#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:56:43 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179085 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/47/4304731.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_4304731
loop_
_publ_author_name
'Subhas Samanta'
'Priti Singh'
'Jan Fiedler'
'Stanislav Záliš'
'Wolfgang Kaim'
'Sreebrata Goswami'
_publ_section_title
;
Singlet Diradical Complexes of Ruthenium and Osmium: Geometrical and
Electronic Structures and their Unexpected Changes on Oxidation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1625
_journal_page_last               1633
_journal_paper_doi               10.1021/ic702301a
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C34 H26 N8 Os, I3'
_chemical_formula_sum            'C34 H26 I3 N8 Os'
_chemical_formula_weight         1117.56
_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                114.751(13)
_cell_angle_beta                 103.044(9)
_cell_angle_gamma                107.607(11)
_cell_formula_units_Z            2
_cell_length_a                   12.2467(13)
_cell_length_b                   13.191(2)
_cell_length_c                   13.6083(15)
_cell_measurement_temperature    293(2)
_cell_volume                     1738.1(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ORTEP-III
_computing_publication_material  'WinGX v1.70.01'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SHELXS-97
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.881
_diffrn_measured_fraction_theta_max 0.881
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0381
_diffrn_reflns_av_sigmaI/netI    0.0612
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            23183
_diffrn_reflns_theta_full        32.74
_diffrn_reflns_theta_max         32.74
_diffrn_reflns_theta_min         3.07
_exptl_absorpt_coefficient_mu    6.368
_exptl_absorpt_correction_T_max  0.295
_exptl_absorpt_correction_T_min  0.222
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    2.136
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Square
_exptl_crystal_F_000             1142
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_refine_diff_density_max         2.654
_refine_diff_density_min         -1.477
_refine_diff_density_rms         0.214
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         11302
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0385
_refine_ls_shift/su_max          0.574
_refine_ls_shift/su_mean         0.194
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0554P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.1041
_reflns_number_gt                8324
_reflns_number_total             11302
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic702301a-file005.cif
_cod_data_source_block           gkl033
_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.

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' 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_cell_volume        1738.1(4)
_cod_database_code               4304731
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 0.777036(16) 0.916846(16) 0.609624(16) 0.01670(5) Uani 1 1 d . . .
I2 I 0.5000 0.5000 0.0000 0.02605(10) Uani 1 2 d S . .
I3 I 0.0000 0.5000 0.5000 0.02807(11) Uani 1 2 d S . .
I1 I 0.39096(3) 0.66587(3) -0.00473(3) 0.03105(9) Uani 1 1 d . . .
N3 N 0.8644(3) 1.0297(4) 0.5632(3) 0.0176(8) Uani 1 1 d . . .
N6 N 0.6431(4) 0.6914(4) 0.6077(4) 0.0223(8) Uani 1 1 d . . .
N7 N 0.6853(4) 0.8129(4) 0.6619(3) 0.0200(8) Uani 1 1 d . . .
C17 C 0.4348(4) 0.7594(5) 0.4716(5) 0.0247(10) Uani 1 1 d . . .
H17 H 0.4545 0.8267 0.5450 0.030 Uiso 1 1 calc R . .
N1 N 0.9648(3) 0.9838(4) 0.7081(3) 0.0176(8) Uani 1 1 d . . .
N8 N 0.7777(4) 1.0492(4) 0.7527(3) 0.0196(8) Uani 1 1 d . . .
N5 N 0.7604(4) 0.7404(4) 0.5030(3) 0.0191(8) Uani 1 1 d . . .
C27 C 0.7075(4) 1.0808(4) 0.9150(4) 0.0205(9) Uani 1 1 d . . .
H27 H 0.7459 1.1672 0.9512 0.025 Uiso 1 1 calc R . .
N4 N 0.6329(3) 0.8774(4) 0.4730(3) 0.0150(7) Uani 1 1 d . . .
N2 N 0.9849(4) 1.1013(4) 0.6156(4) 0.0208(8) Uani 1 1 d . . .
C6 C 0.7893(4) 1.0370(4) 0.4752(4) 0.0188(9) Uani 1 1 d . . .
C22 C 0.6844(4) 0.6522(4) 0.5177(4) 0.0204(9) Uani 1 1 d . . .
