#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/00/2010083.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_2010083
loop_
_publ_author_name
'Bruhn, Clemens'
'Preetz, Wilhelm'
_publ_section_title
;
 Dipyridiniomethane cis-dichlorotetrafluoroosmate(IV)
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1555
_journal_page_last               1557
_journal_paper_doi               10.1107/S010827019400627X
_journal_volume                  50
_journal_year                    1994
_chemical_formula_moiety         'C11 H12 Cl2 F4 N2 Os1'
_chemical_formula_structural     '[(C5H5N)CH2][OsF4Cl2]'
_chemical_formula_sum            'C11 H12 Cl2 F4 N2 Os'
_chemical_formula_weight         509.33
_chemical_name_systematic
;
cis-N,N'-dipyridiniomethane Dichlorotetrafluoroosmate(IV)
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.172(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.9689(3)
_cell_length_b                   6.7658(3)
_cell_length_c                   28.994(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11.897
_cell_measurement_theta_min      6.490
_cell_volume                     1367.07(13)
_computing_cell_refinement       CAD4-PC
_computing_data_collection       'CAD4-PC (Enraf-Nonius, 1993)'
_computing_data_reduction        'MolEN (Fair, 1990)'
_computing_molecular_graphics    'ORTEPII (Johnson 1976)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1994)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'CAD4-Turbo four-circle'
_diffrn_measurement_method       ω/2θ
_diffrn_radiation_monochromator  Zr
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_av_sigmaI/netI    0.0197
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            2612
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.81
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  240
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    9.754
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.69
_exptl_absorpt_correction_type   'empirical, \y sans'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.475
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.410
_refine_diff_density_min         -2.181
_refine_ls_extinction_coef       0.0363(12)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1994)'
_refine_ls_goodness_of_fit_all   1.186
_refine_ls_goodness_of_fit_obs   1.159
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         2384
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.187
_refine_ls_restrained_S_obs      1.159
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_obs          0.0294
_refine_ls_shift/esd_max         0.006
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
; calc w = 1/[\s^2^(F~o~^2^) + (0.0600P)^2^
+3.3849P] where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.1687
_refine_ls_wR_factor_obs         0.0846
_reflns_number_observed          2150
_reflns_number_total             2402
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            bk1048.cif
_cod_data_source_block           cf4a2
_cod_original_cell_volume        1367.07(14)
_cod_original_sg_symbol_Hall     '-P 2yn'
_cod_original_sg_symbol_H-M      'P 2/n'
_cod_original_formula_sum        'C11 H12 Cl2 F4 N2 Os1'
_cod_database_code               2010083
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z-1/2'
loop_
_atom_site_label
_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_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_group
_atom_site_type_symbol
Os 0.89761(3) 0.38209(3) 0.364512(8) 0.0197(2) Uani d . 1 . Os
Cl1 0.5903(3) 0.3930(2) 0.39527(7) 0.0280(4) Uani d . 1 . Cl
Cl2 1.0352(3) 0.3050(4) 0.43582(7) 0.0446(5) Uani d . 1 . Cl
F1 0.7927(7) 0.4366(7) 0.3038(2) 0.0410(10) Uani d . 1 . F
F2 1.1490(7) 0.3737(6) 0.3350(2) 0.0391(12) Uani d . 1 . F
F3 0.9363(7) 0.6619(7) 0.3739(2) 0.0430(11) Uani d . 1 . F
