#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/31/7013153.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_7013153
loop_
_publ_author_name
'Yip, Ka-Lai'
'Yu, Wing-Yiu'
'Chan, Pui-Ming'
'Zhu, Nian-Yong'
'Che, Chi-Ming'
_publ_section_title
;
 Nitrido-ruthenium(vi) and -osmium(vi) complexes of multianionic
 chelating (N, O) ligands. Reactions with nucleophiles, electrophiles
 and oxidizing agentsElectronic supplementary information (ESI)
 available: Fig. S1?S6. See http://www.rsc.org/suppdata/dt/b3/b304920p/
;
_journal_issue                   18
_journal_name_full               'Dalton Transactions'
_journal_page_first              3556
_journal_paper_doi               10.1039/b304920p
_journal_year                    2003
_chemical_formula_moiety         'C36 H46 Cl2 N4 O7 Os'
_chemical_formula_sum            'C36 H46 Cl2 N4 O7 Os'
_chemical_formula_weight         907.87
_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                 99.81(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.732(3)
_cell_length_b                   18.256(4)
_cell_length_c                   15.546(3)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    301(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     3840.3(14)
_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 (Sheldrick, 1997)'
_diffrn_ambient_temperature      301(2)
_diffrn_measured_fraction_theta_full 0.735
_diffrn_measured_fraction_theta_max 0.735
_diffrn_measurement_device_type  'Marresearch IPDS mar300'
_diffrn_measurement_method       Oscillation
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0545
_diffrn_reflns_av_sigmaI/netI    0.0941
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12707
_diffrn_reflns_theta_full        23.74
_diffrn_reflns_theta_max         23.74
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    3.511
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.654
_refine_diff_density_min         -0.975
_refine_diff_density_rms         0.243
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         4308
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.0864
_refine_ls_R_factor_gt           0.0393
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0720P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0974
_refine_ls_wR_factor_ref         0.1397
_reflns_number_gt                2536
_reflns_number_total             4308
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b304920p.txt
_cod_data_source_block           mar341
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7013153
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 0.54121(4) 0.09388(3) 0.14584(3) 0.0880(3) Uani 1 1 d . . .
Cl1 Cl 0.5596(3) 0.46709(19) 0.1108(3) 0.1252(12) Uani 1 1 d . . .
Cl2 Cl 0.7821(3) 0.42002(18) 0.1361(3) 0.1296(14) Uani 1 1 d . . .
O1 O 0.4181(6) 0.0369(4) 0.1007(5) 0.093(2) Uani 1 1 d . . .
O2 O 0.6031(6) -0.0014(4) 0.1181(5) 0.092(2) Uani 1 1 d . . .
O3 O 0.3402(7) 0.2637(5) 0.1259(7) 0.136(4) Uani 1 1 d . . .
O4 O 0.8088(8) 0.1608(5) 0.0846(7) 0.132(4) Uani 1 1 d . . .
O5 O 0.9378(8) 0.0653(6) 0.1741(6) 0.132(3) Uani 1 1 d . . .
O6 O 0.6593(8) -0.1366(5) 0.1215(6) 0.132(3) Uani 1 1 d . . .
O7 O 0.5353(5) 0.0990(3) 0.9777(4) 0.085(2) Uani 1 1 d . . .
N1 N 0.5502(8) 0.0887(5) 0.2513(6) 0.107(3) Uani 1 1 d . . .
N2 N 0.4753(9) 0.1893(5) 0.1195(5) 0.082(3) Uani 1 1 d . . .
N3 N 0.6510(10) 0.1502(5) 0.1358(5) 0.098(4) Uani 1 1 d . . .
N4 N 0.6228(8) 0.2904(6) 0.8351(7) 0.100(3) Uani 1 1 d . . .
C1 C 0.3241(10) 0.0660(10) 0.0937(7) 0.098(4) Uani 1 1 d . . .
C2 C 0.3004(13) 0.1398(8) 0.0983(7) 0.091(4) Uani 1 1 d . . .
C3 C 0.2002(12) 0.1601(10) 0.0830(8) 0.115(5) Uani 1 1 d . . .
H3 H 0.1848 0.2097 0.0809 0.138 Uiso 1 1 calc R . .
C4 C 0.1227(15) 0.1101(9) 0.0708(10) 0.126(6) Uani 1 1 d . . .
H4 H 0.0570 0.1249 0.0637 0.151 Uiso 1 1 calc R . .
C5 C 0.1494(11) 0.0357(12) 0.0700(8) 0.127(6) Uani 1 1 d . . .
H5 H 0.0992 0.0009 0.0623 0.152 Uiso 1 1 calc R . .
