#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/18/4331871.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_4331871
loop_
_publ_author_name
'Singh, Priti'
'Sarkar, Biprajit'
'Sieger, Monika'
'Niemeyer, Mark'
'Fiedler, Jan'
'Záliš, Stanislav'
'Kaim, Wolfgang'
_publ_section_title
;
 The Metal−NO Interaction in the Redox Systems [Cl5Os(NO)]n-,n=
 1−3, andcis-[(bpy)2ClOs(NO)]2+/+:  Calculations,
 Structural, Electrochemical, and Spectroscopic Results
;
_journal_issue                   12
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4602
_journal_page_last               4609
_journal_paper_doi               10.1021/ic0517669
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C28 H26 Cl2.5 N2.5 O0.5 Os0.5 P'
_chemical_formula_weight         620.21
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 98.262(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.50560(10)
_cell_length_b                   19.4011(2)
_cell_length_c                   14.8581(2)
_cell_measurement_temperature    173(2)
_cell_volume                     2711.68(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_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  0.0602
_diffrn_reflns_av_sigmaI/netI    0.0217
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            59472
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         2.96
_exptl_absorpt_coefficient_mu    2.701
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1244
_refine_diff_density_max         0.440
_refine_diff_density_min         -1.192
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.581
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         6695
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.581
_refine_ls_R_factor_all          0.0211
_refine_ls_R_factor_gt           0.0183
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0209P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0536
_refine_ls_wR_factor_ref         0.0548
_reflns_number_gt                6160
_reflns_number_total             6695
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0517669sup1.cif
_cod_data_source_block           OsNO
_cod_original_cell_volume        2711.68(5)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C28 H26 Cl2.50 N2.50 O0.50 Os0.50 P'
_cod_database_code               4331871
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Os Os 0.0000 0.5000 0.5000 0.01393(4) Uani 1 2 d S . .
Cl1 Cl 0.05417(4) 0.382816(19) 0.53900(2) 0.01850(8) Uani 1 1 d . A .
Cl2 Cl 0.11602(4) 0.48859(2) 0.36852(3) 0.01739(8) Uani 1 1 d . A .
Cl3 Cl 0.20574(19) 0.53393(12) 0.58535(13) 0.0144(3) Uani 0.50 1 d P A 1
N1 N 0.1695(7) 0.5256(4) 0.5660(5) 0.0157(11) Uani 0.50 1 d P A 2
O1 O 0.2751(3) 0.54079(16) 0.60886(19) 0.0256(6) Uani 0.50 1 d P A 2
P P 0.34225(4) 0.804737(19) 0.56690(2) 0.01269(7) Uani 1 1 d . . .
C11 C 0.26210(15) 0.84814(8) 0.46590(9) 0.0171(3) Uani 1 1 d . . .
C12 C 0.14179(16) 0.88840(8) 0.46729(11) 0.0226(3) Uani 1 1 d . . .
H12A H 0.1028 0.8943 0.5222 0.017(4) Uiso 1 1 calc R . .
C13 C 0.07852(18) 0.92026(9) 0.38727(13) 0.0325(4) Uani 1 1 d . . .
H13A H -0.0041 0.9477 0.3876 0.038(5) Uiso 1 1 calc R . .
C14 C 0.1359(2) 0.91186(10) 0.30807(12) 0.0348(4) Uani 1 1 d . . .
H14A H 0.0911 0.9328 0.2536 0.041(6) Uiso 1 1 calc R . .
C15 C 0.25821(19) 0.87325(10) 0.30689(11) 0.0316(4) Uani 1 1 d . . .
H15A H 0.2985 0.8690 0.2522 0.050(7) Uiso 1 1 calc R . .
C16 C 0.32164(17) 0.84089(9) 0.38550(10) 0.0235(3) Uani 1 1 d . . .
H16A H 0.4050 0.8140 0.3849 0.047(6) Uiso 1 1 calc R . .
C21 C 0.41240(14) 0.72446(7) 0.53336(9) 0.0151(3) Uani 1 1 d . . .
C22 C 0.33240(16) 0.68427(8) 0.46611(10) 0.0199(3) Uani 1 1 d . . .
H22A H 0.2410 0.6994 0.4389 0.018(4) Uiso 1 1 calc R . .
C23 C 0.38674(19) 0.62258(9) 0.43943(12) 0.0252(4) Uani 1 1 d . . .
H23A H 0.3320 0.5949 0.3946 0.024(4) Uiso 1 1 calc R . .
C24 C 0.52160(18) 0.60106(9) 0.47826(12) 0.0256(3) Uani 1 1 d . . .