F4 0.8684(7) 0.1044(5) 0.3503(2) 0.0344(10) Uani d . 1 . F
CM 0.2936(10) 0.9645(11) 0.3684(3) 0.0300(15) Uani d . 1 . C
HM1 0.278(15) 1.099(13) 0.375(4) 0.041(19) Uiso d . 1 . H
HM2 0.174(15) 0.901(12) 0.368(3) 0.041(19) Uiso d . 1 . H
C11 0.5836(10) 0.9009(9) 0.4141(3) 0.0245(14) Uani d . 1 . C
C12 0.6680(12) 0.8394(11) 0.4554(3) 0.034(2) Uani d . 1 . C
C13 0.5558(11) 0.7548(11) 0.4890(3) 0.032(2) Uani d . 1 . C
C14 0.3625(11) 0.7249(11) 0.4815(3) 0.034(2) Uani d . 1 . C
C15 0.2857(10) 0.7840(11) 0.4405(3) 0.0282(15) Uani d . 1 . C
N1 0.3935(9) 0.8748(7) 0.4088(2) 0.0209(13) Uani d . 1 . N
H11 0.662(11) 0.966(12) 0.392(3) 0.029(7) Uiso d . 1 . H
H12 0.778(14) 0.860(11) 0.461(3) 0.029(7) Uiso d . 1 . H
H13 0.617(11) 0.716(12) 0.516(3) 0.029(7) Uiso d . 1 . H
H14 0.281(12) 0.657(11) 0.505(3) 0.029(7) Uiso d . 1 . H
H15 0.168(11) 0.765(12) 0.430(3) 0.029(7) Uiso d . 1 . H
C21 0.4069(11) 0.7326(11) 0.3100(3) 0.031(2) Uani d . 1 . C
C22 0.4790(11) 0.6955(12) 0.2672(3) 0.037(2) Uani d . 1 . C
C23 0.5291(11) 0.8499(13) 0.2384(3) 0.036(2) Uani d . 1 . C
C24 0.5131(11) 1.0410(12) 0.2548(3) 0.034(2) Uani d . 1 . C
C25 0.4464(11) 1.0736(11) 0.2979(3) 0.032(2) Uani d . 1 . C
N2 0.3900(8) 0.9216(9) 0.3248(2) 0.0240(12) Uani d . 1 . N
H21 0.365(12) 0.656(13) 0.329(3) 0.029(7) Uiso d . 1 . H
H22 0.471(12) 0.585(12) 0.259(3) 0.029(7) Uiso d . 1 . H
H23 0.575(11) 0.822(12) 0.209(3) 0.029(7) Uiso d . 1 . H
H24 0.549(12) 1.132(11) 0.233(3) 0.029(7) Uiso d . 1 . H
H25 0.433(11) 1.204(14) 0.306(3) 0.029(7) Uiso d . 1 . H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F .0171 .0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl .1484 .1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 '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
F3 Os F4 175.4(2) yes
F3 Os F1 89.6(2) yes
F4 Os F1 87.3(2) yes
F3 Os F2 88.0(2) yes
F4 Os F2 88.4(2) yes
F1 Os F2 86.8(2) yes
F3 Os Cl1 92.48(15) yes
F4 Os Cl1 90.92(14) yes
F1 Os Cl1 89.83(15) yes
F2 Os Cl1 176.6(2) yes
F3 Os Cl2 92.2(2) yes
F4 Os Cl2 90.8(2) yes
F1 Os Cl2 177.00(15) yes
F2 Os Cl2 90.9(2) yes
Cl1 Os Cl2 92.51(7) yes
N2 CM N1 112.6(6) yes
N2 CM HM1 116.(6) ?
N1 CM HM1 106.(6) ?
N2 CM HM2 109.(6) ?
N1 CM HM2 103.(6) ?
HM1 CM HM2 110.(8) ?
N1 C11 C12 118.1(7) yes
N1 C11 H11 124.(5) ?
C12 C11 H11 118.(5) ?
C13 C12 C11 119.5(7) yes
C13 C12 H12 118.(7) ?
C11 C12 H12 122.(7) ?
C12 C13 C14 120.4(7) yes
C12 C13 H13 117.(5) ?
C14 C13 H13 123.(5) ?
C15 C14 C13 118.5(7) yes
C15 C14 H14 120.(5) ?
C13 C14 H14 121.(5) ?
N1 C15 C14 120.9(7) yes
N1 C15 H15 111.(5) ?
C14 C15 H15 128.(5) ?
C15 N1 C11 122.5(6) yes
C15 N1 CM 117.7(6) yes
C11 N1 CM 119.6(6) yes
N2 C21 C22 119.7(7) yes
N2 C21 H21 111.(6) ?
C22 C21 H21 129.(6) ?
C21 C22 C23 120.3(8) yes
C21 C22 H22 114.(7) ?
C23 C22 H22 124.(7) ?
C24 C23 C22 118.5(8) yes
C24 C23 H23 122.(5) ?
C22 C23 H23 120.(5) ?
C25 C24 C23 119.9(7) yes
C25 C24 H24 129.(5) ?
C23 C24 H24 111.(5) ?
C24 C25 N2 120.8(7) yes
C24 C25 H25 116.(5) ?
N2 C25 H25 123.(5) ?
C25 N2 C21 120.6(7) yes
C25 N2 CM 119.0(6) yes
C21 N2 CM 120.2(6) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Os F3 . 1.931(5) yes
Os F4 . 1.934(4) yes
Os F1 . 1.941(4) yes
Os F2 . 1.953(5) yes
Os Cl1 . 2.324(2) yes
Os Cl2 . 2.335(2) yes
CM N2 . 1.461(9) yes
CM N1 . 1.492(9) yes
CM HM1 . 0.94(9) ?
CM HM2 . 0.94(10) ?
C11 N1 . 1.345(10) yes
C11 C12 . 1.395(12) yes
C11 H11 . 0.95(9) ?
C12 C13 . 1.376(11) yes
C12 H12 . 0.80(10) ?
C13 C14 . 1.379(11) yes
C13 H13 . 0.93(8) ?
C14 C15 . 1.361(11) yes
C14 H14 . 1.00(9) ?
C15 N1 . 1.338(9) yes
C15 H15 . 0.89(8) ?
C21 N2 . 1.355(9) yes
C21 C22 . 1.362(12) yes
C21 H21 . 0.81(9) ?
C22 C23 . 1.383(12) yes
C22 H22 . 0.78(8) ?
C23 C24 . 1.383(12) yes
C23 H23 . 0.94(9) ?
C24 C25 . 1.350(11) yes
C24 H24 . 0.92(8) ?
C25 N2 . 1.351(9) yes
C25 H25 . 0.92(9) ?
