#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:44:31 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179202 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/37/4313760.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_4313760
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 H23 F6 N5 O6 Os S2'
_chemical_formula_weight         689.66
_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                94.6700(10)
_cell_angle_beta                 111.5450(10)
_cell_angle_gamma                111.4460(10)
_cell_formula_units_Z            2
_cell_length_a                   10.0245(3)
_cell_length_b                   10.3111(3)
_cell_length_c                   12.4820(3)
_cell_measurement_temperature    169(2)
_cell_volume                     1081.73(5)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      169(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  0.0298
_diffrn_reflns_av_sigmaI/netI    0.0359
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5918
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    6.177
_exptl_crystal_density_diffrn    2.117
_exptl_crystal_F_000             668
_refine_diff_density_max         1.352
_refine_diff_density_min         -1.458
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.051
_refine_ls_goodness_of_fit_obs   1.057
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         3632
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_restrained_S_obs      1.057
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_obs          0.0253
_refine_ls_shift/esd_max         -0.179
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0392P)²+1.2081P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0657
_refine_ls_wR_factor_obs         0.0635
_reflns_number_observed          3502
_reflns_number_total             3676
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic030091b_1.cif
_cod_data_source_block           sma2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0392P)^2^+1.2081P] 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^)+(0.0392P)^2^+1.2081P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4313760
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 0.19195(2) -0.12164(2) -0.183704(14) 0.01430(8) Uani 1 d . .
H1 H 0.3520(65) -0.0432(61) -0.0619(53) 0.027(15) Uiso 1 d . .
H2 H 0.3535(84) -0.1065(80) -0.1095(69) 0.061(22) Uiso 1 d . .
N1P N -0.0429(4) -0.2152(4) -0.3231(3) 0.0174(8) Uani 1 d . .
C1P C -0.1486(6) -0.1616(5) -0.3249(4) 0.0241(10) Uani 1 d . .
H1PA H -0.1139(6) -0.0782(5) -0.2651(4) 0.029 Uiso 1 calc R .
C2P C -0.3032(6) -0.2221(5) -0.4089(5) 0.0269(11) Uani 1 d . .
H2PA H -0.3745(6) -0.1831(5) -0.4057(5) 0.032 Uiso 1 calc R .
C3P C -0.3527(6) -0.3397(5) -0.4974(5) 0.0281(11) Uani 1 d . .
H3PA H -0.4585(6) -0.3823(5) -0.5576(5) 0.034 Uiso 1 calc R .
C4P C -0.2475(6) -0.3956(5) -0.4980(5) 0.0284(11) Uani 1 d . .
H4PA H -0.2801(6) -0.4776(5) -0.5583(5) 0.034 Uiso 1 calc R .
C5P C -0.0940(6) -0.3312(5) -0.4101(4) 0.0214(10) Uani 1 d . .
H5PA H -0.0220(6) -0.3703(5) -0.4112(4) 0.026 Uiso 1 calc R .
N1 N 0.1701(5) -0.3301(4) -0.1571(3) 0.0192(8) Uani 1 d . .
H1C H 0.1235(5) -0.3950(4) -0.2295(3) 0.023 Uiso 1 calc R .
H1D H 0.2692(5) -0.3261(4) -0.1152(3) 0.023 Uiso 1 calc R .
N2 N 0.0862(5) -0.1386(4) -0.0608(3) 0.0195(8) Uani 1 d . .
H2C H 0.1324(5) -0.0516(4) -0.0064(3) 0.023 Uiso 1 calc R .
H2D H -0.0204(5) -0.1631(4) -0.1010(3) 0.023 Uiso 1 calc R .
N3 N 0.2749(5) -0.1151(4) -0.3190(3) 0.0193(8) Uani 1 d . .
H3C H 0.3453(5) -0.1563(4) -0.3037(3) 0.023 Uiso 1 calc R .
H3D H 0.1910(5) -0.1664(4) -0.3917(3) 0.023 Uiso 1 calc R .