H24A H 0.5597 0.5592 0.4589 0.040(6) Uiso 1 1 calc R . .
C25 C 0.60024(18) 0.64043(9) 0.54502(12) 0.0246(4) Uani 1 1 d . . .
H25A H 0.6920 0.6253 0.5715 0.025(5) Uiso 1 1 calc R . .
C26 C 0.54623(15) 0.70174(8) 0.57352(10) 0.0194(3) Uani 1 1 d . . .
H26A H 0.6000 0.7282 0.6201 0.024(5) Uiso 1 1 calc R . .
C31 C 0.48570(14) 0.85486(7) 0.62486(9) 0.0143(3) Uani 1 1 d . . .
C32 C 0.55625(15) 0.90187(8) 0.57681(10) 0.0185(3) Uani 1 1 d . . .
H32A H 0.5226 0.9110 0.5146 0.024(5) Uiso 1 1 calc R . .
C33 C 0.67658(16) 0.93558(8) 0.62019(10) 0.0225(3) Uani 1 1 d . . .
H33A H 0.7255 0.9676 0.5875 0.036(5) Uiso 1 1 calc R . .
C34 C 0.72491(15) 0.92248(8) 0.71102(10) 0.0218(3) Uani 1 1 d . . .
H34A H 0.8072 0.9455 0.7403 0.019(4) Uiso 1 1 calc R . .
C35 C 0.65418(16) 0.87617(8) 0.75935(10) 0.0215(3) Uani 1 1 d . . .
H35A H 0.6879 0.8676 0.8217 0.032(5) Uiso 1 1 calc R . .
C36 C 0.53423(15) 0.84223(8) 0.71702(10) 0.0181(3) Uani 1 1 d . . .
H36A H 0.4853 0.8106 0.7502 0.023(4) Uiso 1 1 calc R . .
C41 C 0.20832(14) 0.79175(8) 0.63909(9) 0.0146(3) Uani 1 1 d . . .
C42 C 0.18082(15) 0.84391(8) 0.69922(10) 0.0202(3) Uani 1 1 d . . .
H42A H 0.2381 0.8842 0.7057 0.019(4) Uiso 1 1 calc R . .
C43 C 0.06924(16) 0.83632(9) 0.74928(11) 0.0254(3) Uani 1 1 d . . .
H43A H 0.0505 0.8712 0.7909 0.029(5) Uiso 1 1 calc R . .
C44 C -0.01496(16) 0.77751(10) 0.73830(11) 0.0246(3) Uani 1 1 d . . .
H44A H -0.0919 0.7727 0.7721 0.027(5) Uiso 1 1 calc R . .
C45 C 0.01175(15) 0.72616(9) 0.67894(10) 0.0226(3) Uani 1 1 d . . .
H45A H -0.0466 0.6862 0.6721 0.034(5) Uiso 1 1 calc R . .
C46 C 0.12442(15) 0.73276(8) 0.62886(10) 0.0182(3) Uani 1 1 d . . .
H46A H 0.1436 0.6973 0.5882 0.028(5) Uiso 1 1 calc R . .
N51 N -0.35480(19) 0.70123(9) 0.82270(13) 0.0467(4) Uani 1 1 d . . .
C52 C -0.27708(19) 0.70399(9) 0.88849(14) 0.0326(4) Uani 1 1 d . . .
C53 C -0.17704(18) 0.70815(10) 0.97100(13) 0.0343(4) Uani 1 1 d . . .
H53A H -0.0805 0.7126 0.9558 0.095(10) Uiso 1 1 calc R . .
H53B H -0.1835 0.6663 1.0071 0.080(9) Uiso 1 1 calc R . .
H53C H -0.1991 0.7484 1.0063 0.099(10) Uiso 1 1 calc R . .
N61 N 0.2750(2) 1.02296(11) 0.59807(13) 0.0441(4) Uani 1 1 d . . .
C62 C 0.34112(18) 1.02939(10) 0.66752(13) 0.0289(4) Uani 1 1 d . . .
C63 C 0.42415(18) 1.03796(11) 0.75648(12) 0.0328(4) Uani 1 1 d . . .
H63A H 0.4422 1.0871 0.7683 0.060(7) Uiso 1 1 calc R . .
H63B H 0.5149 1.0136 0.7584 0.049(8) Uiso 1 1 calc R . .
H63C H 0.3716 1.0190 0.8029 0.054(7) Uiso 1 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'
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
N1 Os N1 180.000(1) . 3_566
N1 Os Cl3 177.9(3) . 3_566
N1 Os Cl3 2.1(3) 3_566 3_566
N1 Os Cl3 2.1(3) . .
N1 Os Cl3 177.9(3) 3_566 .
