#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:56:43 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179085 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/47/4304730.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_4304730
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'
_chemical_formula_sum            'C34 H26 N8 Os'
_chemical_formula_weight         736.83
_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                 90.453(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.3341(10)
_cell_length_b                   16.0851(15)
_cell_length_c                   16.7074(16)
_cell_measurement_reflns_used    18226
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.4
_cell_measurement_theta_min      2.3
_cell_volume                     2777.1(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 0.973
_diffrn_measured_fraction_theta_max 0.973
_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  0.0484
_diffrn_reflns_av_sigmaI/netI    0.0610
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18226
_diffrn_reflns_theta_full        28.35
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    4.633
_exptl_absorpt_correction_T_max  0.543
_exptl_absorpt_correction_T_min  0.455
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.762
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Square
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.800
_refine_diff_density_min         -1.019
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         6757
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0373
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0384P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0776
_refine_ls_wR_factor_ref         0.0817
_reflns_number_gt                5520
_reflns_number_total             6757
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic702301a-file004.cif
_cod_data_source_block           30mayfm
_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 2.4.1 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_database_code               4304730
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 0.424655(15) 0.282106(10) 0.109518(10) 0.01113(6) Uani 1 1 d . . .
N3 N 0.2711(3) 0.2180(2) 0.1409(2) 0.0108(7) Uani 1 1 d . . .
N1 N 0.2768(3) 0.3667(2) 0.1042(2) 0.0132(8) Uani 1 1 d . . .
N7 N 0.5546(3) 0.3646(2) 0.0797(2) 0.0132(7) Uani 1 1 d . . .
N8 N 0.4964(3) 0.3149(2) 0.2189(2) 0.0129(7) Uani 1 1 d . . .
N5 N 0.4409(3) 0.2691(2) -0.0125(2) 0.0125(7) Uani 1 1 d . . .
C7 C 0.1895(4) 0.0812(3) 0.1861(3) 0.0158(9) Uani 1 1 d . . .
H7 H 0.1063 0.1015 0.1939 0.019 Uiso 1 1 calc R . .
N2 N 0.1542(3) 0.2520(2) 0.1489(2) 0.0140(8) Uani 1 1 d . . .
C13 C 0.6463(4) 0.0779(3) 0.0359(3) 0.0188(10) Uani 1 1 d . . .
H13 H 0.5752 0.0492 0.0155 0.023 Uiso 1 1 calc R . .
C2 C 0.1759(4) 0.4980(3) 0.0836(3) 0.0210(10) Uani 1 1 d . . .
H2 H 0.1823 0.5532 0.0675 0.025 Uiso 1 1 calc R . .
C29 C 0.4791(4) 0.2716(3) 0.2932(3) 0.0163(9) Uani 1 1 d . . .
C24 C 0.6884(4) 0.4816(3) 0.1300(3) 0.0188(10) Uani 1 1 d . . .
H24 H 0.7085 0.5006 0.0791 0.023 Uiso 1 1 calc R . .
N4 N 0.5023(3) 0.1636(2) 0.1188(2) 0.0145(8) Uani 1 1 d . . .
C30 C 0.3585(4) 0.2696(3) 0.3286(3) 0.0172(10) Uani 1 1 d . . .
H30 H 0.2868 0.2917 0.3021 0.021 Uiso 1 1 calc R . .
C21 C 0.5349(4) 0.3325(3) -0.1289(3) 0.0186(10) Uani 1 1 d . . .
H21 H 0.5820 0.3756 -0.1518 0.022 Uiso 1 1 calc R . .
C14 C 0.7691(5) 0.0568(3) 0.0111(3) 0.0232(11) Uani 1 1 d . . .
H14 H 0.7803 0.0136 -0.0251 0.028 Uiso 1 1 calc R . .
C3 C 0.0572(4) 0.4666(3) 0.1087(3) 0.0205(10) Uani 1 1 d . . .
H3 H -0.0154 0.5007 0.1102 0.025 Uiso 1 1 calc R . .
C20 C 0.4837(5) 0.2709(3) -0.1763(3) 0.0244(11) Uani 1 1 d . . .
H20 H 0.4956 0.2721 -0.2314 0.029 Uiso 1 1 calc R . .
C11 C 0.4161(4) 0.1055(3) 0.1458(2) 0.0117(8) Uani 1 1 d . . .
C8 C 0.2171(4) 0.0000(3) 0.2014(3) 0.0181(10) Uani 1 1 d . . .
H8 H 0.1527 -0.0358 0.2192 0.022 Uiso 1 1 calc R . .
C17 C 0.7358(4) 0.1861(3) 0.1183(3) 0.0165(9) Uani 1 1 d . . .
H17 H 0.7254 0.2303 0.1535 0.020 Uiso 1 1 calc R . .
C18 C 0.3935(4) 0.2082(3) -0.0607(3) 0.0175(10) Uani 1 1 d . . .
H18 H 0.3450 0.1658 -0.0377 0.021 Uiso 1 1 calc R . .
C6 C 0.2870(4) 0.1340(3) 0.1586(3) 0.0130(9) Uani 1 1 d . . .
