#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/02/7010260.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_7010260
loop_
_publ_author_name
'Majumder, Kanchana'
'Peng, Shie-Ming'
'Bhattacharya, Samaresh'
_publ_section_title
;
 Cyclometallation and NN bond cleavage of 2-(arylazo)phenols by
 osmium. Synthesis, structure and redox properties †
;
_journal_issue                   3
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              284
_journal_paper_doi               10.1039/b007486l
_journal_year                    2001
_chemical_formula_sum            'C38.5 H31.5 Cl2 N3 O2 Os P'
_chemical_formula_weight         860.24
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 112.731(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   40.4327(2)
_cell_length_b                   10.9195(2)
_cell_length_c                   17.5688(3)
_cell_measurement_reflns_used    6551
_cell_measurement_temperature    295(2)
_cell_volume                     7154.24(19)
_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      295(2)
_diffrn_measurement_device       'Siemens SMART 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  0.0630
_diffrn_reflns_av_sigmaI/netI    0.0716
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19051
_diffrn_reflns_theta_max         26.39
_diffrn_reflns_theta_min         1.94
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    3.797
_exptl_absorpt_correction_T_max  0.7195
_exptl_absorpt_correction_T_min  0.5139
_exptl_absorpt_correction_type   ' empirical used sadabs'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             3396
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.342
_refine_diff_density_min         -1.944
_refine_diff_density_rms         0.183
_refine_ls_extinction_coef       0.00007(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.021
_refine_ls_goodness_of_fit_obs   1.117
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         7104
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_restrained_S_obs      1.117
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_obs          0.0564
_refine_ls_shift/esd_max         0.018
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0849P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1456
_refine_ls_wR_factor_obs         0.1353
_reflns_number_observed          5205
_reflns_number_total             7104
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b007486l.txt
_cod_data_source_block           ic6515
_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^)+(0.0849P)^2^+0.0000P] 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^)+(0.0849P)^2^+0.0000P] 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        7154.2(2)
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C38.50 H31.50 Cl2 N3 O2 Os P'
_cod_database_code               7010260
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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 0.139625(8) 0.42756(2) 0.78675(2) 0.03708(13) Uani 1 d . .
Cl1 Cl 0.11397(10) 0.0887(3) 1.0145(2) 0.0971(11) Uani 1 d . .
P1 P 0.13587(6) 0.5816(2) 0.87570(12) 0.0387(5) Uani 1 d . .
O1 O 0.1555(2) 0.5659(4) 0.7273(4) 0.0503(14) Uani 1 d . .
O2 O 0.1327(2) 0.3135(5) 0.6874(3) 0.0535(15) Uani 1 d . .
N1 N 0.1936(2) 0.3984(5) 0.8249(4) 0.0356(14) Uani 1 d . .
N2 N 0.2113(2) 0.3163(6) 0.8795(4) 0.047(2) Uani 1 d . .
N3 N 0.0888(2) 0.3978(5) 0.7448(4) 0.047(2) Uani 1 d . .
H3B H 0.0756(2) 0.4302(5) 0.7678(4) 0.057 Uiso 1 calc R .
C1 C 0.1880(3) 0.5503(6) 0.7287(5) 0.044(2) Uani 1 d . .
C2 C 0.2023(3) 0.6214(8) 0.6809(6) 0.058(2) Uani 1 d . .
H2A H 0.1881(3) 0.6788(8) 0.6434(6) 0.069 Uiso 1 calc R .
C3 C 0.2370(3) 0.6052(8) 0.6902(6) 0.059(3) Uani 1 d . .
H3A H 0.2459(3) 0.6530(8) 0.6587(6) 0.071 Uiso 1 calc R .
C4 C 0.2601(3) 0.5198(8) 0.7452(6) 0.055(2) Uani 1 d . .
C5 C 0.2467(2) 0.4481(7) 0.7906(5) 0.048(2) Uani 1 d . .
H5A H 0.2613(2) 0.3902(7) 0.8272(5) 0.057 Uiso 1 calc R .
C6 C 0.2114(2) 0.4625(7) 0.7817(5) 0.043(2) Uani 1 d . .
C7 C 0.1878(2) 0.2630(7) 0.9117(5) 0.042(2) Uani 1 d . .
C8 C 0.2014(3) 0.1706(7) 0.9727(5) 0.054(2) Uani 1 d . .
H8A H 0.2253(3) 0.1471(7) 0.9915(5) 0.065 Uiso 1 calc R .
C9 C 0.1784(3) 0.1165(8) 1.0036(5) 0.061(3) Uani 1 d . .
H9A H 0.1865(3) 0.0545(8) 1.0428(5) 0.073 Uiso 1 calc R .