C18 C 0.8046(4) 0.7035(4) 0.4186(4) 0.0207(9) Uani 1 1 d . . .
H18 H 0.8573 0.7631 0.4092 0.025 Uiso 1 1 calc R . .
C21 C 0.6497(4) 0.5251(5) 0.4447(5) 0.0246(11) Uani 1 1 d . . .
H21 H 0.5972 0.4655 0.4542 0.029 Uiso 1 1 calc R . .
C29 C 0.8623(4) 1.1801(4) 0.8112(4) 0.0197(9) Uani 1 1 d . . .
C23 C 0.6623(5) 0.8754(4) 0.7607(4) 0.0219(10) Uani 1 1 d . . .
C28 C 0.7167(4) 1.0044(5) 0.8108(4) 0.0190(9) Uani 1 1 d . . .
C12 C 0.5152(4) 0.7681(4) 0.4153(4) 0.0207(10) Uani 1 1 d . . .
C7 C 0.8292(5) 1.1214(5) 0.4387(5) 0.0224(10) Uani 1 1 d . . .
H7 H 0.9124 1.1814 0.4755 0.027 Uiso 1 1 calc R . .
C11 C 0.6623(4) 0.9488(4) 0.4236(4) 0.0183(9) Uani 1 1 d . . .
C5 C 1.0399(4) 1.0784(4) 0.6990(4) 0.0204(9) Uani 1 1 d . . .
C8 C 0.7441(5) 1.1146(5) 0.3479(5) 0.0268(11) Uani 1 1 d . . .
H8 H 0.7690 1.1704 0.3233 0.032 Uiso 1 1 calc R . .
C24 C 0.5935(4) 0.8193(5) 0.8108(4) 0.0244(10) Uani 1 1 d . . .
H24 H 0.5563 0.7330 0.7758 0.029 Uiso 1 1 calc R . .
C10 C 0.5773(4) 0.9407(5) 0.3285(4) 0.0225(10) Uani 1 1 d . . .
H10 H 0.4940 0.8808 0.2904 0.027 Uiso 1 1 calc R . .
C4 C 1.1682(5) 1.1472(5) 0.7717(5) 0.0256(11) Uani 1 1 d . . .
H4 H 1.2186 1.2101 0.7645 0.031 Uiso 1 1 calc R . .
C20 C 0.6954(5) 0.4904(5) 0.3583(5) 0.0291(12) Uani 1 1 d . . .
H20 H 0.6736 0.4067 0.3082 0.035 Uiso 1 1 calc R . .
C19 C 0.7737(5) 0.5812(5) 0.3471(5) 0.0283(11) Uani 1 1 d . . .
H19 H 0.8058 0.5584 0.2899 0.034 Uiso 1 1 calc R . .
C1 C 1.0181(5) 0.9586(5) 0.7881(5) 0.0241(10) Uani 1 1 d . . .
H1 H 0.9679 0.8936 0.7930 0.029 Uiso 1 1 calc R . .
C25 C 0.5825(5) 0.8921(6) 0.9094(5) 0.0290(12) Uani 1 1 d . . .
H25 H 0.5375 0.8560 0.9425 0.035 Uiso 1 1 calc R . .
C3 C 1.2191(5) 1.1219(5) 0.8528(5) 0.0274(11) Uani 1 1 d . . .
H3 H 1.3041 1.1683 0.9023 0.033 Uiso 1 1 calc R . .
C26 C 0.6398(5) 1.0243(6) 0.9628(5) 0.0279(11) Uani 1 1 d . . .
H26 H 0.6319 1.0738 1.0308 0.033 Uiso 1 1 calc R . .
C9 C 0.6193(5) 1.0226(5) 0.2929(5) 0.0287(12) Uani 1 1 d . . .
H9 H 0.5629 1.0169 0.2299 0.034 Uiso 1 1 calc R . .
C16 C 0.3255(5) 0.6507(6) 0.4186(5) 0.0311(13) Uani 1 1 d . . .
H16 H 0.2703 0.6461 0.4555 0.037 Uiso 1 1 calc R . .
C34 C 0.8447(5) 1.2449(5) 0.7555(5) 0.0274(11) Uani 1 1 d . . .
H34 H 0.7728 1.2070 0.6872 0.033 Uiso 1 1 calc R . .
C30 C 0.9681(5) 1.2373(5) 0.9147(5) 0.0313(12) Uani 1 1 d . . .
