#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2003575.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_2003575
loop_
_publ_author_name
'Bruhn, C.'
'Preetz, W.'
_publ_section_title
;
 <i>fac</i>- and <i>mer</i>-Dipyridiniomethane
 Trichlorotrifluoroosmate(IV), <i>fac</i>- and
 <i>mer</i>-[(C~5~H~5~N)~2~CH~2~][OsCl~3~F~3~]
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1112
_journal_page_last               1116
_journal_volume                  51
_journal_year                    1995
_chemical_formula_structural     mer-[(C~5~H~5~N)~2~CH~2~][OsF~3~Cl~3~]
_chemical_formula_sum            'C11 H12 Cl3 F3 N2 Os'
_chemical_formula_weight         525.78
_chemical_name_common
;
 mer-Dipyridiniomethane-Trifluorotrichloroosmate(IV)
;
_chemical_name_systematic
;
 mer-N,N'-methylenedipyridinium trichlorotrifluoroosmate(IV)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 97.357(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.676(5)
_cell_length_b                   14.046(3)
_cell_length_c                   10.476(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11.79
_cell_measurement_theta_min      4.18
_cell_volume                     1412.1(9)
_computing_cell_refinement
;
CAD4-PC (Enraf-Nonius, 1993)
;
_computing_data_collection
;
CAD4-PC (Enraf-Nonius, 1993)
;
_computing_data_reduction        'MolEN (Fair, 1990)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SIR92 (Altomare et al, 1992)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device
;
Enraf-Nonius CAD4-Turbo four-circle
;
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0166
_diffrn_reflns_av_sigmaI/netI    0.0311
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2627
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.44
_diffrn_standards_decay_%        2.1
_diffrn_standards_interval_count 400
_diffrn_standards_interval_time  250
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    9.620
_exptl_absorpt_correction_T_max  0.9987
_exptl_absorpt_correction_T_min  0.6329
_exptl_absorpt_correction_type   'empirical (\y scans)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    2.473
_exptl_crystal_description       prism
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         .518
_refine_diff_density_min         -.537
_refine_ls_extinction_coef       0.00092(8)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   1.139
_refine_ls_goodness_of_fit_obs   1.094
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         2474
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.139
_refine_ls_restrained_S_obs      1.094
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_obs          0.0183
_refine_ls_shift/esd_max         -0.001
_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^) + (0.0142P)^2^ + 0.4674P]
  where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.0453
_refine_ls_wR_factor_obs         0.0390
_reflns_number_observed          2033
_reflns_number_total             2474
_reflns_observed_criterion       >2sigma(I)
_[local]_cod_data_source_file    jz1030.cif
_[local]_cod_data_source_block   mosf3a2
_[local]_cod_cif_authors_sg_H-M  'P 21/n'
_cod_database_code               2003575
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Os 0.02133(11) 0.02017(10) 0.02162(10) -0.00287(9) 0.00042(7) 0.00211(8)
Cl1 0.0350(7) 0.0245(6) 0.0371(6) -0.0091(5) 0.0033(5) 0.0025(5)
Cl2 0.0354(7) 0.0333(7) 0.0585(8) 0.0003(6) 0.0211(6) 0.0038(7)
Cl3 0.0392(7) 0.0438(8) 0.0470(8) 0.0012(7) 0.0173(6) -0.0044(7)
