#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/92/2209284.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# 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_2209284
loop_
_publ_author_name
'Sun, Bai-Wang'
'Liu, Hui'
'Yang, Guo-Ying'
'Ang. Siau Gek'
'Ang, How Ghee'
_publ_section_title
;
 Bis[1,3-bis(pentafluorophenyl)triazenido]tricarbonylosmium(II)
;
_journal_coeditor_code           RN6079
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1329
_journal_page_last               m1331
_journal_paper_doi               10.1107/S1600536806017430
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Os (C12 F10 N3)2 (C O)3]'
_chemical_formula_moiety         'C27 F20 N6 O3 Os'
_chemical_formula_sum            'C27 F20 N6 O3 Os'
_chemical_formula_weight         1026.53
_chemical_name_systematic
;
Bis[1,3-bis(pentafluorophenyl)triazenido]tricarbonylosmium
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.4352(7)
_cell_length_b                   14.7412(8)
_cell_length_c                   16.5795(9)
_cell_measurement_reflns_used    3891
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      1.85
_cell_volume                     3039.2(3)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1998)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker AXS SMART CCD'
_diffrn_measurement_method       'φ and ω'
_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  0.0274
_diffrn_reflns_av_sigmaI/netI    0.0406
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21297
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.85
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.364
_exptl_absorpt_correction_T_max  0.648
_exptl_absorpt_correction_T_min  0.462
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.243
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.030
_refine_diff_density_min         -0.552
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   -0.002(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         6961
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0238
_refine_ls_R_factor_gt           0.0222
_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)+(0.0328P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0553
_refine_ls_wR_factor_ref         0.0654
_reflns_number_gt                6717
_reflns_number_total             6961
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            rn6079.cif
_cod_data_source_block           I
_cod_database_code               2209284
_cod_database_fobs_code          2209284
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
Os Os1 0.788498(11) 0.283724(10) 0.851392(8) 0.02578(5) Uani d 1
F F45 0.7155(3) 0.2774(2) 0.60450(18) 0.0634(9) Uani d 1
F F44 0.8494(5) 0.2384(3) 0.4803(2) 0.0951(15) Uani d 1
F F43 1.0071(4) 0.1128(4) 0.4985(3) 0.116(2) Uani d 1
F F42 1.0304(3) 0.0263(3) 0.6426(3) 0.0899(14) Uani d 1
F F41 0.9049(3) 0.0699(2) 0.7670(2) 0.0530(8) Uani d 1
F F35 0.4796(2) 0.1363(2) 0.64233(19) 0.0532(7) Uani d 1
F F34 0.2721(3) 0.0977(3) 0.63251(19) 0.0618(9) Uani d 1
F F33 0.1408(2) 0.1194(2) 0.7621(2) 0.0575(8) Uani d 1
F F32 0.2240(2) 0.1787(2) 0.90412(18) 0.0506(7) Uani d 1
F F31 0.4341(2) 0.2118(2) 0.91791(15) 0.0424(6) Uani d 1
F F21 1.0444(2) 0.3158(2) 0.79188(19) 0.0507(7) Uani d 1
F F22 1.2057(3) 0.3228(2) 0.6861(2) 0.0649(9) Uani d 1
F F23 1.1762(3) 0.4016(3) 0.5384(2) 0.0749(11) Uani d 1
F F24 0.9801(3) 0.4678(2) 0.49993(18) 0.0626(9) Uani d 1
F F25 0.8175(2) 0.4608(2) 0.60188(18) 0.0524(8) Uani d 1