Cl3 Os Cl3 180.0 3_566 .
N1 Os Cl1 90.8(3) . 3_566
N1 Os Cl1 89.2(3) 3_566 3_566
Cl3 Os Cl1 90.12(6) 3_566 3_566
Cl3 Os Cl1 89.88(6) . 3_566
N1 Os Cl1 89.2(3) . .
N1 Os Cl1 90.8(3) 3_566 .
Cl3 Os Cl1 89.88(6) 3_566 .
Cl3 Os Cl1 90.12(6) . .
Cl1 Os Cl1 180.0 3_566 .
N1 Os Cl2 90.7(3) . 3_566
N1 Os Cl2 89.3(3) 3_566 3_566
Cl3 Os Cl2 91.25(6) 3_566 3_566
Cl3 Os Cl2 88.75(6) . 3_566
Cl1 Os Cl2 90.083(13) 3_566 3_566
Cl1 Os Cl2 89.917(13) . 3_566
N1 Os Cl2 89.3(3) . .
N1 Os Cl2 90.7(3) 3_566 .
Cl3 Os Cl2 88.75(6) 3_566 .
Cl3 Os Cl2 91.25(6) . .
Cl1 Os Cl2 89.917(13) 3_566 .
Cl1 Os Cl2 90.083(13) . .
Cl2 Os Cl2 180.0 3_566 .
O1 N1 Os 178.5(8) . .
C31 P C11 110.50(7) . .
C31 P C21 108.50(6) . .
C11 P C21 107.80(7) . .
C31 P C41 110.17(7) . .
C11 P C41 108.26(7) . .
C21 P C41 111.58(7) . .
C12 C11 C16 120.28(14) . .
C12 C11 P 120.27(12) . .
C16 C11 P 119.45(12) . .
C11 C12 C13 119.43(16) . .
C14 C13 C12 120.03(17) . .
C13 C14 C15 120.75(15) . .
C16 C15 C14 119.91(17) . .
C15 C16 C11 119.56(16) . .
C26 C21 C22 119.76(14) . .
C26 C21 P 120.52(11) . .
C22 C21 P 119.72(11) . .
C23 C22 C21 119.90(15) . .
C22 C23 C24 120.00(16) . .
C25 C24 C23 120.14(16) . .
C24 C25 C26 120.49(15) . .
C25 C26 C21 119.68(14) . .
C32 C31 C36 120.09(13) . .
C32 C31 P 119.98(11) . .
C36 C31 P 119.70(11) . .
C31 C32 C33 119.72(14) . .
C34 C33 C32 119.99(14) . .
C35 C34 C33 120.47(14) . .
C34 C35 C36 120.14(14) . .
C35 C36 C31 119.58(14) . .
C46 C41 C42 120.54(13) . .
C46 C41 P 119.65(11) . .
C42 C41 P 119.55(11) . .
C43 C42 C41 119.51(15) . .
C42 C43 C44 119.72(15) . .
C45 C44 C43 120.84(14) . .
C44 C45 C46 120.07(15) . .
C41 C46 C45 119.30(14) . .
N51 C52 C53 179.0(2) . .
N61 C62 C63 179.4(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Os N1 1.830(5) .
Os N1 1.830(5) 3_566
Os Cl3 2.2701(15) 3_566
Os Cl3 2.2701(15) .
Os Cl1 2.3841(4) 3_566
Os Cl1 2.3841(4) .
Os Cl2 2.3877(4) 3_566
Os Cl2 2.3877(4) .
N1 O1 1.147(4) .
P C31 1.7914(14) .
P C11 1.7924(14) .
P C21 1.7929(15) .
P C41 1.7965(14) .
C11 C12 1.387(2) .
C11 C16 1.401(2) .
C12 C13 1.397(2) .
C13 C14 1.376(3) .
C14 C15 1.386(3) .
C15 C16 1.386(2) .
C21 C26 1.397(2) .
C21 C22 1.402(2) .
C22 C23 1.384(2) .
C23 C24 1.392(3) .
C24 C25 1.383(3) .
C25 C26 1.386(2) .
C31 C32 1.389(2) .
C31 C36 1.4022(19) .
C32 C33 1.393(2) .
C33 C34 1.385(2) .
C34 C35 1.383(2) .
C35 C36 1.387(2) .
C41 C46 1.391(2) .
C41 C42 1.399(2) .
C42 C43 1.388(2) .
C43 C44 1.390(2) .
C44 C45 1.378(2) .
C45 C46 1.395(2) .
N51 C52 1.139(2) .
C52 C53 1.442(3) .
N61 C62 1.135(3) .
C62 C63 1.449(3) .