C10 C 0.1427(3) 0.1564(8) 0.9750(6) 0.057(2) Uani 1 d . .
C11 C 0.1298(2) 0.2462(7) 0.9150(5) 0.048(2) Uani 1 d . .
H11A H 0.1058(2) 0.2685(7) 0.8968(5) 0.058 Uiso 1 calc R .
C12 C 0.1513(2) 0.3033(7) 0.8815(4) 0.041(2) Uani 1 d . .
C13 C 0.2989(3) 0.5049(11) 0.7512(7) 0.081(3) Uani 1 d . .
H13A H 0.3034(3) 0.5626(11) 0.7151(7) 0.122 Uiso 1 calc R .
H13B H 0.3023(3) 0.4232(11) 0.7354(7) 0.122 Uiso 1 calc R .
H13C H 0.3153(3) 0.5196(11) 0.8070(7) 0.122 Uiso 1 calc R .
C14 C 0.0996(3) 0.2792(7) 0.6475(5) 0.049(2) Uani 1 d . .
C15 C 0.0886(3) 0.2012(7) 0.5775(6) 0.068(3) Uani 1 d . .
H15A H 0.1052(3) 0.1709(7) 0.5577(6) 0.082 Uiso 1 calc R .
C16 C 0.0538(4) 0.1718(8) 0.5402(6) 0.086(4) Uani 1 d . .
H16A H 0.0466(4) 0.1222(8) 0.4936(6) 0.103 Uiso 1 calc R .
C17 C 0.0277(3) 0.2136(10) 0.5693(8) 0.095(4) Uani 1 d . .
C18 C 0.0379(3) 0.2875(9) 0.6369(7) 0.075(3) Uani 1 d . .
H18A H 0.0211(3) 0.3150(9) 0.6573(7) 0.090 Uiso 1 calc R .
C19 C 0.0739(2) 0.3215(7) 0.6754(5) 0.053(2) Uani 1 d . .
C20 C -0.0132(4) 0.1830(12) 0.5209(11) 0.161(8) Uani 1 d . .
H20A H -0.0158(4) 0.1301(12) 0.4752(11) 0.241 Uiso 1 calc R .
H20B H -0.0263(4) 0.2574(12) 0.5008(11) 0.241 Uiso 1 calc R .
H20C H -0.0224(4) 0.1427(12) 0.5572(11) 0.241 Uiso 1 calc R .
C21 C 0.1747(2) 0.6212(7) 0.9691(5) 0.043(2) Uani 1 d . .
C22 C 0.2093(3) 0.5993(8) 0.9742(6) 0.058(2) Uani 1 d . .
H22A H 0.2124(3) 0.5591(8) 0.9308(6) 0.069 Uiso 1 calc R .
C23 C 0.2393(3) 0.6349(9) 1.0415(6) 0.063(2) Uani 1 d . .
H23A H 0.2622(3) 0.6171(9) 1.0443(6) 0.076 Uiso 1 calc R .
C24 C 0.2342(3) 0.6985(8) 1.1052(5) 0.069(3) Uani 1 d . .
H24A H 0.2540(3) 0.7270(8) 1.1498(5) 0.082 Uiso 1 calc R .
C25 C 0.2003(3) 0.7193(9) 1.1025(5) 0.070(3) Uani 1 d . .
H25A H 0.1971(3) 0.7597(9) 1.1458(5) 0.084 Uiso 1 calc R .
C26 C 0.1710(3) 0.6797(8) 1.0350(5) 0.058(2) Uani 1 d . .
H26A H 0.1481(3) 0.6929(8) 1.0340(5) 0.070 Uiso 1 calc R .
C27 C 0.1230(2) 0.7284(7) 0.8203(5) 0.049(2) Uani 1 d . .
C28 C 0.1373(3) 0.8390(8) 0.8547(6) 0.063(3) Uani 1 d . .
H28A H 0.1539(3) 0.8414(8) 0.9089(6) 0.076 Uiso 1 calc R .
C29 C 0.1273(4) 0.9484(9) 0.8096(8) 0.084(4) Uani 1 d . .
H29A H 0.1376(4) 1.0222(9) 0.8337(8) 0.101 Uiso 1 calc R .
C30 C 0.1029(4) 0.9464(9) 0.7319(7) 0.084(4) Uani 1 d . .
H30A H 0.0954(4) 1.0196(9) 0.7033(7) 0.101 Uiso 1 calc R .
C31 C 0.0888(3) 0.8360(9) 0.6935(6) 0.073(3) Uani 1 d . .
