#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:07:36 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180061 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/07/7050717.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_7050717
loop_
_publ_author_name
'Das, Chayan'
'Peng, Shie-Ming'
'Lee, Gene-Hsiang'
'Goswami, Sreebrata'
_publ_section_title
;
 Osmium(II) complexes of 2-[(arylamido)phenylazo]pyridines. New
 examples of deamination reactions---X-ray structure and redox
 propertiesElectronic supplementary information (ESI) available:
 partial energy level diagrams and molecular orbitals of 1a, 2a and 4a,
 UV-vis spectra of 4 complexes and cyclic voltammograms of 1b, 2b and
 4b. See http://www.rsc.org/suppdata/nj/b1/b108507g/
;
_journal_issue                   2
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              222
_journal_paper_doi               10.1039/b108507g
_journal_volume                  26
_journal_year                    2002
_chemical_formula_sum            'C34 H27 Br N8 Os'
_chemical_formula_weight         817.75
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 110.873(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.0940(2)
_cell_length_b                   19.9527(3)
_cell_length_c                   14.5400(3)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    150(1)
_cell_volume                     3007.28(10)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(1)
_diffrn_measurement_device       'Siemens SMART 1K CCD'
_diffrn_measurement_method       'ω 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  0.0264
_diffrn_reflns_av_sigmaI/netI    0.0249
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21518
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.81
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    5.608
_exptl_absorpt_correction_T_max  0.4929
_exptl_absorpt_correction_T_min  0.3159
_exptl_absorpt_correction_type   'empirical used sadabs'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.806
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.651
_refine_diff_density_min         -0.772
_refine_diff_density_rms         0.089
_refine_ls_extinction_coef       0.00050(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.079
_refine_ls_goodness_of_fit_obs   1.098
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         6877
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_restrained_S_obs      1.098
_refine_ls_R_factor_all          0.0282
_refine_ls_R_factor_obs          0.0227
_refine_ls_shift/esd_max         -0.004
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0214P)²+2.8083P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0499
_refine_ls_wR_factor_obs         0.0482
_reflns_number_observed          6257
_reflns_number_total             6877
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b108507g.txt
_cod_data_source_block           ic7581
_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.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0214P)^2^+2.8083P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0214P)^2^+2.8083P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3007.28(9)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7050717
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Os Os 0.767022(9) 0.366931(5) 0.776104(7) 0.01485(4) Uani 1 d . .
Br Br 1.00438(2) 0.374157(15) 0.87995(2) 0.02291(7) Uani 1 d . .
N1 N 0.7936(2) 0.40746(11) 0.6533(2) 0.0182(5) Uani 1 d . .
N2 N 0.5719(2) 0.42440(12) 0.6043(2) 0.0216(5) Uani 1 d . .
N3 N 0.5942(2) 0.38941(12) 0.6870(2) 0.0171(4) Uani 1 d . .
N4 N 0.4840(2) 0.26539(13) 0.6873(2) 0.0260(5) Uani 1 d . .
H4A H 0.5382(2) 0.27533(13) 0.6575(2) 0.031 Uiso 1 calc R .
N5 N 0.7424(2) 0.44623(11) 0.8614(2) 0.0177(5) Uani 1 d . .
N6 N 0.6864(2) 0.35569(12) 0.9442(2) 0.0196(5) Uani 1 d . .
N7 N 0.7258(2) 0.32304(11) 0.8813(2) 0.0169(4) Uani 1 d . .
N8 N 0.7976(2) 0.27017(11) 0.7468(2) 0.0202(5) Uani 1 d . .
C1 C 0.9031(3) 0.40896(15) 0.6311(2) 0.0231(6) Uani 1 d . .
H1A H 0.9805(3) 0.39124(15) 0.6773(2) 0.028 Uiso 1 calc R .
C2 C 0.9053(3) 0.4351(2) 0.5448(2) 0.0288(7) Uani 1 d . .
H2A H 0.9829(3) 0.4348(2) 0.5311(2) 0.035 Uiso 1 calc R .
C3 C 0.7926(3) 0.4622(2) 0.4768(2) 0.0311(7) Uani 1 d . .