F F15 0.5707(2) 0.4445(2) 0.65793(18) 0.0502(7) Uani d 1
F F14 0.3605(3) 0.4824(2) 0.6661(2) 0.0634(9) Uani d 1
F F13 0.2510(2) 0.4611(3) 0.8070(3) 0.0658(10) Uani d 1
F F12 0.3550(2) 0.4052(2) 0.9411(2) 0.0577(8) Uani d 1
F F11 0.5683(2) 0.36965(19) 0.93483(17) 0.0404(6) Uani d 1
O O1 0.6580(3) 0.1765(3) 0.9743(2) 0.0470(9) Uani d 1
O O2 0.8440(3) 0.4283(3) 0.9766(2) 0.0533(10) Uani d 1
O O3 0.9791(3) 0.1689(3) 0.9038(2) 0.0506(9) Uani d 1
N N1' 0.7404(3) 0.1983(2) 0.7556(2) 0.0292(8) Uani d 1
N N2' 0.6398(3) 0.1736(2) 0.7410(2) 0.0293(7) Uani d 1
N N3' 0.5743(3) 0.1986(2) 0.7959(2) 0.0292(8) Uani d 1
N N3 0.8408(3) 0.3724(2) 0.7572(2) 0.0285(7) Uani d 1
N N2 0.7491(3) 0.4142(2) 0.7441(2) 0.0286(7) Uani d 1
N N1 0.6845(3) 0.3801(2) 0.7984(2) 0.0284(7) Uani d 1
C C1 0.7033(3) 0.2162(3) 0.9275(2) 0.0334(8) Uani d 1
C C2 0.8255(4) 0.3735(3) 0.9318(3) 0.0361(10) Uani d 1
C C3 0.9082(3) 0.2102(3) 0.8828(2) 0.0344(9) Uani d 1
C C45 0.7950(5) 0.2165(3) 0.6147(3) 0.0450(10) Uani d 1
C C44 0.8633(6) 0.1967(4) 0.5510(3) 0.0652(18) Uani d 1
C C43 0.9428(5) 0.1331(5) 0.5620(4) 0.0660(18) Uani d 1
C C42 0.9561(4) 0.0912(5) 0.6336(4) 0.0593(17) Uani d 1
C C41 0.8920(4) 0.1133(4) 0.6989(3) 0.0433(12) Uani d 1
C C46 0.8073(4) 0.1766(3) 0.6886(3) 0.0346(10) Uani d 1
C C36 0.4669(3) 0.1745(3) 0.7814(3) 0.0282(8) Uani d 1
C C35 0.4211(4) 0.1464(3) 0.7087(3) 0.0344(9) Uani d 1
C C34 0.3128(4) 0.1264(3) 0.7034(3) 0.0394(10) Uani d 1
C C33 0.2466(4) 0.1374(3) 0.7680(3) 0.0385(10) Uani d 1
C C32 0.2876(4) 0.1671(3) 0.8406(3) 0.0351(9) Uani d 1
C C31 0.3964(3) 0.1845(3) 0.8456(3) 0.0315(8) Uani d 1
C C21 1.0256(4) 0.3538(3) 0.7200(3) 0.0373(10) Uani d 1
C C22 1.1106(4) 0.3572(3) 0.6663(3) 0.0435(12) Uani d 1
C C23 1.0952(5) 0.3958(3) 0.5913(3) 0.0466(12) Uani d 1
C C24 0.9972(5) 0.4310(3) 0.5725(3) 0.0424(11) Uani d 1
C C25 0.9119(4) 0.4268(3) 0.6254(3) 0.0372(10) Uani d 1
C C26 0.9241(3) 0.3863(3) 0.7015(3) 0.0286(8) Uani d 1
C C16 0.5761(3) 0.4062(3) 0.7968(3) 0.0296(9) Uani d 1
C C15 0.5204(4) 0.4357(3) 0.7291(3) 0.0375(10) Uani d 1
C C14 0.4112(4) 0.4539(3) 0.7325(3) 0.0434(11) Uani d 1
C C13 0.3560(4) 0.4435(3) 0.8044(4) 0.0446(12) Uani d 1
C C12 0.4094(4) 0.4148(3) 0.8711(3) 0.0401(11) Uani d 1
C C11 0.5174(4) 0.3976(3) 0.8684(3) 0.0326(9) Uani d 1
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'
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'
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_publ_flag
C3 Os1 C1 87.53(18) yes
C3 Os1 C2 90.9(2) y
C1 Os1 C2 91.89(19) y
C3 Os1 N1 166.00(16) y
C1 Os1 N1 106.47(16) y
C2 Os1 N1 88.38(18) y
C3 Os1 N1' 95.02(17) y
C1 Os1 N1' 91.62(16) y
C2 Os1 N1' 173.28(18) y
N1 Os1 N1' 85.13(13) y
C3 Os1 N3 107.96(16) y
C1 Os1 N3 164.26(15) y
C2 Os1 N3 90.74(16) y
N1 Os1 N3 58.09(14) yes
N1' Os1 N3 84.35(14) y
N2' N1' C46 110.3(3) ?
N2' N1' Os1 124.6(3) ?
C46 N1' Os1 123.6(3) ?
N3' N2' N1' 113.1(3) yes
N2' N3' C36 114.3(4) ?
N2 N3 C26 117.6(3) ?
N2 N3 Os1 98.2(2) ?
C26 N3 Os1 142.7(3) ?
N1 N2 N3 103.8(3) yes
N2 N1 C16 118.2(4) ?
N2 N1 Os1 99.7(2) ?
C16 N1 Os1 141.3(3) ?
O1 C1 Os1 176.5(4) ?
O2 C2 Os1 176.8(5) ?
O3 C3 Os1 177.4(4) ?
F45 C45 C46 118.8(4) ?
F45 C45 C44 119.6(5) ?
C46 C45 C44 121.6(5) ?
F44 C44 C43 121.6(6) ?
F44 C44 C45 119.5(7) ?
C43 C44 C45 118.9(6) ?
C42 C43 F43 120.7(7) ?
C42 C43 C44 121.2(5) ?
F43 C43 C44 118.1(7) ?
F42 C42 C43 120.7(5) ?
F42 C42 C41 118.6(6) ?
C43 C42 C41 120.7(6) ?
F41 C41 C46 121.2(4) ?
F41 C41 C42 119.3(5) ?
