#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:44:31 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179202 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/37/4313761.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_4313761
loop_
_publ_author_name
'J. Scott McQueen'
'Noriharu Nagao'
'Todd Eberspacher'
'Z. W. Li'
'Henry Taube'
_publ_section_title
;
 Synthesis and Characterization of trans-[Os(en)2py(H)]2+ and Related
 Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3815
_journal_page_last               3821
_journal_paper_doi               10.1021/ic030091b
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C11 H22 F6 N5 O6 Os S2'
_chemical_formula_weight         688.66
_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
_cell_angle_alpha                94.81(3)
_cell_angle_beta                 111.03(3)
_cell_angle_gamma                111.25(3)
_cell_formula_units_Z            2
_cell_length_a                   10.021(2)
_cell_length_b                   10.330(2)
_cell_length_c                   12.470(3)
_cell_measurement_temperature    183(2)
_cell_volume                     1088.5(6)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_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  0.0207
_diffrn_reflns_av_sigmaI/netI    0.0379
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5970
_diffrn_reflns_theta_max         25.94
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    6.138
_exptl_crystal_density_diffrn    2.101
_exptl_crystal_F_000             666
_refine_diff_density_max         1.598
_refine_diff_density_min         -1.103
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.013
_refine_ls_goodness_of_fit_obs   1.030
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         3652
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_restrained_S_obs      1.030
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_obs          0.0279
_refine_ls_shift/esd_max         -0.032
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0416P)²+1.1714P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0700
_refine_ls_wR_factor_obs         0.0673
_reflns_number_observed          3412
_reflns_number_total             3721
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic030091b_2.cif
_cod_data_source_block           sma1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0416P)^2^+1.1714P] 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^)+(0.0416P)^2^+1.1714P] 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        1088.5(4)
_cod_database_code               4313761
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Os Os -0.18443(2) 0.12636(2) 0.18594(2) 0.02150(8) Uani 1 d . .
N1P N 0.0540(5) 0.2210(5) 0.3272(4) 0.0256(10) Uani 1 d . .
C1P C 0.1597(6) 0.1670(6) 0.3303(5) 0.0307(13) Uani 1 d . .
H1PA H 0.1262(6) 0.0852(6) 0.2697(5) 0.037 Uiso 1 calc R .
C2P C 0.3111(7) 0.2227(7) 0.4146(5) 0.0374(14) Uani 1 d . .
H2PA H 0.3810(7) 0.1811(7) 0.4129(5) 0.045 Uiso 1 calc R .
C3P C 0.3593(8) 0.3413(7) 0.5026(6) 0.043(2) Uani 1 d . .
H3PA H 0.4640(8) 0.3833(7) 0.5627(6) 0.051 Uiso 1 calc R .
C4P C 0.2546(7) 0.3987(6) 0.5027(5) 0.0384(14) Uani 1 d . .
H4PA H 0.2860(7) 0.4803(6) 0.5628(5) 0.046 Uiso 1 calc R .
C5P C 0.1048(7) 0.3358(6) 0.4148(5) 0.0297(12) Uani 1 d . .
H5PA H 0.0330(7) 0.3753(6) 0.4157(5) 0.036 Uiso 1 calc R .
N1 N -0.1727(5) 0.3287(5) 0.1565(4) 0.0273(10) Uani 1 d . .
H1C H -0.2730(5) 0.3221(5) 0.1169(4) 0.033 Uiso 1 calc R .
H1D H -0.1254(5) 0.3948(5) 0.2280(4) 0.033 Uiso 1 calc R .
N2 N -0.0908(5) 0.1388(5) 0.0569(4) 0.0283(10) Uani 1 d . .
H2C H 0.0156(5) 0.1627(5) 0.0931(4) 0.034 Uiso 1 calc R .
H2D H -0.1390(5) 0.0512(5) 0.0034(4) 0.034 Uiso 1 calc R .
N3 N -0.2772(5) 0.1159(5) 0.3138(4) 0.0279(10) Uani 1 d . .