H30 H 0.9792 1.1961 0.9544 0.038 Uiso 1 1 calc R . .
C15 C 0.2974(5) 0.5491(5) 0.3118(5) 0.0350(14) Uani 1 1 d . . .
H15 H 0.2253 0.4750 0.2780 0.042 Uiso 1 1 calc R . .
C2 C 1.1420(5) 1.0246(5) 0.8613(5) 0.0323(13) Uani 1 1 d . . .
H2 H 1.1755 1.0061 0.9163 0.039 Uiso 1 1 calc R . .
C14 C 0.3770(5) 0.5576(5) 0.2548(5) 0.0330(13) Uani 1 1 d . . .
H14 H 0.3575 0.4891 0.1822 0.040 Uiso 1 1 calc R . .
C13 C 0.4848(5) 0.6660(5) 0.3042(4) 0.0244(10) Uani 1 1 d . . .
H13 H 0.5368 0.6717 0.2644 0.029 Uiso 1 1 calc R . .
C33 C 0.9326(6) 1.3643(5) 0.8004(6) 0.0364(14) Uani 1 1 d . . .
H33 H 0.9188 1.4080 0.7641 0.044 Uiso 1 1 calc R . .
C32 C 1.0416(6) 1.4195(5) 0.8994(6) 0.0417(15) Uani 1 1 d . . .
H32 H 1.1039 1.4979 0.9267 0.050 Uiso 1 1 calc R . .
C31 C 1.0574(6) 1.3577(6) 0.9578(6) 0.0434(17) Uani 1 1 d . . .
H31 H 1.1288 1.3970 1.0270 0.052 Uiso 1 1 calc R . .
I4 I -0.06551(4) 0.33996(4) 0.24738(3) 0.03554(10) Uani 1 1 d . . .
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'
I I -0.4742 1.8119 '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'
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
N3 Os1 N7 175.79(16) . . ?
N3 Os1 N8 95.99(16) . . ?
N7 Os1 N8 80.22(17) . . ?
N3 Os1 N4 79.88(15) . . ?
N7 Os1 N4 99.27(15) . . ?
N8 Os1 N4 105.21(16) . . ?
N3 Os1 N1 75.59(16) . . ?
N7 Os1 N1 105.85(16) . . ?
N8 Os1 N1 86.66(16) . . ?
N4 Os1 N1 153.76(15) . . ?
N3 Os1 N5 108.65(16) . . ?
N7 Os1 N5 75.36(16) . . ?
N8 Os1 N5 154.14(17) . . ?
N4 Os1 N5 87.20(15) . . ?
N1 Os1 N5 91.85(15) . . ?
I1 I2 I1 180.0 . 2_665 ?
I4 I3 I4 180.0 2_566 . ?
N2 N3 C6 120.1(4) . . ?
N2 N3 Os1 123.2(3) . . ?
C6 N3 Os1 116.6(3) . . ?
N7 N6 C22 109.1(4) . . ?
N6 N7 C23 119.8(4) . . ?
N6 N7 Os1 124.0(3) . . ?
C23 N7 Os1 116.3(3) . . ?
C16 C17 C12 120.0(5) . . ?
C1 N1 C5 118.7(4) . . ?
C1 N1 Os1 128.6(3) . . ?
C5 N1 Os1 112.1(3) . . ?
C28 N8 C29 120.5(4) . . ?
C28 N8 Os1 114.1(3) . . ?
C29 N8 Os1 123.2(3) . . ?
C18 N5 C22 119.0(4) . . ?
C18 N5 Os1 128.6(3) . . ?
C22 N5 Os1 112.1(3) . . ?
C26 C27 C28 118.7(5) . . ?
C11 N4 C12 121.4(4) . . ?
C11 N4 Os1 114.7(3) . . ?
C12 N4 Os1 122.7(3) . . ?
N3 N2 C5 110.0(4) . . ?
N3 C6 C7 126.2(4) . . ?
N3 C6 C11 112.7(4) . . ?
C7 C6 C11 121.1(4) . . ?
N5 C22 N6 118.7(4) . . ?
N5 C22 C21 121.1(5) . . ?
N6 C22 C21 120.2(4) . . ?
N5 C18 C19 121.3(5) . . ?
C20 C21 C22 118.4(5) . . ?
