#------------------------------------------------------------------------------
#$Date: 2016-02-19 16:29:56 +0200 (Fri, 19 Feb 2016) $
#$Revision: 176759 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/44/2004480.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_2004480
loop_
_publ_author_name
'Bruhn, C.'
'Preetz, W.'
_publ_section_title
;
 Dipyridiniomethane cis- and
 trans-Difluorotetrachloroosmate(IV), cis- and
 trans-[(C₅H₅N)₂CH₂][OsCl₄F₂]
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              321
_journal_page_last               325
_journal_paper_doi               10.1107/S0108270195010717
_journal_volume                  52
_journal_year                    1996
_chemical_formula_moiety         'C11 H12 Cl4 F2 N2 Os'
_chemical_formula_structural     trans-[(C~5~H~5~N)~2~CH~2~][OsF~2~Cl~4~]
_chemical_formula_sum            'C11 H12 Cl4 F2 N2 Os'
_chemical_formula_weight         542.23
_chemical_name_systematic
;
 N,N'-methylenedipyridinium trans-difluorotetrachloroosmate(IV)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL
_cell_angle_alpha                89.649(7)
_cell_angle_beta                 70.346(6)
_cell_angle_gamma                75.112(6)
_cell_formula_units_Z            2
_cell_length_a                   7.7562(5)
_cell_length_b                   10.0127(8)
_cell_length_c                   11.0057(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11.85
_cell_measurement_theta_min      4.01
_cell_volume                     774.86(11)
_computing_cell_refinement       CAD-4-PC
_computing_data_collection       'CAD-4-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, 1993)'
_computing_structure_solution    'SIR92 (Altomare et al., 1992)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       ω/2θ
_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  0.0122
_diffrn_reflns_av_sigmaI/netI    0.0165
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3007
_diffrn_reflns_theta_max         29.94
_diffrn_reflns_theta_min         2.11
_diffrn_standards_decay_%        2.4
_diffrn_standards_interval_count 300
_diffrn_standards_interval_time  240min
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    8.928
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.73
_exptl_absorpt_correction_type
'empirical via \y scans (North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.324
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             508
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         .69
_refine_diff_density_min         -.46
_refine_ls_extinction_coef       0.0183(4)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   1.132
_refine_ls_goodness_of_fit_obs   1.096
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     233
_refine_ls_number_reflns         2795
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.132
_refine_ls_restrained_S_obs      1.096
_refine_ls_R_factor_all          0.0231
_refine_ls_R_factor_obs          0.0148
_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^) + (0.018P)^2^ + 0.31P]
where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.0389
_refine_ls_wR_factor_obs         0.0343
_reflns_number_observed          2354
_reflns_number_total             2795
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            bm1027.cif
_cod_data_source_block           II
_cod_original_cell_volume        774.76(14)
_cod_database_code               2004480
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_occupancy
_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_type_symbol
Os1 1 0 0 0 .02399(7) Uani d S Os
F1 1 -0.1246(3) .1371(2) .1459(2) .0355(5) Uani d . F
Cl11 1 .19078(12) .14176(9) -0.10534(9) .0360(2) Uani d . Cl
Cl12 1 -0.22903(14) .10522(10) -.09175(9) .0415(2) Uani d . Cl
Os2 1 .5 .5 .5 .02644(7) Uani d S Os
F2 1 .5527(3) .3321(2) .3933(2) .0365(5) Uani d . F
Cl21 1 .18906(13) .56678(10) .49972(10) .0407(2) Uani d . Cl
Cl22 1 .59682(13) .61427(9) .31263(9) .0401(2) Uani d . Cl
CM 1 .4380(6) .1528(4) .2233(4) .0337(8) Uani d . C
N1 1 .3252(4) .2828(3) .1953(3) .0278(6) Uani d . N
C11 1 .3931(7) .3947(4) .1807(4) .0428(10) Uani d . C
C12 1 .2893(9) .5154(4) .1519(4) .0590(13) Uani d . C
C13 1 .1193(9) .5206(5) .1389(5) .066(2) Uani d . C
C14 1 .0535(7) .4053(5) .1534(4) .0552(12) Uani d . C
C15 1 .1595(6) .2855(4) .1809(4) .0392(9) Uani d . C
N2 1 .3345(4) .1099(3) .3509(3) .0265(6) Uani d . N
C21 1 .3521(6) -.0266(4) .3614(4) .0369(9) Uani d . C
C22 1 .2727(6) -.0715(4) .4789(4) .0449(10) Uani d . C
C23 1 .1771(6) .0211(4) .5856(4) .0449(10) Uani d . C
C24 1 .1606(6) .1595(4) .5721(4) .0431(10) Uani d . C
C25 1 .2413(5) .2030(4) .4546(3) .0316(8) Uani d . C
HM1 1 .556(6) .162(4) .230(4) .051(12) Uiso d . H
HM2 1 .452(5) .088(4) .164(4) .038(11) Uiso d . H
H11 1 .498(6) .382(4) .194(4) .052(14) Uiso d . H
H12 1 .349(6) .590(5) .138(4) .063(14) Uiso d . H
H13 1 .046(7) .603(5) .123(5) .074(15) Uiso d . H
H14 1 -.060(7) .409(5) .148(5) .074(16) Uiso d . H
H15 1 .124(6) .197(4) .188(4) .048(12) Uiso d . H
H21 1 .423(5) -.084(4) .287(3) .025(9) Uiso d . H
H22 1 .280(6) -0.160(4) .485(4) .045(11) Uiso d . H
H23 1 .123(6) -.010(4) .666(4) .051(12) Uiso d . H
H24 1 .104(6) .221(4) .639(4) .045(12) Uiso d . H
H25 1 .235(5) .299(4) .438(3) .035(10) Uiso d . 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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
F1 Os1 F1 2 . 180.0 n
F1 Os1 Cl11 2 2 89.90(6) ?