H3A H 0.7938(3) 0.4821(2) 0.4178(2) 0.037 Uiso 1 calc R .
C4 C 0.6808(3) 0.4598(2) 0.4959(2) 0.0274(6) Uani 1 d . .
H4B H 0.6031(3) 0.4775(2) 0.4501(2) 0.033 Uiso 1 calc R .
C5 C 0.6824(3) 0.43063(14) 0.5847(2) 0.0202(6) Uani 1 d . .
C6 C 0.4817(2) 0.38370(15) 0.7144(2) 0.0204(6) Uani 1 d . .
C7 C 0.4273(3) 0.4412(2) 0.7368(2) 0.0253(6) Uani 1 d . .
H7A H 0.4623(3) 0.4839(2) 0.7319(2) 0.030 Uiso 1 calc R .
C8 C 0.3219(3) 0.4362(2) 0.7663(2) 0.0328(8) Uani 1 d . .
H8A H 0.2854(3) 0.4753(2) 0.7832(2) 0.039 Uiso 1 calc R .
C9 C 0.2705(3) 0.3737(2) 0.7709(2) 0.0345(8) Uani 1 d . .
H9A H 0.1983(3) 0.3701(2) 0.7911(2) 0.041 Uiso 1 calc R .
C10 C 0.3226(3) 0.3161(2) 0.7465(2) 0.0308(7) Uani 1 d . .
H10A H 0.2848(3) 0.2738(2) 0.7493(2) 0.037 Uiso 1 calc R .
C11 C 0.4306(3) 0.3197(2) 0.7179(2) 0.0230(6) Uani 1 d . .
C12 C 0.4642(3) 0.1966(2) 0.6970(2) 0.0250(6) Uani 1 d . .
C13 C 0.4445(3) 0.1692(2) 0.7789(2) 0.0332(7) Uani 1 d . .
H13A H 0.4385(3) 0.1976(2) 0.8296(2) 0.040 Uiso 1 calc R .
C14 C 0.4337(4) 0.0997(2) 0.7855(3) 0.0412(8) Uani 1 d . .
H14A H 0.4201(4) 0.0809(2) 0.8410(3) 0.049 Uiso 1 calc R .
C15 C 0.4426(3) 0.0584(2) 0.7130(3) 0.0367(8) Uani 1 d . .
H15A H 0.4349(3) 0.0112(2) 0.7183(3) 0.044 Uiso 1 calc R .
C16 C 0.4628(3) 0.0854(2) 0.6322(3) 0.0319(7) Uani 1 d . .
H16A H 0.4693(3) 0.0568(2) 0.5820(3) 0.038 Uiso 1 calc R .
C17 C 0.4736(3) 0.1541(2) 0.6240(2) 0.0275(6) Uani 1 d . .
H17A H 0.4876(3) 0.1723(2) 0.5683(2) 0.033 Uiso 1 calc R .
C18 C 0.7581(3) 0.51263(14) 0.8537(2) 0.0218(6) Uani 1 d . .
H18A H 0.7930(3) 0.52821(14) 0.8067(2) 0.026 Uiso 1 calc R .
C19 C 0.7255(3) 0.5588(2) 0.9111(2) 0.0272(6) Uani 1 d . .
H19A H 0.7379(3) 0.6053(2) 0.9038(2) 0.033 Uiso 1 calc R .
C20 C 0.6741(3) 0.5363(2) 0.9800(2) 0.0281(7) Uani 1 d . .
H20A H 0.6500(3) 0.5675(2) 1.0198(2) 0.034 Uiso 1 calc R .
C21 C 0.6585(3) 0.4686(2) 0.9902(2) 0.0244(6) Uani 1 d . .
H21A H 0.6236(3) 0.4526(2) 1.0371(2) 0.029 Uiso 1 calc R .
C22 C 0.6945(2) 0.42372(14) 0.9308(2) 0.0189(5) Uani 1 d . .
C23 C 0.7454(3) 0.25438(14) 0.8906(2) 0.0200(6) Uani 1 d . .
C24 C 0.7304(3) 0.21514(15) 0.9657(2) 0.0257(6) Uani 1 d . .
H24A H 0.7026(3) 0.23490(15) 1.0142(2) 0.031 Uiso 1 calc R .