H31A H 0.0733(3) 0.8350(9) 0.6383(6) 0.088 Uiso 1 calc R .
C32 C 0.0979(3) 0.7275(9) 0.7378(6) 0.063(3) Uani 1 d . .
H32A H 0.0875(3) 0.6542(9) 0.7131(6) 0.076 Uiso 1 calc R .
C33 C 0.1007(2) 0.5513(7) 0.9159(5) 0.048(2) Uani 1 d . .
C34 C 0.0658(3) 0.5867(9) 0.8716(8) 0.073(3) Uani 1 d . .
H34A H 0.0599(3) 0.6297(9) 0.8224(8) 0.087 Uiso 1 calc R .
C35 C 0.0390(4) 0.5569(12) 0.9017(11) 0.096(4) Uani 1 d . .
H35A H 0.0155(4) 0.5811(12) 0.8718(11) 0.115 Uiso 1 calc R .
C36 C 0.0467(4) 0.4944(11) 0.9725(11) 0.098(5) Uani 1 d . .
H36A H 0.0289(4) 0.4750(11) 0.9916(11) 0.118 Uiso 1 calc R .
C37 C 0.0817(4) 0.4600(10) 1.0159(8) 0.086(4) Uani 1 d . .
H37A H 0.0875(4) 0.4179(10) 1.0654(8) 0.103 Uiso 1 calc R .
C38 C 0.1087(3) 0.4865(8) 0.9876(6) 0.063(3) Uani 1 d . .
H38A H 0.1321(3) 0.4602(8) 1.0173(6) 0.075 Uiso 1 calc R .
C39 C 0.0000 0.9669 0.7500 0.305 Uiso 1 d S .
H39A H 0.0181 0.9788 0.8042 0.366 Uiso 0.50 d P .
Cl2 Cl -0.0222 1.0697 0.7078 0.268 Uiso 0.50 d P .
Cl3 Cl -0.0046 0.8451 0.7118 0.248 Uiso 0.50 d P .
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'
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 N1 161.0(2) . . ?
N3 Os C12 94.3(3) . . ?
N1 Os C12 75.6(3) . . ?
N3 Os O2 78.4(3) . . ?
N1 Os O2 87.8(2) . . ?
C12 Os O2 101.5(3) . . ?
N3 Os O1 115.0(3) . . ?
N1 Os O1 77.2(2) . . ?
C12 Os O1 150.4(3) . . ?
O2 Os O1 88.9(2) . . ?
N3 Os P1 92.4(2) . . ?
N1 Os P1 103.3(2) . . ?
C12 Os P1 89.3(2) . . ?
O2 Os P1 166.2(2) . . ?
O1 Os P1 85.7(2) . . ?
C21 P1 C27 103.7(4) . . ?
C21 P1 C33 102.7(4) . . ?
C27 P1 C33 104.8(4) . . ?
C21 P1 Os 120.9(3) . . ?
C27 P1 Os 110.5(3) . . ?
C33 P1 Os 112.6(3) . . ?
C1 O1 Os 113.5(5) . . ?
C14 O2 Os 113.7(5) . . ?
N2 N1 C6 119.1(7) . . ?
N2 N1 Os 124.0(5) . . ?
C6 N1 Os 116.5(5) . . ?
N1 N2 C7 108.5(7) . . ?
C19 N3 Os 118.1(6) . . ?
O1 C1 C6 120.5(7) . . ?
O1 C1 C2 123.4(8) . . ?
C6 C1 C2 116.1(9) . . ?
C3 C2 C1 119.6(9) . . ?
C2 C3 C4 123.4(8) . . ?
C5 C4 C3 118.1(9) . . ?
C5 C4 C13 121.4(9) . . ?
C3 C4 C13 120.4(9) . . ?
C4 C5 C6 119.5(8) . . ?
C5 C6 C1 123.3(8) . . ?
C5 C6 N1 126.7(7) . . ?
C1 C6 N1 109.9(8) . . ?
N2 C7 C8 118.4(8) . . ?
N2 C7 C12 118.9(7) . . ?
C8 C7 C12 122.7(8) . . ?
C9 C8 C7 118.7(9) . . ?
C8 C9 C10 118.9(8) . . ?
C11 C10 C9 121.6(8) . . ?
C11 C10 Cl1 119.6(8) . . ?
C9 C10 Cl1 118.8(7) . . ?
C12 C11 C10 122.2(8) . . ?
C11 C12 C7 115.8(7) . . ?
C11 C12 Os 131.4(6) . . ?
C7 C12 Os 112.5(5) . . ?
O2 C14 C19 117.9(7) . . ?
O2 C14 C15 123.4(9) . . ?