C30 C29 C34 119.9(5) . . ?
C30 C29 N8 120.6(5) . . ?
C34 C29 N8 119.0(4) . . ?
C28 C23 N7 112.9(4) . . ?
C28 C23 C24 121.0(5) . . ?
N7 C23 C24 126.1(5) . . ?
N8 C28 C23 116.4(4) . . ?
N8 C28 C27 124.1(4) . . ?
C23 C28 C27 119.5(4) . . ?
C17 C12 C13 119.7(4) . . ?
C17 C12 N4 120.3(4) . . ?
C13 C12 N4 119.9(4) . . ?
C8 C7 C6 119.3(5) . . ?
N4 C11 C10 125.6(4) . . ?
N4 C11 C6 115.7(4) . . ?
C10 C11 C6 118.7(4) . . ?
N2 C5 N1 118.0(4) . . ?
N2 C5 C4 121.5(5) . . ?
N1 C5 C4 120.5(5) . . ?
C7 C8 C9 119.3(5) . . ?
C25 C24 C23 119.6(5) . . ?
C9 C10 C11 118.9(4) . . ?
C3 C4 C5 119.9(5) . . ?
C19 C20 C21 119.3(5) . . ?
C18 C19 C20 120.8(5) . . ?
N1 C1 C2 122.4(5) . . ?
C24 C25 C26 120.0(5) . . ?
C4 C3 C2 119.4(5) . . ?
C27 C26 C25 121.2(5) . . ?
C10 C9 C8 122.5(5) . . ?
C15 C16 C17 120.5(5) . . ?
C33 C34 C29 120.6(5) . . ?
C29 C30 C31 118.7(6) . . ?
C16 C15 C14 119.7(5) . . ?
C1 C2 C3 119.1(5) . . ?
C13 C14 C15 120.9(5) . . ?
C14 C13 C12 119.2(5) . . ?
C34 C33 C32 120.0(6) . . ?
C31 C32 C33 119.7(6) . . ?
C32 C31 C30 121.0(6) . . ?
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 N3 1.972(4) . ?
Os1 N7 1.973(4) . ?
Os1 N8 1.995(4) . ?
Os1 N4 1.999(4) . ?
Os1 N1 2.062(4) . ?
Os1 N5 2.077(4) . ?
I2 I1 2.9020(5) . ?
I2 I1 2.9020(5) 2_665 ?
I3 I4 2.9278(7) 2_566 ?
I3 I4 2.9278(7) . ?
N3 N2 1.303(5) . ?
N3 C6 1.394(6) . ?
N6 N7 1.310(6) . ?
N6 C22 1.390(6) . ?
N7 C23 1.397(7) . ?
C17 C16 1.381(7) . ?
C17 C12 1.384(7) . ?
N1 C1 1.356(6) . ?
N1 C5 1.379(6) . ?
N8 C28 1.387(6) . ?
N8 C29 1.443(6) . ?
N5 C18 1.350(6) . ?
N5 C22 1.373(6) . ?
C27 C26 1.394(7) . ?
C27 C28 1.407(7) . ?
N4 C11 1.379(6) . ?
N4 C12 1.434(6) . ?
N2 C5 1.378(6) . ?
C6 C7 1.404(7) . ?
C6 C11 1.412(6) . ?
C22 C21 1.401(7) . ?
C18 C19 1.357(7) . ?
C21 C20 1.380(8) . ?
C29 C30 1.388(7) . ?
C29 C34 1.389(7) . ?
C23 C28 1.394(7) . ?
C23 C24 1.423(7) . ?
C12 C13 1.405(7) . ?
C7 C8 1.374(7) . ?
C11 C10 1.407(7) . ?
C5 C4 1.399(7) . ?
C8 C9 1.404(7) . ?
C24 C25 1.349(8) . ?
C10 C9 1.372(7) . ?
C4 C3 1.356(8) . ?
C20 C19 1.379(8) . ?
C1 C2 1.358(7) . ?
C25 C26 1.424(8) . ?
C3 C2 1.412(8) . ?
C16 C15 1.376(9) . ?
C34 C33 1.373(8) . ?
C30 C31 1.394(8) . ?
C15 C14 1.382(8) . ?
C14 C13 1.376(7) . ?
C33 C32 1.380(9) . ?
C32 C31 1.379(10) . ?