C46 C41 C42 119.3(5) ?
C45 C46 C41 118.3(4) ?
C45 C46 N1' 122.5(4) ?
C41 C46 N1' 119.2(4) ?
C31 C36 C35 116.0(4) ?
C31 C36 N3' 116.3(4) ?
C35 C36 N3' 127.7(4) ?
F35 C35 C34 117.2(4) ?
F35 C35 C36 121.8(4) ?
C34 C35 C36 121.0(4) ?
F34 C34 C33 119.8(4) ?
F34 C34 C35 119.3(5) ?
C33 C34 C35 120.9(4) ?
F33 C33 C34 120.7(5) ?
F33 C33 C32 119.2(4) ?
C34 C33 C32 120.1(4) ?
F32 C32 C31 120.8(4) ?
F32 C32 C33 120.9(4) ?
C31 C32 C33 118.3(4) ?
F31 C31 C32 116.8(4) ?
F31 C31 C36 119.6(3) ?
C32 C31 C36 123.6(4) ?
F21 C21 C22 117.1(4) ?
F21 C21 C26 120.1(4) ?
C22 C21 C26 122.8(4) ?
F22 C22 C23 120.3(4) ?
F22 C22 C21 120.5(4) ?
C23 C22 C21 119.2(4) ?
F23 C23 C24 120.0(5) ?
F23 C23 C22 120.7(5) ?
C24 C23 C22 119.2(4) ?
F24 C24 C23 120.3(5) ?
F24 C24 C25 118.0(5) ?
C23 C24 C25 121.7(4) ?
F25 C25 C24 118.2(4) ?
F25 C25 C26 121.2(4) ?
C24 C25 C26 120.6(4) ?
C21 C26 C25 116.4(4) ?
C21 C26 N3 118.5(4) ?
C25 C26 N3 125.0(4) ?
C15 C16 C11 117.0(4) ?
C15 C16 N1 125.5(4) ?
C11 C16 N1 117.4(4) ?
F15 C15 C14 118.3(4) ?
F15 C15 C16 120.5(4) ?
C14 C15 C16 121.1(5) ?
F14 C14 C13 120.7(4) ?
F14 C14 C15 119.3(5) ?
C13 C14 C15 120.0(5) ?
F13 C13 C12 120.9(5) ?
F13 C13 C14 119.5(5) ?
C12 C13 C14 119.6(4) ?
F12 C12 C13 119.3(4) ?
F12 C12 C11 120.0(5) ?
C13 C12 C11 120.7(5) ?
F11 C11 C12 119.7(4) ?
F11 C11 C16 118.7(4) ?
C12 C11 C16 121.6(4) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Os1 C3 1.913(4) y
Os1 C1 1.925(4) y
Os1 C2 1.934(5) y
Os1 N1 2.113(3) yes
Os1 N1' 2.113(4) yes
Os1 N3 2.138(4) yes
F45 C45 1.346(6) ?
F44 C44 1.335(8) ?
F43 C43 1.356(6) ?
F42 C42 1.338(7) ?
F41 C41 1.307(7) ?
F35 C35 1.327(5) ?
F34 C34 1.348(5) ?
F33 C33 1.346(5) ?
F32 C32 1.328(5) ?
F31 C31 1.348(5) ?
F21 C21 1.338(5) ?
F22 C22 1.327(6) ?
F23 C23 1.339(6) ?
F24 C24 1.337(6) ?
F25 C25 1.335(6) ?
F15 C15 1.342(6) ?
F14 C14 1.335(6) ?
F13 C13 1.332(6) ?
F12 C12 1.350(6) ?
F11 C11 1.335(5) ?
O1 C1 1.123(5) ?
O2 C2 1.122(6) ?
O3 C3 1.127(5) ?
N1' N2' 1.325(5) y
N1' C46 1.424(5) yes
N2' N3' 1.276(5) y
N3' C36 1.404(5) yes
N3 N2 1.315(5) y
N3 C26 1.402(5) yes
N2 N1 1.307(5) y
N1 C16 1.402(5) yes
C45 C46 1.368(7) ?
C45 C44 1.386(8) ?
C44 C43 1.375(10) ?
C43 C42 1.348(10) ?
C42 C41 1.385(7) ?
C41 C46 1.417(7) ?
C36 C31 1.387(6) ?
C36 C35 1.395(6) ?
C35 C34 1.382(6) ?
C34 C33 1.361(7) ?
C33 C32 1.379(7) ?
C32 C31 1.380(6) ?
C21 C22 1.383(6) ?
C21 C26 1.385(6) ?
C22 C23 1.380(7) ?
C23 C24 1.360(8) ?
C24 C25 1.378(7) ?
C25 C26 1.404(6) ?
C16 C15 1.389(6) ?
C16 C11 1.400(6) ?
C15 C14 1.386(7) ?
C14 C13 1.384(8) ?
C13 C12 1.358(8) ?
C12 C11 1.368(7) ?