C6 C 0.2482(12) 0.0110(8) 0.0800(7) 0.104(4) Uani 1 1 d . . .
H6 H 0.2634 -0.0385 0.0779 0.125 Uiso 1 1 calc R . .
C7 C 0.3731(13) 0.2028(9) 0.1164(8) 0.103(4) Uani 1 1 d . . .
C8 C 0.5422(11) 0.2486(7) 0.1233(7) 0.086(4) Uani 1 1 d . . .
C9 C 0.6412(10) 0.2269(7) 0.1281(6) 0.074(3) Uani 1 1 d . . .
C10 C 0.7129(9) 0.2802(8) 0.1326(7) 0.090(3) Uani 1 1 d . . .
H10 H 0.7788 0.2662 0.1380 0.108 Uiso 1 1 calc R . .
C11 C 0.6892(11) 0.3547(8) 0.1295(7) 0.095(4) Uani 1 1 d . . .
C12 C 0.5902(13) 0.3752(7) 0.1203(8) 0.098(4) Uani 1 1 d . . .
C13 C 0.5183(9) 0.3226(8) 0.1194(7) 0.091(4) Uani 1 1 d . . .
H13 H 0.4527 0.3367 0.1161 0.109 Uiso 1 1 calc R . .
C14 C 0.7016(10) -0.0093(7) 0.1315(7) 0.083(3) Uani 1 1 d . . .
C15 C 0.7691(10) 0.0450(8) 0.1368(7) 0.091(4) Uani 1 1 d . . .
C16 C 0.8708(11) 0.0208(9) 0.1562(8) 0.096(4) Uani 1 1 d . . .
C17 C 0.8994(12) -0.0565(9) 0.1631(8) 0.112(4) Uani 1 1 d . . .
H17 H 0.9660 -0.0690 0.1738 0.134 Uiso 1 1 calc R . .
C18 C 0.8304(12) -0.1099(8) 0.1540(8) 0.104(4) Uani 1 1 d . . .
H18 H 0.8493 -0.1588 0.1594 0.125 Uiso 1 1 calc R . .
C19 C 0.7275(12) -0.0904(8) 0.1359(8) 0.099(4) Uani 1 1 d . . .
C20 C 0.7444(16) 0.1260(7) 0.1175(9) 0.110(6) Uani 1 1 d . . .
C24 C 0.7158(11) 0.2582(8) 0.8910(9) 0.125(5) Uani 1 1 d . . .
H24A H 0.7028 0.2077 0.9044 0.151 Uiso 1 1 calc R . .
H24B H 0.7292 0.2849 0.9457 0.151 Uiso 1 1 calc R . .
C25 C 0.8087(12) 0.2608(11) 0.8476(12) 0.187(8) Uani 1 1 d . . .
H25A H 0.8164 0.3092 0.8237 0.224 Uiso 1 1 calc R . .
H25B H 0.8035 0.2253 0.8006 0.224 Uiso 1 1 calc R . .
C26 C 0.8979(16) 0.2426(18) 0.9193(18) 0.291(18) Uani 1 1 d . . .
H26A H 0.8968 0.2738 0.9697 0.349 Uiso 1 1 calc R . .
H26B H 0.8936 0.1921 0.9376 0.349 Uiso 1 1 calc R . .
C27 C 0.981(2) 0.253(2) 0.8894(19) 0.37(2) Uani 1 1 d . . .
H27A H 1.0358 0.2436 0.9352 0.551 Uiso 1 1 calc R . .
H27B H 0.9837 0.3023 0.8694 0.551 Uiso 1 1 calc R . .
H27C H 0.9835 0.2196 0.8419 0.551 Uiso 1 1 calc R . .
C28 C 0.6424(9) 0.3679(8) 0.8099(9) 0.106(4) Uani 1 1 d . . .
H28A H 0.5829 0.3864 0.7736 0.127 Uiso 1 1 calc R . .
H28B H 0.6937 0.3667 0.7741 0.127 Uiso 1 1 calc R . .
C29 C 0.6731(11) 0.4224(8) 0.8829(9) 0.118(5) Uani 1 1 d . . .
H29A H 0.7316 0.4041 0.9208 0.141 Uiso 1 1 calc R . .
H29B H 0.6207 0.4264 0.9174 0.141 Uiso 1 1 calc R . .
C30 C 0.6950(11) 0.4979(9) 0.8501(10) 0.143(6) Uani 1 1 d . . .
H30A H 0.7458 0.4936 0.8140 0.171 Uiso 1 1 calc R . .
H30B H 0.6359 0.5167 0.8137 0.171 Uiso 1 1 calc R . .
C31 C 0.7280(13) 0.5507(10) 0.9207(11) 0.176(7) Uani 1 1 d . . .
