#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:45:02 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179126 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/88/4308866.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_4308866
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_moiety         'C36 H52 Cl N2 O3 Os'
_chemical_formula_sum            'C36 H52 Cl N2 O3 Os'
_chemical_formula_weight         786.45
_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                 94.43(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.688(2)
_cell_length_b                   11.9410(10)
_cell_length_c                   20.078(2)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    301(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     4467.1(8)
_computing_cell_refinement       Scalepack
_computing_data_collection       MarControl
_computing_data_reduction        Denzo
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    Shelxs-97
_diffrn_ambient_temperature      301(2)
_diffrn_measured_fraction_theta_full 0.890
_diffrn_measured_fraction_theta_max 0.890
_diffrn_measurement_device_type  'Marreasearch Imaging Plate mar300'
_diffrn_measurement_method       Oscillation
_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  0.0527
_diffrn_reflns_av_sigmaI/netI    0.0703
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22173
_diffrn_reflns_theta_full        25.57
_diffrn_reflns_theta_max         25.57
_diffrn_reflns_theta_min         1.43
_exptl_absorpt_coefficient_mu    2.943
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1596
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.308
_refine_diff_density_min         -1.290
_refine_diff_density_rms         0.298
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         7467
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.1022
_refine_ls_R_factor_gt           0.0593
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1246P)²+1.7274P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2019
_refine_ls_wR_factor_ref         0.2265
_reflns_number_gt                4241
_reflns_number_total             7467
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0481935si20041222_032247.cif
_cod_data_source_block           mar51
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4308866
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Os1 Os 0.47146(2) 0.25006(3) 0.082019(18) 0.0661(2) Uani 1 1 d D . .
N1 N 0.4557(4) 0.3387(6) -0.0020(4) 0.068(2) Uani 1 1 d . . .
N2 N 0.5342(4) 0.1590(6) 0.0279(4) 0.070(2) Uani 1 1 d . . .
Cl1 Cl 0.5733(4) 0.3517(8) 0.1196(6) 0.069(2) Uani 0.50 1 d PD . .
Cl2 Cl 0.3698(6) 0.1496(8) 0.0491(8) 0.081(3) Uani 0.50 1 d PD . .
O3 O 0.4063(4) 0.3468(5) 0.1313(3) 0.0781(18) Uani 1 1 d . . .
O4 O 0.4930(3) 0.1560(5) 0.1623(3) 0.0783(19) Uani 1 1 d . . .
C1 C 0.3582(5) 0.4196(7) 0.1043(5) 0.063(2) Uani 1 1 d . . .
C2 C 0.3060(5) 0.4618(7) 0.1450(5) 0.064(2) Uani 1 1 d . . .
C3 C 0.2579(5) 0.5382(8) 0.1171(5) 0.073(3) Uani 1 1 d . . .
H3 H 0.2229 0.5652 0.1434 0.087 Uiso 1 1 calc R . .
C4 C 0.2582(6) 0.5778(9) 0.0521(5) 0.080(3) Uani 1 1 d . . .
C5 C 0.3093(5) 0.5364(7) 0.0137(5) 0.070(3) Uani 1 1 d . . .
H5 H 0.3109 0.5630 -0.0297 0.084 Uiso 1 1 calc R . .
C6 C 0.3602(5) 0.4546(7) 0.0374(5) 0.062(2) Uani 1 1 d . . .
C7 C 0.4092(5) 0.4173(7) -0.0101(5) 0.070(2) Uani 1 1 d . . .
H7 H 0.4068 0.4543 -0.0509 0.084 Uiso 1 1 calc R . .
C8 C 0.3040(5) 0.4184(8) 0.2159(5) 0.071(3) Uani 1 1 d . . .
C9 C 0.3732(6) 0.4478(9) 0.2571(5) 0.095(3) Uani 1 1 d . . .
H9A H 0.3713 0.4192 0.3016 0.142 Uiso 1 1 calc R . .