C19 C14 C15 118.6(9) . . ?
C16 C15 C14 119.1(11) . . ?
C15 C16 C17 122.3(10) . . ?
C18 C17 C16 119.4(10) . . ?
C18 C17 C20 119.8(13) . . ?
C16 C17 C20 120.7(12) . . ?
C17 C18 C19 119.1(11) . . ?
C14 C19 C18 121.5(9) . . ?
C14 C19 N3 111.9(8) . . ?
C18 C19 N3 126.5(9) . . ?
C26 C21 C22 117.4(8) . . ?
C26 C21 P1 121.8(7) . . ?
C22 C21 P1 120.7(6) . . ?
C23 C22 C21 122.4(9) . . ?
C22 C23 C24 118.2(10) . . ?
C25 C24 C23 120.6(9) . . ?
C24 C25 C26 119.4(9) . . ?
C21 C26 C25 122.0(10) . . ?
C28 C27 C32 118.1(8) . . ?
C28 C27 P1 123.2(6) . . ?
C32 C27 P1 118.7(6) . . ?
C27 C28 C29 121.3(10) . . ?
C30 C29 C28 119.9(10) . . ?
C29 C30 C31 120.7(9) . . ?
C30 C31 C32 119.9(9) . . ?
C31 C32 C27 119.9(9) . . ?
C38 C33 C34 119.3(9) . . ?
C38 C33 P1 120.1(8) . . ?
C34 C33 P1 120.4(7) . . ?
C33 C34 C35 119.3(12) . . ?
C36 C35 C34 121.8(13) . . ?
C35 C36 C37 118.1(12) . . ?
C36 C37 C38 121.8(13) . . ?
C33 C38 C37 119.7(11) . . ?
Cl2 C39 Cl2 78.5 2_556 . ?
Cl2 C39 Cl3 121.6 2_556 2_556 ?
Cl2 C39 Cl3 151.5 . 2_556 ?
Cl2 C39 Cl3 151.5 2_556 . ?
Cl2 C39 Cl3 121.6 . . ?
Cl3 C39 Cl3 50.3 2_556 . ?
C39 Cl2 Cl2 50.8 . 2_556 ?
Cl3 Cl3 C39 64.9 2_556 . ?
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 1.923(7) . ?
Os N1 2.047(6) . ?
Os C12 2.056(7) . ?
Os O2 2.074(5) . ?
Os O1 2.075(5) . ?
Os P1 2.341(2) . ?
Cl1 C10 1.731(9) . ?
P1 C21 1.832(8) . ?
P1 C27 1.842(8) . ?
P1 C33 1.845(9) . ?
O1 C1 1.317(10) . ?
O2 C14 1.305(10) . ?
N1 N2 1.305(8) . ?
N1 C6 1.416(10) . ?
N2 C7 1.406(10) . ?
N3 C19 1.407(10) . ?
C1 C6 1.413(11) . ?
C1 C2 1.421(11) . ?
C2 C3 1.358(13) . ?
C3 C4 1.406(14) . ?
C4 C5 1.370(11) . ?
C4 C13 1.540(13) . ?
C5 C6 1.384(12) . ?
C7 C8 1.419(11) . ?
C7 C12 1.433(11) . ?
C8 C9 1.377(12) . ?
C9 C10 1.404(13) . ?
C10 C11 1.386(11) . ?
C11 C12 1.373(11) . ?
C14 C19 1.388(13) . ?
C14 C15 1.419(11) . ?
C15 C16 1.338(15) . ?
C16 C17 1.42(2) . ?
C17 C18 1.362(15) . ?
C17 C20 1.58(2) . ?
C18 C19 1.396(12) . ?
C21 C26 1.381(11) . ?
C21 C22 1.386(12) . ?
C22 C23 1.382(12) . ?
C23 C24 1.398(13) . ?
C24 C25 1.371(14) . ?
C25 C26 1.382(12) . ?
C27 C28 1.374(12) . ?
C27 C32 1.413(11) . ?
C28 C29 1.404(13) . ?
C29 C30 1.34(2) . ?
C30 C31 1.391(14) . ?
C31 C32 1.387(12) . ?
C33 C38 1.370(12) . ?
C33 C34 1.379(14) . ?
C34 C35 1.41(2) . ?
C35 C36 1.35(2) . ?
C36 C37 1.38(2) . ?
C37 C38 1.393(15) . ?
C39 Cl2 1.45 2_556 ?
C39 Cl2 1.45 . ?
C39 Cl3 1.47 2_556 ?
C39 Cl3 1.47 . ?
Cl2 Cl2 1.83 2_556 ?
Cl3 Cl3 1.25 2_556 ?