H3C H -0.1973(5) 0.1663(5) 0.3875(4) 0.033 Uiso 1 calc R .
H3D H -0.3482(5) 0.1563(5) 0.2963(4) 0.033 Uiso 1 calc R .
N4 N -0.2144(5) -0.0826(5) 0.2058(4) 0.0266(10) Uani 1 d . .
H4C H -0.2962(5) -0.1493(5) 0.1389(4) 0.032 Uiso 1 calc R .
H4D H -0.1241(5) -0.0937(5) 0.2152(4) 0.032 Uiso 1 calc R .
C1 C -0.0811(8) 0.3761(6) 0.0855(6) 0.0366(14) Uani 1 d . .
H1A H 0.0331(8) 0.4216(6) 0.1380(6) 0.044 Uiso 1 calc R .
H1B H -0.1089(8) 0.4475(6) 0.0457(6) 0.044 Uiso 1 calc R .
C2 C -0.1182(8) 0.2482(7) -0.0053(5) 0.0400(15) Uani 1 d . .
H2A H -0.2294(8) 0.2097(7) -0.0640(5) 0.048 Uiso 1 calc R .
H2B H -0.0496(8) 0.2760(7) -0.0478(5) 0.048 Uiso 1 calc R .
C3 C -0.3570(7) -0.0363(6) 0.3142(5) 0.0345(13) Uani 1 d . .
H3A H -0.4598(7) -0.0848(6) 0.2443(5) 0.041 Uiso 1 calc R .
H3B H -0.3756(7) -0.0427(6) 0.3868(5) 0.041 Uiso 1 calc R .
C4 C -0.2487(7) -0.1059(6) 0.3105(5) 0.0342(13) Uani 1 d . .
H4A H -0.1496(7) -0.0627(6) 0.3838(5) 0.041 Uiso 1 calc R .
H4B H -0.3001(7) -0.2098(6) 0.3043(5) 0.041 Uiso 1 calc R .
S1A S 0.4098(2) 0.26272(15) 0.12643(12) 0.0279(3) Uani 1 d . .
O1A O 0.5150(5) 0.2710(5) 0.2437(4) 0.0456(11) Uani 1 d . .
O2A O 0.4702(5) 0.2608(4) 0.0376(3) 0.0376(10) Uani 1 d . .
O3A O 0.2476(5) 0.1633(4) 0.0882(4) 0.0447(11) Uani 1 d . .
C1A C 0.3992(8) 0.4337(7) 0.1405(6) 0.045(2) Uani 1 d . .
F1A F 0.3411(6) 0.4515(5) 0.2196(4) 0.0723(13) Uani 1 d . .
F2A F 0.5394(6) 0.5408(4) 0.1769(5) 0.0785(14) Uani 1 d . .
F3A F 0.3083(6) 0.4458(5) 0.0389(4) 0.080(2) Uani 1 d . .
S1B S 0.9460(2) 0.26537(15) 0.66109(12) 0.0273(3) Uani 1 d . .
O1B O 0.9953(6) 0.4056(5) 0.6409(5) 0.0556(13) Uani 1 d . .
O2B O 1.0249(5) 0.2583(6) 0.7797(4) 0.0510(12) Uani 1 d . .
O3B O 0.9254(5) 0.1554(4) 0.5707(4) 0.0357(9) Uani 1 d . .
C1B C 0.7458(8) 0.2205(8) 0.6443(6) 0.049(2) Uani 1 d . .
F1B F 0.7379(5) 0.3132(4) 0.7191(3) 0.0562(11) Uani 1 d . .
F2B F 0.6888(6) 0.0940(5) 0.6704(6) 0.101(2) Uani 1 d . .
F3B F 0.6551(6) 0.2154(8) 0.5374(4) 0.107(2) Uani 1 d . .
H1 H -0.3690(54) 0.0466(50) 0.0776(41) 0.014(12) Uiso 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
H1 Os N3 89.8(16) . . ?
H1 Os N4 85.9(16) . . ?
N3 Os N4 80.8(2) . . ?