H9B H 0.3787 0.5278 0.2588 0.142 Uiso 1 1 calc R . .
H9C H 0.4131 0.4151 0.2370 0.142 Uiso 1 1 calc R . .
C10 C 0.2941(7) 0.2881(9) 0.2187(6) 0.092(3) Uani 1 1 d . . .
H10A H 0.2929 0.2647 0.2643 0.139 Uiso 1 1 calc R . .
H10B H 0.3334 0.2522 0.1992 0.139 Uiso 1 1 calc R . .
H10C H 0.2498 0.2677 0.1942 0.139 Uiso 1 1 calc R . .
C11 C 0.2399(6) 0.4758(10) 0.2496(5) 0.112(4) Uani 1 1 d . . .
H11A H 0.2380 0.4478 0.2943 0.167 Uiso 1 1 calc R . .
H11B H 0.1956 0.4590 0.2241 0.167 Uiso 1 1 calc R . .
H11C H 0.2470 0.5554 0.2509 0.167 Uiso 1 1 calc R . .
C12 C 0.2030(6) 0.6695(10) 0.0258(6) 0.092(3) Uani 1 1 d . . .
C13 C 0.1305(8) 0.6034(13) 0.0137(9) 0.174(7) Uani 1 1 d . . .
H13A H 0.1363 0.5442 -0.0178 0.261 Uiso 1 1 calc R . .
H13B H 0.0935 0.6534 -0.0037 0.261 Uiso 1 1 calc R . .
H13C H 0.1175 0.5721 0.0551 0.261 Uiso 1 1 calc R . .
C14 C 0.2011(9) 0.7657(11) 0.0749(9) 0.135(6) Uani 1 1 d . . .
H14A H 0.1907 0.7374 0.1178 0.203 Uiso 1 1 calc R . .
H14B H 0.1646 0.8181 0.0593 0.203 Uiso 1 1 calc R . .
H14C H 0.2469 0.8026 0.0786 0.203 Uiso 1 1 calc R . .
C15 C 0.2199(12) 0.7121(17) -0.0422(9) 0.219(12) Uani 1 1 d . . .
H15A H 0.2211 0.6503 -0.0727 0.328 Uiso 1 1 calc R . .
H15B H 0.2657 0.7489 -0.0386 0.328 Uiso 1 1 calc R . .
H15C H 0.1835 0.7642 -0.0584 0.328 Uiso 1 1 calc R . .
C16 C 0.5076(6) 0.3077(9) -0.0515(5) 0.084(3) Uani 1 1 d . . .
C17 C 0.4869(7) 0.3424(8) -0.1215(5) 0.088(3) Uani 1 1 d . . .
H17A H 0.4811 0.4231 -0.1236 0.105 Uiso 1 1 calc R . .
H17B H 0.4414 0.3083 -0.1367 0.105 Uiso 1 1 calc R . .
C18 C 0.5454(8) 0.3056(11) -0.1670(7) 0.114(5) Uani 1 1 d . . .
H18A H 0.5292 0.3215 -0.2131 0.136 Uiso 1 1 calc R . .
H18B H 0.5885 0.3490 -0.1559 0.136 Uiso 1 1 calc R . .
C19 C 0.5622(8) 0.1887(11) -0.1606(6) 0.111(4) Uani 1 1 d . . .
H19A H 0.6041 0.1736 -0.1849 0.133 Uiso 1 1 calc R . .
H19B H 0.5226 0.1461 -0.1818 0.133 Uiso 1 1 calc R . .
C20 C 0.5769(7) 0.1468(8) -0.0901(6) 0.096(4) Uani 1 1 d . . .
H20A H 0.6238 0.1728 -0.0725 0.116 Uiso 1 1 calc R . .
H20B H 0.5776 0.0656 -0.0903 0.116 Uiso 1 1 calc R . .
C21 C 0.5205(7) 0.1872(9) -0.0453(6) 0.093(4) Uani 1 1 d . . .