C25 C 0.7565(3) 0.1476(2) 0.9684(2) 0.0323(7) Uani 1 d . .
H25A H 0.7477(3) 0.1203(2) 1.0192(2) 0.039 Uiso 1 calc R .
C26 C 0.7964(4) 0.1194(2) 0.8949(3) 0.0373(8) Uani 1 d . .
H26A H 0.8133(4) 0.0726(2) 0.8967(3) 0.045 Uiso 1 calc R .
C27 C 0.8115(3) 0.1571(2) 0.8209(2) 0.0297(7) Uani 1 d . .
H27A H 0.8385(3) 0.1364(2) 0.7727(2) 0.036 Uiso 1 calc R .
C28 C 0.7869(3) 0.22682(14) 0.8165(2) 0.0213(6) Uani 1 d . .
C29 C 0.8515(3) 0.24778(14) 0.6755(2) 0.0239(6) Uani 1 d . .
C30 C 0.9759(3) 0.2229(2) 0.7030(3) 0.0329(7) Uani 1 d . .
H30A H 1.0285(3) 0.2197(2) 0.7706(3) 0.040 Uiso 1 calc R .
C31 C 1.0238(3) 0.2025(2) 0.6296(3) 0.0406(9) Uani 1 d . .
H31A H 1.1086(3) 0.1846(2) 0.6480(3) 0.049 Uiso 1 calc R .
C32 C 0.9488(4) 0.2082(2) 0.5320(3) 0.0397(9) Uani 1 d . .
H32A H 0.9820(4) 0.1947(2) 0.4830(3) 0.048 Uiso 1 calc R .
C33 C 0.8255(4) 0.2333(2) 0.5046(3) 0.0371(8) Uani 1 d . .
H33A H 0.7737(4) 0.2368(2) 0.4368(3) 0.045 Uiso 1 calc R .
C34 C 0.7766(3) 0.2538(2) 0.5758(2) 0.0277(6) Uani 1 d . .
H34A H 0.6919(3) 0.2718(2) 0.5565(2) 0.033 Uiso 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'
Br Br -0.2901 2.4595 '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 Os N7 100.05(9) . . ?
N3 Os N8 106.15(9) . . ?
N7 Os N8 80.86(9) . . ?
N3 Os N1 75.26(9) . . ?
N7 Os N1 173.49(9) . . ?
N8 Os N1 96.00(9) . . ?
N3 Os N5 85.08(9) . . ?
N7 Os N5 75.98(9) . . ?
N8 Os N5 155.75(9) . . ?
N1 Os N5 107.76(9) . . ?
N3 Os Br 162.44(7) . . ?
N7 Os Br 92.43(6) . . ?
N8 Os Br 87.89(7) . . ?
N1 Os Br 93.14(6) . . ?
N5 Os Br 86.04(6) . . ?
C5 N1 C1 118.0(2) . . ?
C5 N1 Os 113.2(2) . . ?
C1 N1 Os 128.6(2) . . ?
N3 N2 C5 110.2(2) . . ?
N2 N3 C6 112.9(2) . . ?
N2 N3 Os 122.9(2) . . ?
C6 N3 Os 122.8(2) . . ?
C11 N4 C12 129.3(2) . . ?
C18 N5 C22 118.6(2) . . ?
C18 N5 Os 130.4(2) . . ?
C22 N5 Os 110.8(2) . . ?
N7 N6 C22 109.5(2) . . ?
N6 N7 C23 120.0(2) . . ?
N6 N7 Os 123.4(2) . . ?
C23 N7 Os 116.6(2) . . ?
C28 N8 C29 120.3(2) . . ?
C28 N8 Os 112.4(2) . . ?
C29 N8 Os 126.1(2) . . ?
N1 C1 C2 122.3(3) . . ?
C1 C2 C3 119.5(3) . . ?
C4 C3 C2 119.5(3) . . ?
C3 C4 C5 119.0(3) . . ?
N2 C5 N1 117.7(2) . . ?
N2 C5 C4 120.7(3) . . ?
N1 C5 C4 121.6(3) . . ?
C7 C6 C11 121.9(3) . . ?
C7 C6 N3 119.4(3) . . ?