F1 Os1 Cl11 . 2 90.10(6) ?
F1 Os1 Cl11 2 . 90.10(6) y
F1 Os1 Cl11 . . 89.90(6) y
Cl11 Os1 Cl11 2 . 180.0 n
F1 Os1 Cl12 2 2 89.69(7) ?
F1 Os1 Cl12 . 2 90.31(7) y
Cl11 Os1 Cl12 2 2 90.37(3) ?
Cl11 Os1 Cl12 . 2 89.62(3) ?
F1 Os1 Cl12 2 . 90.31(7) ?
F1 Os1 Cl12 . . 89.69(7) y
Cl11 Os1 Cl12 2 . 89.63(3) ?
Cl11 Os1 Cl12 . . 90.37(3) y
Cl12 Os1 Cl12 2 . 180.0 n
F2 Os2 F2 2_666 . 180.0 n
F2 Os2 Cl21 2_666 2_666 90.59(7) ?
F2 Os2 Cl21 . 2_666 89.41(7) y
F2 Os2 Cl21 2_666 . 89.41(7) ?
F2 Os2 Cl21 . . 90.59(7) y
Cl21 Os2 Cl21 2_666 . 180.0 n
F2 Os2 Cl22 2_666 . 90.44(7) y
F2 Os2 Cl22 . . 89.56(7) y
Cl21 Os2 Cl22 2_666 . 90.46(3) y
Cl21 Os2 Cl22 . . 89.54(3) y
F2 Os2 Cl22 2_666 2_666 89.56(7) ?
F2 Os2 Cl22 . 2_666 90.44(7) ?
Cl21 Os2 Cl22 2_666 2_666 89.54(3) ?
Cl21 Os2 Cl22 . 2_666 90.46(3) ?
Cl22 Os2 Cl22 . 2_666 180.0 n
N1 CM N2 . . 111.0(3) y
N1 CM HM1 . . 112.(2) ?
N2 CM HM1 . . 105.(3) ?
N1 CM HM2 . . 108.(3) ?
N2 CM HM2 . . 107.(2) ?
HM1 CM HM2 . . 114.(4) ?
C15 N1 C11 . . 121.7(3) ?
C15 N1 CM . . 119.0(3) ?
C11 N1 CM . . 119.3(3) ?
N1 C11 C12 . . 119.2(4) ?
N1 C11 H11 . . 114.(3) ?
C12 C11 H11 . . 127.(3) ?
C13 C12 C11 . . 119.8(5) ?
C13 C12 H12 . . 125.(3) ?
C11 C12 H12 . . 115.(3) ?
C12 C13 C14 . . 120.0(4) ?
C12 C13 H13 . . 120.(3) ?
C14 C13 H13 . . 120.(3) ?
C15 C14 C13 . . 119.5(5) ?
C15 C14 H14 . . 120.(3) ?
C13 C14 H14 . . 121.(3) ?
N1 C15 C14 . . 119.8(4) ?
N1 C15 H15 . . 116.(2) ?
C14 C15 H15 . . 124.(2) ?
C25 N2 C21 . . 121.3(3) ?
C25 N2 CM . . 120.9(3) ?
C21 N2 CM . . 117.6(3) ?
N2 C21 C22 . . 119.5(4) ?
N2 C21 H21 . . 116.(2) ?
C22 C21 H21 . . 124.(2) ?
C21 C22 C23 . . 120.2(4) ?
C21 C22 H22 . . 120.(3) ?
C23 C22 H22 . . 120.(3) ?
C22 C23 C24 . . 119.0(4) ?
C22 C23 H23 . . 120.(3) ?
C24 C23 H23 . . 121.(3) ?
C25 C24 C23 . . 120.2(4) ?
C25 C24 H24 . . 118.(3) ?
C23 C24 H24 . . 122.(3) ?
N2 C25 C24 . . 119.7(3) ?
N2 C25 H25 . . 116.(2) ?
C24 C25 H25 . . 125.(2) ?
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
Os1 F1 2 1.923(2) ?
Os1 F1 . 1.923(2) y
Os1 Cl11 2 2.3353(8) ?
Os1 Cl11 . 2.3353(8) y
Os1 Cl12 2 2.3488(9) ?
Os1 Cl12 . 2.3488(9) y
Os2 F2 2_666 1.929(2) ?
Os2 F2 . 1.929(2) y
Os2 Cl21 2_666 2.3323(9) ?
Os2 Cl21 . 2.3323(9) y
Os2 Cl22 . 2.3444(9) y
Os2 Cl22 2_666 2.3444(9) ?
CM N1 . 1.465(4) y
CM N2 . 1.488(4) y
CM HM1 . 0.96(4) ?
CM HM2 . 0.88(4) ?
N1 C15 . 1.341(5) y
N1 C11 . 1.343(5) y
C11 C12 . 1.370(6) y
C11 H11 . 0.85(4) ?
C12 C13 . 1.361(8) y
C12 H12 . 0.96(4) ?
C13 C14 . 1.365(8) y
C13 H13 . 0.92(5) ?
C14 C15 . 1.365(6) y
C14 H14 . 0.89(5) ?
C15 H15 . 0.98(4) ?
N2 C25 . 1.344(4) y
N2 C21 . 1.346(4) y
C21 C22 . 1.362(5) y
C21 H21 . 0.92(3) ?
C22 C23 . 1.365(6) y
C22 H22 . 0.88(4) ?
C23 C24 . 1.370(6) y
C23 H23 . 0.93(4) ?
C24 C25 . 1.357(5) y
C24 H24 . 0.87(4) ?
C25 H25 . 0.97(4) ?