H31A H 0.7407 0.5972 0.8960 0.264 Uiso 1 1 calc R . .
H31B H 0.7875 0.5330 0.9563 0.264 Uiso 1 1 calc R . .
H31C H 0.6775 0.5562 0.9559 0.264 Uiso 1 1 calc R . .
C32 C 0.5435(10) 0.2871(7) 0.8893(8) 0.103(4) Uani 1 1 d . . .
H32A H 0.5627 0.3177 0.9404 0.123 Uiso 1 1 calc R . .
H32B H 0.5387 0.2371 0.9095 0.123 Uiso 1 1 calc R . .
C33 C 0.4419(10) 0.3112(8) 0.8434(7) 0.106(4) Uani 1 1 d . . .
H33A H 0.4482 0.3571 0.8133 0.128 Uiso 1 1 calc R . .
H33B H 0.4160 0.2749 0.7999 0.128 Uiso 1 1 calc R . .
C34 C 0.3694(10) 0.3212(7) 0.9060(8) 0.106(4) Uani 1 1 d . . .
H34A H 0.3672 0.2762 0.9389 0.127 Uiso 1 1 calc R . .
H34B H 0.3939 0.3596 0.9472 0.127 Uiso 1 1 calc R . .
C35 C 0.2675(10) 0.3401(9) 0.8641(9) 0.136(5) Uani 1 1 d . . .
H35A H 0.2266 0.3454 0.9081 0.204 Uiso 1 1 calc R . .
H35B H 0.2415 0.3019 0.8244 0.204 Uiso 1 1 calc R . .
H35C H 0.2682 0.3853 0.8327 0.204 Uiso 1 1 calc R . .
C36 C 0.5964(11) 0.2505(8) 0.7506(9) 0.115(4) Uani 1 1 d . . .
H36A H 0.5399 0.2746 0.7162 0.138 Uiso 1 1 calc R . .
H36B H 0.6512 0.2548 0.7189 0.138 Uiso 1 1 calc R . .
C37 C 0.5730(12) 0.1726(10) 0.7580(10) 0.142(6) Uani 1 1 d . . .
H37A H 0.5162 0.1670 0.7869 0.170 Uiso 1 1 calc R . .
H37B H 0.6285 0.1473 0.7922 0.170 Uiso 1 1 calc R . .
C38 C 0.5499(15) 0.1393(9) 0.6637(16) 0.195(10) Uani 1 1 d . . .
H38A H 0.4907 0.1616 0.6314 0.234 Uiso 1 1 calc R . .
H38B H 0.6043 0.1493 0.6328 0.234 Uiso 1 1 calc R . .
C39 C 0.5365(13) 0.0640(15) 0.6693(13) 0.223(10) Uani 1 1 d . . .
H39A H 0.5215 0.0436 0.6117 0.334 Uiso 1 1 calc R . .
H39B H 0.4829 0.0544 0.7001 0.334 Uiso 1 1 calc R . .
H39C H 0.5959 0.0420 0.7001 0.334 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
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'
O O 0.0106 0.0060 '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'
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'
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
N1 Os1 N3 101.2(4) . . ?
N1 Os1 N2 102.3(4) . . ?
N3 Os1 N2 81.0(5) . . ?
N1 Os1 O1 103.7(4) . . ?
N3 Os1 O1 155.1(3) . . ?
N2 Os1 O1 93.2(4) . . ?
N1 Os1 O2 101.7(4) . . ?
N3 Os1 O2 94.7(4) . . ?
N2 Os1 O2 155.9(3) . . ?
O1 Os1 O2 80.7(3) . . ?
C1 O1 Os1 123.1(8) . . ?
C14 O2 Os1 120.7(7) . . ?
C8 N2 C7 120.1(11) . . ?
C8 N2 Os1 113.3(9) . . ?
C7 N2 Os1 125.2(9) . . ?
C9 N3 C20 111.6(11) . . ?
C9 N3 Os1 119.4(9) . . ?
C20 N3 Os1 127.9(9) . . ?
C32 N4 C36 112.9(10) . . ?
C32 N4 C28 111.5(10) . . ?
C36 N4 C28 105.0(10) . . ?
C32 N4 C24 106.4(10) . . ?
C36 N4 C24 111.4(11) . . ?
C28 N4 C24 109.8(11) . . ?
O1 C1 C2 126.3(14) . . ?
O1 C1 C6 112.7(15) . . ?
C2 C1 C6 121.0(13) . . ?
C1 C2 C3 118.5(13) . . ?
C1 C2 C7 126.2(15) . . ?
C3 C2 C7 115.2(14) . . ?