C22 C 0.5789(5) 0.0829(8) 0.0509(6) 0.078(3) Uani 1 1 d . . .
H22 H 0.6062 0.0461 0.0209 0.094 Uiso 1 1 calc R . .
C23 C 0.5885(5) 0.0524(8) 0.1193(6) 0.075(3) Uani 1 1 d . . .
C24 C 0.6464(6) -0.0287(9) 0.1345(7) 0.100(4) Uani 1 1 d . . .
H24 H 0.6718 -0.0559 0.0999 0.120 Uiso 1 1 calc R . .
C25 C 0.6642(6) -0.0656(11) 0.1982(7) 0.102(4) Uani 1 1 d . . .
C26 C 0.6240(6) -0.0224(9) 0.2484(6) 0.096(4) Uani 1 1 d . . .
H26 H 0.6364 -0.0464 0.2918 0.115 Uiso 1 1 calc R . .
C27 C 0.5685(5) 0.0513(8) 0.2396(5) 0.072(3) Uani 1 1 d . . .
C28 C 0.5489(5) 0.0898(8) 0.1717(6) 0.076(3) Uani 1 1 d . . .
C29 C 0.7228(9) -0.1524(15) 0.2144(9) 0.137(6) Uani 1 1 d . . .
C30 C 0.7424(11) -0.2153(18) 0.1560(10) 0.213(12) Uani 1 1 d . . .
H30A H 0.7787 -0.2693 0.1696 0.319 Uiso 1 1 calc R . .
H30B H 0.7606 -0.1647 0.1242 0.319 Uiso 1 1 calc R . .
H30C H 0.7008 -0.2531 0.1360 0.319 Uiso 1 1 calc R . .
C31 C 0.7809(10) -0.1010(19) 0.2603(14) 0.303(18) Uani 1 1 d . . .
H31A H 0.7599 -0.0657 0.2971 0.455 Uiso 1 1 calc R . .
H31B H 0.8063 -0.0461 0.2364 0.455 Uiso 1 1 calc R . .
H31C H 0.8137 -0.1582 0.2769 0.455 Uiso 1 1 calc R . .
C32 C 0.6979(16) -0.2504(15) 0.2589(14) 0.237(15) Uani 1 1 d . . .
H32A H 0.6828 -0.2206 0.2999 0.355 Uiso 1 1 calc R . .
H32B H 0.7370 -0.3014 0.2685 0.355 Uiso 1 1 calc R . .
H32C H 0.6586 -0.2892 0.2355 0.355 Uiso 1 1 calc R . .
C33 C 0.5249(5) 0.0945(9) 0.2973(5) 0.079(3) Uani 1 1 d . . .
C34 C 0.5552(7) 0.0490(11) 0.3656(6) 0.119(4) Uani 1 1 d . . .
H34A H 0.6043 0.0719 0.3739 0.179 Uiso 1 1 calc R . .
H34B H 0.5525 -0.0313 0.3655 0.179 Uiso 1 1 calc R . .
H34C H 0.5276 0.0781 0.4001 0.179 Uiso 1 1 calc R . .
C35 C 0.4493(5) 0.0566(9) 0.2876(5) 0.087(3) Uani 1 1 d . . .
H35A H 0.4480 -0.0236 0.2842 0.130 Uiso 1 1 calc R . .
H35B H 0.4271 0.0888 0.2474 0.130 Uiso 1 1 calc R . .
H35C H 0.4239 0.0800 0.3250 0.130 Uiso 1 1 calc R . .
C36 C 0.5296(7) 0.2208(10) 0.3027(7) 0.105(4) Uani 1 1 d . . .
H36A H 0.5791 0.2429 0.3090 0.157 Uiso 1 1 calc R . .
H36B H 0.5047 0.2455 0.3400 0.157 Uiso 1 1 calc R . .
H36C H 0.5081 0.2540 0.2624 0.157 Uiso 1 1 calc R . .