H1 Os N1 89.7(16) . . ?
N3 Os N1 98.8(2) . . ?
N4 Os N1 175.6(2) . . ?
H1 Os N2 90.2(16) . . ?
N3 Os N2 179.5(2) . . ?
N4 Os N2 99.7(2) . . ?
N1 Os N2 80.7(2) . . ?
H1 Os N1P 177.6(16) . . ?
N3 Os N1P 89.9(2) . . ?
N4 Os N1P 91.7(2) . . ?
N1 Os N1P 92.6(2) . . ?
N2 Os N1P 90.1(2) . . ?
C5P N1P C1P 116.4(5) . . ?
C5P N1P Os 122.3(4) . . ?
C1P N1P Os 121.3(4) . . ?
N1P C1P C2P 124.2(5) . . ?
C1P C2P C3P 117.7(6) . . ?
C4P C3P C2P 119.7(6) . . ?
C5P C4P C3P 118.7(6) . . ?
N1P C5P C4P 123.3(5) . . ?
C1 N1 Os 109.9(3) . . ?
C2 N2 Os 109.2(3) . . ?
C3 N3 Os 109.2(3) . . ?
C4 N4 Os 109.8(3) . . ?
N1 C1 C2 109.0(5) . . ?
N2 C2 C1 108.0(5) . . ?
N3 C3 C4 106.8(4) . . ?
N4 C4 C3 108.0(4) . . ?
O1A S1A O3A 115.6(3) . . ?
O1A S1A O2A 115.2(3) . . ?
O3A S1A O2A 114.5(3) . . ?
O1A S1A C1A 103.5(3) . . ?
O3A S1A C1A 102.3(3) . . ?
O2A S1A C1A 103.3(3) . . ?
F3A C1A F2A 107.3(6) . . ?
F3A C1A F1A 107.9(6) . . ?
F2A C1A F1A 107.4(5) . . ?
F3A C1A S1A 111.7(4) . . ?
F2A C1A S1A 111.5(5) . . ?
F1A C1A S1A 110.9(5) . . ?
O1B S1B O2B 115.0(3) . . ?
O1B S1B O3B 114.8(3) . . ?
O2B S1B O3B 115.0(3) . . ?
O1B S1B C1B 103.4(3) . . ?
O2B S1B C1B 103.5(3) . . ?
O3B S1B C1B 102.8(3) . . ?
F3B C1B F1B 108.0(6) . . ?
F3B C1B F2B 110.1(7) . . ?
F1B C1B F2B 105.1(6) . . ?
F3B C1B S1B 111.3(5) . . ?
F1B C1B S1B 112.6(5) . . ?
F2B C1B S1B 109.6(5) . . ?
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 H1 1.69(5) . ?
Os N3 2.107(4) . ?
Os N4 2.118(4) . ?
Os N1 2.121(4) . ?
Os N2 2.126(4) . ?
Os N1P 2.183(4) . ?
N1P C5P 1.344(7) . ?
N1P C1P 1.355(7) . ?
C1P C2P 1.363(8) . ?
C2P C3P 1.380(9) . ?
C3P C4P 1.380(9) . ?
C4P C5P 1.368(8) . ?
N1 C1 1.482(7) . ?
N2 C2 1.475(7) . ?
N3 C3 1.485(7) . ?
N4 C4 1.482(7) . ?
C1 C2 1.502(9) . ?
C3 C4 1.514(8) . ?
S1A O1A 1.436(4) . ?
S1A O3A 1.441(4) . ?
S1A O2A 1.442(4) . ?
S1A C1A 1.805(7) . ?
C1A F3A 1.316(8) . ?
C1A F2A 1.318(8) . ?
C1A F1A 1.343(8) . ?
S1B O1B 1.428(5) . ?
S1B O2B 1.427(4) . ?
S1B O3B 1.432(4) . ?
S1B C1B 1.814(7) . ?
C1B F3B 1.300(8) . ?
C1B F1B 1.324(7) . ?
C1B F2B 1.343(9) . ?