N6 N 0.5760(3) 0.3860(2) 0.0034(2) 0.0168(8) Uani 1 1 d . . .
C12 C 0.6274(4) 0.1415(3) 0.0913(3) 0.0140(9) Uani 1 1 d . . .
C19 C 0.4137(4) 0.2064(3) -0.1413(3) 0.0202(10) Uani 1 1 d . . .
H19 H 0.3814 0.1630 -0.1723 0.024 Uiso 1 1 calc R . .
C4 C 0.0489(4) 0.3851(3) 0.1310(3) 0.0182(10) Uani 1 1 d . . .
H4 H -0.0295 0.3632 0.1480 0.022 Uiso 1 1 calc R . .
C10 C 0.4416(4) 0.0213(3) 0.1625(3) 0.0152(9) Uani 1 1 d . . .
H10 H 0.5242 -0.0002 0.1550 0.018 Uiso 1 1 calc R . .
C27 C 0.6285(4) 0.4245(3) 0.2848(3) 0.0161(9) Uani 1 1 d . . .
H27 H 0.6108 0.4058 0.3363 0.019 Uiso 1 1 calc R . .
C23 C 0.6102(4) 0.4117(3) 0.1400(3) 0.0140(9) Uani 1 1 d . . .
C9 C 0.3437(5) -0.0292(3) 0.1900(3) 0.0206(10) Uani 1 1 d . . .
H9 H 0.3622 -0.0846 0.2014 0.025 Uiso 1 1 calc R . .
C32 C 0.4500(5) 0.1989(3) 0.4424(3) 0.0250(12) Uani 1 1 d . . .
H32 H 0.4401 0.1754 0.4928 0.030 Uiso 1 1 calc R . .
C5 C 0.1608(4) 0.3338(3) 0.1282(2) 0.0140(9) Uani 1 1 d . . .
C15 C 0.8763(5) 0.1001(3) 0.0401(3) 0.0231(11) Uani 1 1 d . . .
H15 H 0.9593 0.0856 0.0242 0.028 Uiso 1 1 calc R . .
C1 C 0.2830(4) 0.4482(3) 0.0826(3) 0.0184(10) Uani 1 1 d . . .
H1 H 0.3618 0.4704 0.0667 0.022 Uiso 1 1 calc R . .
C31 C 0.3455(5) 0.2343(3) 0.4038(3) 0.0245(11) Uani 1 1 d . . .
H31 H 0.2652 0.2346 0.4286 0.029 Uiso 1 1 calc R . .
C26 C 0.7034(4) 0.4933(3) 0.2738(3) 0.0193(10) Uani 1 1 d . . .
H26 H 0.7342 0.5220 0.3183 0.023 Uiso 1 1 calc R . .
C25 C 0.7354(4) 0.5222(3) 0.1972(3) 0.0211(10) Uani 1 1 d . . .
H25 H 0.7882 0.5686 0.1916 0.025 Uiso 1 1 calc R . .
C34 C 0.5844(5) 0.2351(3) 0.3312(3) 0.0231(11) Uani 1 1 d . . .
H34 H 0.6650 0.2350 0.3069 0.028 Uiso 1 1 calc R . .
C16 C 0.8574(4) 0.1646(3) 0.0927(3) 0.0190(10) Uani 1 1 d . . .
H16 H 0.9286 0.1944 0.1114 0.023 Uiso 1 1 calc R . .
C33 C 0.5686(5) 0.1983(3) 0.4063(3) 0.0252(12) Uani 1 1 d . . .
H33 H 0.6388 0.1733 0.4319 0.030 Uiso 1 1 calc R . .
C28 C 0.5775(4) 0.3813(2) 0.2171(3) 0.0123(9) Uani 1 1 d . . .
C22 C 0.5159(4) 0.3303(3) -0.0461(3) 0.0172(9) 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'
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
N7 Os1 N3 168.73(14) . . ?
N7 Os1 N8 78.86(14) . . ?
N3 Os1 N8 100.68(14) . . ?
N7 Os1 N1 92.96(15) . . ?
N3 Os1 N1 75.89(14) . . ?
N8 Os1 N1 97.64(14) . . ?
N7 Os1 N5 75.81(14) . . ?
N3 Os1 N5 106.46(14) . . ?
N8 Os1 N5 152.07(14) . . ?
N1 Os1 N5 95.24(14) . . ?
N7 Os1 N4 112.14(14) . . ?
N3 Os1 N4 79.11(14) . . ?
N8 Os1 N4 91.87(14) . . ?
N1 Os1 N4 154.49(14) . . ?
N5 Os1 N4 86.93(14) . . ?
N2 N3 C6 118.8(3) . . ?
N2 N3 Os1 123.1(3) . . ?
C6 N3 Os1 118.1(3) . . ?
C1 N1 C5 119.4(4) . . ?
C1 N1 Os1 128.0(3) . . ?
C5 N1 Os1 112.6(3) . . ?
N6 N7 C23 118.9(4) . . ?
N6 N7 Os1 122.3(3) . . ?
C23 N7 Os1 117.9(3) . . ?
C28 N8 C29 118.7(3) . . ?