O2 O 0.5479(9) 0.359(2) 0.1078(16) 0.072(7) Uani 0.50 1 d PD . .
O1 O 0.3964(13) 0.143(3) 0.056(2) 0.095(10) Uani 0.50 1 d PD . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Os Os -1.2165 7.6030 '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'
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'
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Os1 O2 179.5(16) . . ?
O1 Os1 O4 86.8(11) . . ?
O2 Os1 O4 93.6(9) . . ?
O1 Os1 N2 86.3(12) . . ?
O2 Os1 N2 93.4(9) . . ?
O4 Os1 N2 92.5(3) . . ?
O1 Os1 N1 93.7(12) . . ?
O2 Os1 N1 85.9(9) . . ?
O4 Os1 N1 175.6(3) . . ?
N2 Os1 N1 83.2(3) . . ?
O1 Os1 O3 93.4(11) . . ?
O2 Os1 O3 86.9(8) . . ?
O4 Os1 O3 91.0(3) . . ?
N2 Os1 O3 176.4(3) . . ?
N1 Os1 O3 93.3(3) . . ?
O1 Os1 Cl2 9.9(11) . . ?
O2 Os1 Cl2 170.1(7) . . ?
O4 Os1 Cl2 92.9(4) . . ?
N2 Os1 Cl2 93.8(4) . . ?
N1 Os1 Cl2 88.2(4) . . ?
O3 Os1 Cl2 85.5(4) . . ?
O1 Os1 Cl1 170.1(9) . . ?
O2 Os1 Cl1 10.1(8) . . ?
O4 Os1 Cl1 85.5(3) . . ?
N2 Os1 Cl1 87.8(3) . . ?
N1 Os1 Cl1 93.5(4) . . ?
O3 Os1 Cl1 93.0(3) . . ?
Cl2 Os1 Cl1 177.8(5) . . ?
C7 N1 C16 124.7(8) . . ?
C7 N1 Os1 123.3(7) . . ?
C16 N1 Os1 111.8(6) . . ?
C22 N2 C21 124.1(9) . . ?
C22 N2 Os1 125.5(8) . . ?
C21 N2 Os1 110.4(6) . . ?
O2 Cl1 Os1 41(4) . . ?
O1 Cl2 Os1 40(4) . . ?
C1 O3 Os1 126.4(6) . . ?
C28 O4 Os1 124.7(7) . . ?
O3 C1 C6 120.9(9) . . ?
O3 C1 C2 118.1(9) . . ?
C6 C1 C2 121.1(8) . . ?
C3 C2 C1 117.5(9) . . ?
C3 C2 C8 123.2(8) . . ?
C1 C2 C8 119.3(8) . . ?
C2 C3 C4 124.1(9) . . ?
C5 C4 C3 117.4(9) . . ?
C5 C4 C12 122.2(9) . . ?
C3 C4 C12 120.3(9) . . ?
C4 C5 C6 122.7(9) . . ?
C1 C6 C5 117.2(9) . . ?
C1 C6 C7 127.1(8) . . ?
C5 C6 C7 115.8(9) . . ?
N1 C7 C6 127.1(9) . . ?
C2 C8 C9 110.5(8) . . ?
C2 C8 C10 112.5(8) . . ?
C9 C8 C10 108.0(8) . . ?
C2 C8 C11 109.2(7) . . ?
C9 C8 C11 108.0(9) . . ?
C10 C8 C11 108.7(9) . . ?
C15 C12 C14 110.4(13) . . ?
C15 C12 C4 111.2(10) . . ?
C14 C12 C4 111.0(10) . . ?
C15 C12 C13 105.4(14) . . ?
C14 C12 C13 114.8(12) . . ?
C4 C12 C13 103.8(10) . . ?
C21 C16 N1 107.5(8) . . ?
C21 C16 C17 112.5(9) . . ?
N1 C16 C17 115.2(8) . . ?
C16 C17 C18 109.6(10) . . ?