N4 N 0.2173(5) 0.0869(4) -0.2099(3) 0.0200(8) Uani 1 d . .
H4C H 0.1263(5) 0.0967(4) -0.2194(3) 0.024 Uiso 1 calc R .
H4D H 0.3002(5) 0.1562(4) -0.1439(3) 0.024 Uiso 1 calc R .
C1 C 0.0727(6) -0.3782(5) -0.0906(5) 0.0253(11) Uani 1 d . .
H1A H 0.0961(6) -0.4520(5) -0.0515(5) 0.030 Uiso 1 calc R .
H1B H -0.0413(6) -0.4214(5) -0.1461(5) 0.030 Uiso 1 calc R .
C2 C 0.1103(6) -0.2507(5) 0.0013(5) 0.0276(11) Uani 1 d . .
H2A H 0.0395(6) -0.2790(5) 0.0418(5) 0.033 Uiso 1 calc R .
H2B H 0.2214(6) -0.2133(5) 0.0618(5) 0.033 Uiso 1 calc R .
C3 C 0.3542(6) 0.0366(5) -0.3216(4) 0.0238(10) Uani 1 d . .
H3A H 0.3688(6) 0.0411(5) -0.3957(4) 0.029 Uiso 1 calc R .
H3B H 0.4595(6) 0.0860(5) -0.2529(4) 0.029 Uiso 1 calc R .
C4 C 0.2475(6) 0.1078(5) -0.3158(4) 0.0229(10) Uani 1 d . .
H4A H 0.2995(6) 0.2118(5) -0.3104(4) 0.027 Uiso 1 calc R .
H4B H 0.1461(6) 0.0641(5) -0.3885(4) 0.027 Uiso 1 calc R .
S1A S 0.58732(14) -0.26257(12) -0.13004(11) 0.0210(2) Uani 1 d . .
O1A O 0.4802(4) -0.2742(4) -0.2484(3) 0.0354(9) Uani 1 d . .
O2A O 0.5274(4) -0.2564(4) -0.0414(3) 0.0274(8) Uani 1 d . .
O3A O 0.7505(4) -0.1631(4) -0.0928(4) 0.0357(9) Uani 1 d . .
C1A C 0.5951(6) -0.4361(5) -0.1401(5) 0.0334(12) Uani 1 d . .
F1A F 0.6503(5) -0.4589(4) -0.2194(3) 0.0536(10) Uani 1 d . .
F2A F 0.4526(4) -0.5418(3) -0.1748(4) 0.0599(11) Uani 1 d . .
F3A F 0.6889(5) -0.4451(4) -0.0369(3) 0.0590(11) Uani 1 d . .
S1B S 0.05459(14) -0.26627(12) -0.66264(10) 0.0199(2) Uani 1 d . .
O1B O 0.0134(5) -0.4033(4) -0.6343(4) 0.0426(10) Uani 1 d . .
O2B O -0.0320(4) -0.2699(5) -0.7838(3) 0.0378(9) Uani 1 d . .
O3B O 0.0741(4) -0.1513(4) -0.5759(3) 0.0263(7) Uani 1 d . .
C1B C 0.2556(6) -0.2154(6) -0.6487(5) 0.0338(13) Uani 1 d . .
F1B F 0.2651(4) -0.3116(4) -0.7205(3) 0.0419(8) Uani 1 d . .
F2B F 0.3077(5) -0.0906(4) -0.6781(5) 0.0667(13) Uani 1 d . .
F3B F 0.3538(4) -0.2012(6) -0.5389(4) 0.0754(15) Uani 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
H2 Os H1 31.7(29) . . ?
H2 Os N1P 158.3(30) . . ?
H1 Os N1P 168.1(21) . . ?
H2 Os N3 81.9(30) . . ?
H1 Os N3 103.9(21) . . ?
N1P Os N3 87.30(15) . . ?
H2 Os N4 106.4(28) . . ?
H1 Os N4 88.0(20) . . ?
N1P Os N4 90.05(14) . . ?
N3 Os N4 79.87(15) . . ?