F1 0.040(2) 0.046(2) 0.0295(15) 0.0004(15) -0.0069(13) 0.0028(13)
F2 0.043(2) 0.024(2) 0.052(2) -0.0089(14) 0.0072(15) 0.0005(13)
F3 0.045(2) 0.040(2) 0.034(2) -0.0109(15) -0.0135(14) 0.0066(14)
N1 0.034(2) 0.024(2) 0.020(2) 0.003(2) 0.004(2) -0.001(2)
N2 0.022(2) 0.030(2) 0.030(2) -0.001(2) 0.004(2) 0.000(2)
CM 0.028(3) 0.039(3) 0.031(3) -0.005(3) 0.001(2) -0.006(2)
C11 0.058(4) 0.031(3) 0.034(3) 0.010(3) 0.009(3) -0.005(2)
C12 0.054(4) 0.063(4) 0.031(3) 0.033(4) 0.002(3) -0.004(3)
C13 0.032(3) 0.101(6) 0.023(3) 0.014(4) 0.004(3) -0.010(3)
C14 0.039(3) 0.056(4) 0.030(3) -0.006(3) 0.007(2) -0.005(3)
C15 0.037(3) 0.033(3) 0.027(3) -0.004(3) 0.003(2) 0.003(2)
C21 0.025(3) 0.027(3) 0.038(3) -0.002(2) 0.002(2) 0.003(2)
C22 0.033(3) 0.035(3) 0.034(3) -0.005(2) 0.003(2) 0.004(2)
C23 0.032(3) 0.044(3) 0.037(3) -0.008(3) 0.008(2) -0.013(3)
C24 0.044(3) 0.034(3) 0.051(3) 0.003(3) 0.004(3) -0.010(3)
C25 0.041(3) 0.028(3) 0.041(3) 0.007(3) 0.005(3) 0.007(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_occupancy
_atom_site_type_symbol
Os 0.44963(2) 0.225211(13) 0.55497(2) 0.02124(8) Uani d 1 Os
Cl1 0.52155(13) 0.37830(9) 0.53482(12) 0.0323(3) Uani d 1 Cl
Cl2 0.26497(14) 0.27513(10) 0.65670(14) 0.0411(3) Uani d 1 Cl
Cl3 0.62901(14) 0.16791(10) 0.45067(13) 0.0423(3) Uani d 1 Cl
F1 0.5627(3) 0.2095(2) 0.7206(3) 0.0395(7) Uani d 1 F
F2 0.3839(3) 0.0931(2) 0.5714(3) 0.0398(7) Uani d 1 F
F3 0.3345(3) 0.2371(2) 0.3892(3) 0.0414(8) Uani d 1 F
N1 0.6841(4) 0.5026(3) 0.8098(3) 0.0261(9) Uani d 1 N
N2 0.8449(4) 0.4624(3) 0.6601(4) 0.0275(9) Uani d 1 N
CM 0.8323(5) 0.4957(4) 0.7934(5) 0.0328(12) Uani d 1 C
C11 0.6200(7) 0.5884(4) 0.7916(5) 0.0407(14) Uani d 1 C
C12 0.4815(7) 0.5958(5) 0.8046(5) 0.050(2) Uani d 1 C
C13 0.4108(7) 0.5178(6) 0.8396(5) 0.052(2) Uani d 1 C
C14 0.4773(6) 0.4304(5) 0.8561(5) 0.0418(14) Uani d 1 C
C15 0.6148(6) 0.4248(4) 0.8400(5) 0.0323(12) Uani d 1 C
C21 0.8126(5) 0.5226(4) 0.5602(5) 0.0305(11) Uani d 1 C
C22 0.8210(6) 0.4917(4) 0.4376(5) 0.0343(12) Uani d 1 C
C23 0.8646(5) 0.3999(4) 0.4177(5) 0.0375(13) Uani d 1 C
C24 0.8983(6) 0.3411(4) 0.5213(6) 0.0431(14) Uani d 1 C
C25 0.8866(6) 0.3729(4) 0.6428(5) 0.0367(13) Uani d 1 C
HM1 0.877(6) 0.445(4) 0.862(5) 0.051(17) Uiso d 1 H
HM2 0.868(5) 0.559(3) 0.796(4) 0.019(12) Uiso d 1 H
H11 0.684(6) 0.641(5) 0.776(6) 0.058(19) Uiso d 1 H
H12 0.436(7) 0.660(5) 0.800(6) 0.06(2) Uiso d 1 H
H13 0.328(7) 0.522(4) 0.858(6) 0.053(19) Uiso d 1 H
H14 0.433(7) 0.376(5) 0.876(7) 0.08(2) Uiso d 1 H
H15 0.663(6) 0.370(4) 0.857(5) 0.047(17) Uiso d 1 H
H21 0.788(6) 0.584(4) 0.588(5) 0.050(17) Uiso d 1 H
H22 0.809(5) 0.535(4) 0.371(5) 0.030(14) Uiso d 1 H
H23 0.879(7) 0.371(5) 0.330(7) 0.08(2) Uiso d 1 H
H24 0.936(6) 0.272(5) 0.506(6) 0.058(18) Uiso d 1 H
H25 0.909(6) 0.335(4) 0.714(5) 0.044(16) 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
C C .0033 .0016 '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'
N N .0061 .0033 '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'
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
F1 Os F3 178.35(12) yes
F1 Os F2 88.07(13) yes
F3 Os F2 90.28(13) yes
F1 Os Cl1 92.64(9) yes
F3 Os Cl1 89.01(9) yes
F2 Os Cl1 179.02(9) yes
F1 Os Cl2 90.17(10) yes
F3 Os Cl2 89.85(11) yes
F2 Os Cl2 88.18(10) yes
Cl1 Os Cl2 91.13(5) yes
F1 Os Cl3 90.66(10) yes
F3 Os Cl3 89.24(11) yes
F2 Os Cl3 89.06(10) yes
Cl1 Os Cl3 91.61(5) yes
Cl2 Os Cl3 177.09(5) yes
C15 N1 C11 121.5(5) yes
C15 N1 CM 119.9(4) ?