C19 C18 C17 112.7(10) . . ?
C18 C19 C20 115.5(10) . . ?
C19 C20 C21 111.6(10) . . ?
C16 C21 N2 108.5(9) . . ?
C16 C21 C20 112.3(9) . . ?
N2 C21 C20 115.7(10) . . ?
N2 C22 C23 123.8(10) . . ?
C28 C23 C22 127.4(9) . . ?
C28 C23 C24 118.5(11) . . ?
C22 C23 C24 114.1(10) . . ?
C25 C24 C23 122.0(12) . . ?
C24 C25 C26 116.6(10) . . ?
C24 C25 C29 122.5(13) . . ?
C26 C25 C29 120.8(12) . . ?
C27 C26 C25 126.2(11) . . ?
C26 C27 C28 117.3(10) . . ?
C26 C27 C33 123.8(9) . . ?
C28 C27 C33 118.9(8) . . ?
O4 C28 C23 122.9(10) . . ?
O4 C28 C27 117.7(10) . . ?
C23 C28 C27 119.4(9) . . ?
C30 C29 C31 119.3(16) . . ?
C30 C29 C25 113.5(14) . . ?
C31 C29 C25 109.1(14) . . ?
C30 C29 C32 100.2(16) . . ?
C31 C29 C32 100.9(18) . . ?
C25 C29 C32 112.9(15) . . ?
C35 C33 C36 111.3(9) . . ?
C35 C33 C34 106.8(9) . . ?
C36 C33 C34 105.8(10) . . ?
C35 C33 C27 110.5(9) . . ?
C36 C33 C27 110.7(9) . . ?
C34 C33 C27 111.7(9) . . ?
Cl1 O2 Os1 129(4) . . ?
Cl2 O1 Os1 130(5) . . ?
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 O1 1.94(2) . ?
Os1 O2 1.97(2) . ?
Os1 O4 1.980(6) . ?
Os1 N2 1.983(8) . ?
Os1 N1 1.994(8) . ?
Os1 O3 1.996(6) . ?
Os1 Cl2 2.301(10) . ?
Os1 Cl1 2.333(8) . ?
N1 C7 1.281(11) . ?
N1 C16 1.487(12) . ?
N2 C22 1.296(11) . ?
N2 C21 1.509(14) . ?
Cl1 O2 0.521(19) . ?
Cl2 O1 0.51(3) . ?
O3 C1 1.335(10) . ?
O4 C28 1.312(11) . ?
C1 C6 1.411(12) . ?
C1 C2 1.412(12) . ?
C2 C3 1.370(12) . ?
C2 C8 1.519(12) . ?
C3 C4 1.389(13) . ?
C4 C5 1.366(12) . ?
C4 C12 1.567(13) . ?
C5 C6 1.419(12) . ?
C6 C7 1.442(12) . ?
C8 C9 1.520(13) . ?
C8 C10 1.568(13) . ?
C8 C11 1.577(13) . ?
C12 C15 1.513(19) . ?
C12 C14 1.516(17) . ?
C12 C13 1.570(19) . ?
C16 C21 1.462(16) . ?
C16 C17 1.489(14) . ?
C17 C18 1.542(15) . ?
C18 C19 1.434(19) . ?
C19 C20 1.505(16) . ?
C20 C21 1.517(15) . ?
C22 C23 1.418(14) . ?
C23 C28 1.406(14) . ?
C23 C24 1.466(13) . ?
C24 C25 1.368(16) . ?
C25 C26 1.401(16) . ?
C25 C29 1.524(16) . ?
C26 C27 1.362(13) . ?
C27 C28 1.458(14) . ?
C27 C33 1.554(14) . ?
C29 C30 1.46(2) . ?
C29 C31 1.50(2) . ?
C29 C32 1.57(3) . ?
C33 C35 1.482(13) . ?
C33 C36 1.514(14) . ?
C33 C34 1.542(14) . ?