C28 N8 Os1 113.8(3) . . ?
C29 N8 Os1 127.2(3) . . ?
C18 N5 C22 118.5(4) . . ?
C18 N5 Os1 128.9(3) . . ?
C22 N5 Os1 112.5(3) . . ?
C8 C7 C6 119.7(4) . . ?
N3 N2 C5 108.9(3) . . ?
C14 C13 C12 120.8(4) . . ?
C1 C2 C3 120.4(4) . . ?
C30 C29 C34 120.1(4) . . ?
C30 C29 N8 119.9(4) . . ?
C34 C29 N8 120.0(4) . . ?
C25 C24 C23 118.9(4) . . ?
C11 N4 C12 122.1(4) . . ?
C11 N4 Os1 113.6(3) . . ?
C12 N4 Os1 123.9(3) . . ?
C31 C30 C29 119.4(4) . . ?
C20 C21 C22 119.7(4) . . ?
C13 C14 C15 120.3(4) . . ?
C4 C3 C2 119.1(4) . . ?
C21 C20 C19 119.6(5) . . ?
N4 C11 C10 126.9(4) . . ?
N4 C11 C6 116.1(4) . . ?
C10 C11 C6 116.9(4) . . ?
C7 C8 C9 119.3(4) . . ?
C16 C17 C12 120.0(4) . . ?
N5 C18 C19 122.9(4) . . ?
N3 C6 C7 125.1(4) . . ?
N3 C6 C11 112.9(4) . . ?
C7 C6 C11 122.0(4) . . ?
N7 N6 C22 109.3(4) . . ?
C13 C12 C17 118.3(4) . . ?
C13 C12 N4 122.1(4) . . ?
C17 C12 N4 119.6(4) . . ?
C18 C19 C20 118.8(4) . . ?
C3 C4 C5 119.7(4) . . ?
C9 C10 C11 119.7(4) . . ?
C26 C27 C28 119.6(4) . . ?
N7 C23 C24 126.3(4) . . ?
N7 C23 C28 111.9(4) . . ?
C24 C23 C28 121.8(4) . . ?
C10 C9 C8 122.4(4) . . ?
C33 C32 C31 119.9(5) . . ?
N2 C5 N1 119.5(4) . . ?
N2 C5 C4 120.7(4) . . ?
N1 C5 C4 119.9(4) . . ?
C16 C15 C14 118.9(4) . . ?
N1 C1 C2 121.5(4) . . ?
C32 C31 C30 120.8(5) . . ?
C27 C26 C25 122.0(4) . . ?
C24 C25 C26 120.0(4) . . ?
C29 C34 C33 119.6(5) . . ?
C17 C16 C15 121.6(4) . . ?
C32 C33 C34 120.2(5) . . ?
N8 C28 C23 116.2(4) . . ?
N8 C28 C27 126.1(4) . . ?
C23 C28 C27 117.6(4) . . ?
N6 C22 N5 118.5(4) . . ?
N6 C22 C21 121.0(4) . . ?
N5 C22 C21 120.4(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 N7 1.956(3) . ?
Os1 N3 1.967(3) . ?
Os1 N8 2.035(3) . ?
Os1 N1 2.047(3) . ?
Os1 N5 2.058(4) . ?
Os1 N4 2.074(3) . ?
N3 N2 1.333(5) . ?
N3 C6 1.394(5) . ?
N1 C1 1.361(5) . ?
N1 C5 1.373(5) . ?
N7 N6 1.341(5) . ?
N7 C23 1.381(5) . ?
N8 C28 1.359(5) . ?
N8 C29 1.436(5) . ?
N5 C18 1.357(5) . ?
N5 C22 1.375(6) . ?
C7 C8 1.361(6) . ?
C7 C6 1.398(6) . ?
N2 C5 1.361(6) . ?
C13 C14 1.381(6) . ?
C13 C12 1.394(6) . ?
C2 C1 1.367(6) . ?
C2 C3 1.394(6) . ?
C29 C30 1.384(6) . ?
C29 C34 1.386(6) . ?
C24 C25 1.382(6) . ?
C24 C23 1.396(6) . ?
N4 C11 1.370(5) . ?
N4 C12 1.421(5) . ?
C30 C31 1.387(6) . ?
C21 C20 1.372(6) . ?
C21 C22 1.400(6) . ?
C14 C15 1.392(6) . ?
C3 C4 1.366(6) . ?
C20 C19 1.395(7) . ?
C11 C10 1.407(6) . ?
C11 C6 1.429(6) . ?
C8 C9 1.405(6) . ?
C17 C16 1.375(6) . ?
C17 C12 1.402(6) . ?
C18 C19 1.366(6) . ?
N6 C22 1.366(5) . ?
C4 C5 1.422(6) . ?
C10 C9 1.379(6) . ?
C27 C26 1.364(6) . ?
C27 C28 1.426(6) . ?
C23 C28 1.420(6) . ?
C32 C33 1.370(7) . ?
C32 C31 1.376(7) . ?
C15 C16 1.374(6) . ?
C26 C25 1.403(6) . ?
C34 C33 1.397(7) . ?