H2 Os N1 72.8(28) . . ?
H1 Os N1 91.5(20) . . ?
N1P Os N1 90.60(14) . . ?
N3 Os N1 99.58(14) . . ?
N4 Os N1 179.12(13) . . ?
H2 Os N2 103.0(30) . . ?
H1 Os N2 81.5(21) . . ?
N1P Os N2 87.31(14) . . ?
N3 Os N2 174.59(13) . . ?
N4 Os N2 100.56(14) . . ?
N1 Os N2 80.05(14) . . ?
C5P N1P C1P 117.2(4) . . ?
C5P N1P Os 122.0(3) . . ?
C1P N1P Os 120.8(3) . . ?
N1P C1P C2P 123.1(5) . . ?
C3P C2P C1P 118.7(5) . . ?
C2P C3P C4P 119.2(5) . . ?
C3P C4P C5P 119.3(5) . . ?
N1P C5P C4P 122.3(4) . . ?
C1 N1 Os 110.1(3) . . ?
C2 N2 Os 108.8(3) . . ?
C3 N3 Os 109.2(3) . . ?
C4 N4 Os 110.6(3) . . ?
N1 C1 C2 109.0(4) . . ?
N2 C2 C1 107.7(4) . . ?
N3 C3 C4 106.9(4) . . ?
N4 C4 C3 108.4(4) . . ?
O1A S1A O3A 115.5(3) . . ?
O1A S1A O2A 114.7(2) . . ?
O3A S1A O2A 114.7(2) . . ?
O1A S1A C1A 103.5(2) . . ?
O3A S1A C1A 102.9(2) . . ?
O2A S1A C1A 103.0(2) . . ?
F2A C1A F3A 107.9(5) . . ?
F2A C1A F1A 107.5(4) . . ?
F3A C1A F1A 107.6(4) . . ?
F2A C1A S1A 111.1(4) . . ?
F3A C1A S1A 111.7(4) . . ?
F1A C1A S1A 110.8(4) . . ?
O2B S1B O1B 115.0(3) . . ?
O2B S1B O3B 114.9(2) . . ?
O1B S1B O3B 114.7(2) . . ?
O2B S1B C1B 103.3(3) . . ?
O1B S1B C1B 103.8(3) . . ?
O3B S1B C1B 102.8(2) . . ?
F3B C1B F1B 107.5(4) . . ?
F3B C1B F2B 108.6(5) . . ?
F1B C1B F2B 106.3(5) . . ?
F3B C1B S1B 111.1(4) . . ?
F1B C1B S1B 112.6(4) . . ?
F2B C1B S1B 110.4(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
Os H2 1.48(7) . ?
Os H1 1.61(6) . ?
Os N1P 2.135(4) . ?
Os N3 2.135(4) . ?
Os N4 2.138(4) . ?
Os N1 2.146(4) . ?
Os N2 2.147(4) . ?
N1P C5P 1.343(6) . ?
N1P C1P 1.357(6) . ?
C1P C2P 1.373(7) . ?
C2P C3P 1.370(7) . ?
C3P C4P 1.377(8) . ?
C4P C5P 1.381(7) . ?
N1 C1 1.482(6) . ?
N2 C2 1.486(6) . ?
N3 C3 1.482(6) . ?
N4 C4 1.476(6) . ?
C1 C2 1.504(7) . ?
C3 C4 1.520(7) . ?
S1A O1A 1.437(4) . ?
S1A O3A 1.442(4) . ?
S1A O2A 1.447(4) . ?
S1A C1A 1.815(5) . ?
C1A F2A 1.321(6) . ?
C1A F3A 1.322(6) . ?
C1A F1A 1.343(7) . ?
S1B O2B 1.429(4) . ?
S1B O1B 1.433(4) . ?
S1B O3B 1.443(3) . ?
S1B C1B 1.822(5) . ?
C1B F3B 1.319(7) . ?
C1B F1B 1.336(6) . ?
C1B F2B 1.338(7) . ?