C11 N1 CM 118.5(5) ?
C25 N2 C21 121.8(5) ?
C25 N2 CM 118.8(4) ?
C21 N2 CM 119.4(4) ?
N1 CM N2 109.2(4) yes
N1 CM HM1 107.(3) ?
N2 CM HM1 111.(3) ?
N1 CM HM2 107.(3) ?
N2 CM HM2 104.(3) ?
HM1 CM HM2 120.(4) ?
N1 C11 C12 119.3(6) ?
N1 C11 H11 114.(4) ?
C12 C11 H11 127.(4) ?
C13 C12 C11 119.7(6) ?
C13 C12 H12 120.(4) ?
C11 C12 H12 120.(4) ?
C12 C13 C14 120.2(6) ?
C12 C13 H13 121.(4) ?
C14 C13 H13 118.(5) ?
C15 C14 C13 118.7(6) ?
C15 C14 H14 119.(5) ?
C13 C14 H14 123.(5) ?
N1 C15 C14 120.5(6) ?
N1 C15 H15 118.(4) ?
C14 C15 H15 121.(4) ?
N2 C21 C22 119.5(5) ?
N2 C21 H21 112.(4) ?
C22 C21 H21 129.(4) ?
C21 C22 C23 119.6(5) ?
C21 C22 H22 119.(3) ?
C23 C22 H22 121.(3) ?
C24 C23 C22 119.4(5) ?
C24 C23 H23 115.(4) ?
C22 C23 H23 126.(4) ?
C25 C24 C23 120.1(5) ?
C25 C24 H24 121.(4) ?
C23 C24 H24 119.(4) ?
N2 C25 C24 119.6(5) ?
N2 C25 H25 119.(4) ?
C24 C25 H25 121.(4) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Os F1 1.941(3) yes
Os F2 1.976(3) yes
Os F3 1.946(3) yes
Os Cl1 2.2782(13) yes
Os Cl2 2.3039(15) yes
Os Cl3 2.3108(15) yes
N1 C11 1.358(7) yes
N1 C15 1.341(6) yes
N1 CM 1.469(6) yes
N2 CM 1.492(6) yes
N2 C21 1.351(6) yes
N2 C25 1.340(6) yes
CM HM1 1.06(6) ?
CM HM2 0.96(5) ?
C11 C12 1.369(9) yes
C11 H11 0.99(6) ?
C12 C13 1.367(10) yes
C12 H12 1.00(7) ?
C13 C14 1.387(10) yes
C13 H13 0.85(6) ?
C14 C15 1.365(8) yes
C14 H14 0.91(7) ?
C15 H15 0.90(6) ?
C21 C22 1.369(7) yes
C21 H21 0.95(6) ?
C22 C23 1.380(8) yes
C22 H22 0.92(5) ?
C23 C24 1.369(8) yes
C23 H23 1.03(7) ?
C24 C25 1.367(7) yes
C24 H24 1.06(6) ?
C25 H25 0.92(6) ?