . . ?
N2 C1 C6 106.6(3) . . ?
C2 C1 C6 111.8(3) . . ?
C1 C2 C3 109.9(3) . . ?
C4 C3 C2 112.6(4) . . ?
C3 C4 C5 112.1(3) . . ?
C6 C5 C4 110.2(3) . . ?
N1 C6 C5 117.4(3) . . ?
N1 C6 C1 105.9(2) . . ?
C5 C6 C1 111.7(3) . . ?
N1 C7 C8 125.4(3) . . ?
C10 C9 C8 121.9(3) . . ?
C9 C8 C13 119.3(3) . . ?
C9 C8 C7 115.5(3) . . ?
C13 C8 C7 125.2(3) . . ?
C9 C10 C11 117.2(3) . . ?
C9 C10 C14 122.9(3) . . ?
C11 C10 C14 119.9(3) . . ?
C12 C11 C10 124.9(3) . . ?
C11 C12 C13 117.2(3) . . ?
C11 C12 C18 122.5(3) . . ?
C13 C12 C18 120.3(3) . . ?
O1 C13 C8 121.7(3) . . ?
O1 C13 C12 118.9(3) . . ?
C8 C13 C12 119.4(3) . . ?
C16 C14 C15 112.1(6) . . ?
C16 C14 C10 112.2(4) . . ?
C15 C14 C10 109.9(4) . . ?
C16 C14 C17 107.7(5) . . ?
C15 C14 C17 106.2(5) . . ?
C10 C14 C17 108.5(4) . . ?
C21 C18 C12 109.8(4) . . ?
C21 C18 C20 110.1(4) . . ?
C12 C18 C20 110.6(3) . . ?
C21 C18 C19 107.3(4) . . ?
C12 C18 C19 111.9(3) . . ?
C20 C18 C19 107.2(4) . . ?
N2 C22 C23 125.1(3) . . ?
C24 C23 C28 119.3(3) . . ?
C24 C23 C22 114.8(3) . . ?
C28 C23 C22 125.9(3) . . ?
C25 C24 C23 121.4(3) . . ?
C24 C25 C26 117.6(3) . . ?
C24 C25 C29 119.7(3) . . ?
C26 C25 C29 122.7(3) . . ?
C27 C26 C25 123.8(3) . . ?
C26 C27 C28 118.2(3) . . ?
C26 C27 C33 121.5(3) . . ?
C28 C27 C33 120.2(3) . . ?
O2 C28 C27 119.3(3) . . ?
O2 C28 C23 121.1(3) . . ?
C27 C28 C23 119.6(3) . . ?
C32 C29 C30 111.8(5) . . ?
C32 C29 C31 107.0(5) . . ?
C30 C29 C31 107.8(4) . . ?
C32 C29 C25 111.4(4) . . ?
C30 C29 C25 110.0(4) . . ?
C31 C29 C25 108.6(4) . . ?
C34 C33 C35 108.8(5) . . ?
C34 C33 C36 106.0(4) . . ?
C35 C33 C36 108.2(4) . . ?
C34 C33 C27 111.9(4) . . ?
C35 C33 C27 110.1(4) . . ?
C36 C33 C27 111.7(4) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Os1 O2 1.962(2) . ?
Os1 O1 1.976(2) . ?
Os1 N1 1.991(3) . ?
Os1 N2 1.997(3) . ?
Os1 Cl2 2.3490(10) . ?
Os1 Cl1 2.3495(10) . ?
O1 C13 1.325(4) . ?
O2 C28 1.347(4) . ?
N1 C7 1.305(4) . ?
N1 C6 1.492(4) . ?
N2 C22 1.302(4) . ?
N2 C1 1.492(4) . ?
C1 C2 1.516(5) . ?
C1 C6 1.538(5) . ?
C2 C3 1.532(5) . ?
C3 C4 1.496(6) . ?
C4 C5 1.526(5) . ?
C5 C6 1.505(5) . ?
C7 C8 1.432(4) . ?
C9 C10 1.365(5) . ?
C9 C8 1.424(5) . ?
C8 C13 1.426(4) . ?
C10 C11 1.411(5) . ?
C10 C14 1.528(5) . ?
C11 C12 1.380(5) . ?
C12 C13 1.431(4) . ?
C12 C18 1.534(5) . ?
C14 C16 1.483(8) . ?
C14 C15 1.515(8) . ?
C14 C17 1.565(9) . ?
C18 C21 1.527(7) . ?
C18 C20 1.541(7) . ?
C18 C19 1.541(5) . ?
C22 C23 1.432(5) . ?
C23 C24 1.412(5) . ?
C23 C28 1.414(5) . ?
C24 C25 1.380(5) . ?
C25 C26 1.393(5) . ?
C25 C29 1.553(5) . ?
C26 C27 1.379(5) . ?
C27 C28 1.413(5) . ?
C27 C33 1.542(5) . ?
C29 C32 1.511(7) . ?
C29 C30 1.511(8) . ?
C29 C31 1.542(7) . ?
C33 C34 1.522(6) . ?
C33 C35 1.528(7) . ?
C33 C36 1.537(7) . ?