C11 C6 N3 118.8(2) . . ?
C8 C7 C6 119.9(3) . . ?
C9 C8 C7 119.2(3) . . ?
C8 C9 C10 121.2(3) . . ?
C9 C10 C11 120.7(3) . . ?
N4 C11 C10 124.3(3) . . ?
N4 C11 C6 118.4(2) . . ?
C10 C11 C6 117.1(3) . . ?
C17 C12 C13 119.4(3) . . ?
C17 C12 N4 117.5(3) . . ?
C13 C12 N4 123.0(3) . . ?
C12 C13 C14 119.2(3) . . ?
C15 C14 C13 121.0(3) . . ?
C14 C15 C16 119.7(3) . . ?
C15 C16 C17 120.4(3) . . ?
C16 C17 C12 120.3(3) . . ?
N5 C18 C19 122.6(3) . . ?
C18 C19 C20 119.0(3) . . ?
C21 C20 C19 119.6(3) . . ?
C20 C21 C22 119.1(3) . . ?
N5 C22 N6 119.2(2) . . ?
N5 C22 C21 121.0(3) . . ?
N6 C22 C21 119.7(2) . . ?
N7 C23 C24 124.8(3) . . ?
N7 C23 C28 112.9(2) . . ?
C24 C23 C28 122.3(3) . . ?
C25 C24 C23 119.2(3) . . ?
C24 C25 C26 119.3(3) . . ?
C27 C26 C25 122.2(3) . . ?
C26 C27 C28 120.1(3) . . ?
N8 C28 C27 126.1(3) . . ?
N8 C28 C23 116.9(2) . . ?
C27 C28 C23 117.0(3) . . ?
C30 C29 C34 119.5(3) . . ?
C30 C29 N8 122.0(3) . . ?
C34 C29 N8 118.4(3) . . ?
C29 C30 C31 119.4(3) . . ?
C32 C31 C30 120.3(3) . . ?
C31 C32 C33 120.3(3) . . ?
C32 C33 C34 120.2(3) . . ?
C33 C34 C29 120.2(3) . . ?
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
Os N3 1.946(2) . ?
Os N7 1.953(2) . ?
Os N8 2.031(2) . ?
Os N1 2.074(2) . ?
Os N5 2.088(2) . ?
Os Br 2.5301(3) . ?
N1 C5 1.361(3) . ?
N1 C1 1.364(3) . ?
N2 N3 1.336(3) . ?
N2 C5 1.360(3) . ?
N3 C6 1.443(3) . ?
N4 C11 1.383(4) . ?
N4 C12 1.406(4) . ?
N5 C18 1.346(4) . ?
N5 C22 1.372(3) . ?
N6 N7 1.319(3) . ?
N6 C22 1.379(3) . ?
N7 C23 1.386(3) . ?
N8 C28 1.369(4) . ?
N8 C29 1.440(4) . ?
C1 C2 1.368(4) . ?
C2 C3 1.397(4) . ?
C3 C4 1.365(4) . ?
C4 C5 1.410(4) . ?
C6 C7 1.388(4) . ?
C6 C11 1.405(4) . ?
C7 C8 1.385(4) . ?
C8 C9 1.384(5) . ?
C9 C10 1.387(5) . ?
C10 C11 1.404(4) . ?
C12 C17 1.390(4) . ?
C12 C13 1.397(4) . ?
C13 C14 1.398(5) . ?
C14 C15 1.369(5) . ?
C15 C16 1.382(5) . ?
C16 C17 1.384(5) . ?
C18 C19 1.375(4) . ?
C19 C20 1.392(4) . ?
C20 C21 1.376(4) . ?
C21 C22 1.398(4) . ?
C23 C24 1.401(4) . ?
C23 C28 1.425(4) . ?
C24 C25 1.375(4) . ?
C25 C26 1.412(5) . ?
C26 C27 1.371(5) . ?
C27 C28 1.414(4) . ?
C29 C30 1.385(4) . ?
C29 C34 1.396(4) . ?
C30 C31 1.412(5) . ?
C31 C32 1.371(6) . ?
C32 C33 1.376(5) . ?
C33 C34 1.390(4) . ?