C4 C3 C2 123.7(16) . . ?
C3 C4 C5 116.1(17) . . ?
C4 C5 C6 123.6(16) . . ?
C5 C6 C1 116.9(14) . . ?
O3 C7 N2 122.7(13) . . ?
O3 C7 C2 117.9(15) . . ?
N2 C7 C2 119.4(14) . . ?
C13 C8 C9 119.8(13) . . ?
C13 C8 N2 126.5(13) . . ?
C9 C8 N2 113.7(11) . . ?
C10 C9 C8 118.7(12) . . ?
C10 C9 N3 129.8(13) . . ?
C8 C9 N3 111.3(11) . . ?
C9 C10 C11 121.7(12) . . ?
C12 C11 C10 118.8(12) . . ?
C12 C11 Cl2 121.1(12) . . ?
C10 C11 Cl2 120.1(12) . . ?
C13 C12 C11 120.0(12) . . ?
C13 C12 Cl1 120.9(13) . . ?
C11 C12 Cl1 119.1(13) . . ?
C12 C13 C8 120.9(13) . . ?
O2 C14 C15 126.5(12) . . ?
O2 C14 C19 109.5(12) . . ?
C15 C14 C19 124.0(12) . . ?
C14 C15 C16 114.7(13) . . ?
C14 C15 C20 124.6(13) . . ?
C16 C15 C20 120.6(13) . . ?
O5 C16 C15 120.4(14) . . ?
O5 C16 C17 116.3(14) . . ?
C15 C16 C17 123.2(14) . . ?
C18 C17 C16 120.9(14) . . ?
C17 C18 C19 119.4(13) . . ?
O6 C19 C18 123.2(14) . . ?
O6 C19 C14 119.1(14) . . ?
C18 C19 C14 117.6(13) . . ?
O4 C20 N3 129.5(13) . . ?
O4 C20 C15 114.6(17) . . ?
N3 C20 C15 115.8(14) . . ?
N4 C24 C25 114.3(12) . . ?
C24 C25 C26 106.9(14) . . ?
C27 C26 C25 110(2) . . ?
N4 C28 C29 117.6(11) . . ?
C28 C29 C30 113.0(12) . . ?
C31 C30 C29 113.4(15) . . ?
N4 C32 C33 115.1(10) . . ?
C34 C33 C32 112.5(10) . . ?
C35 C34 C33 114.9(11) . . ?
C37 C36 N4 115.4(12) . . ?
C36 C37 C38 108.4(13) . . ?
C39 C38 C37 109.4(19) . . ?
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 N1 1.625(9) . ?
Os1 N3 1.854(13) . ?
Os1 N2 1.974(9) . ?
Os1 O1 2.007(7) . ?
Os1 O2 2.014(8) . ?
Cl1 C12 1.730(14) . ?
Cl2 C11 1.737(12) . ?
O1 C1 1.384(14) . ?
O2 C14 1.341(12) . ?
O3 C7 1.218(15) . ?
O4 C20 1.266(17) . ?
O5 C16 1.223(13) . ?
O6 C19 1.252(14) . ?
N2 C8 1.415(14) . ?
N2 C7 1.417(16) . ?
N3 C9 1.409(14) . ?
N3 C20 1.430(19) . ?
N4 C32 1.488(14) . ?
N4 C36 1.490(14) . ?
N4 C28 1.505(14) . ?
N4 C24 1.534(15) . ?
C1 C2 1.390(18) . ?
C1 C6 1.437(16) . ?
C2 C3 1.406(16) . ?
C2 C7 1.518(18) . ?
C3 C4 1.390(18) . ?
C4 C5 1.41(2) . ?
C5 C6 1.413(17) . ?
C8 C13 1.389(15) . ?
C8 C9 1.405(15) . ?
C9 C10 1.378(15) . ?
C10 C11 1.398(15) . ?
C11 C12 1.394(16) . ?
C12 C13 1.375(16) . ?
C14 C15 1.350(15) . ?
C14 C19 1.522(16) . ?
C15 C16 1.446(16) . ?
C15 C20 1.535(19) . ?
C16 C17 1.463(17) . ?
C17 C18 1.350(17) . ?
C18 C19 1.438(18) . ?
C24 C25 1.542(19) . ?
C25 C26 1.55(3) . ?
C26 C27 1.31(2) . ?
C28 C29 1.514(17) . ?
C29 C30 1.518(17) . ?
C30 C31 1.473(18) . ?
C32 C33 1.520(15) . ?
C33 C34 1.518(14) . ?
C34 C35 1.480(15) . ?
C36 C37 1.467(17) . ?
C37 C38 1.57(2) . ?
C38 C39 1.39(3) . ?
