#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2007176.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_2007176
loop_
_publ_author_name
'H\"ohling, M.'
'Preetz, W.'
_publ_section_title
;
 Dipyridiniomethane <i>cis</i>-Dibromotetrafluoroosmate(IV),
 <i>cis</i>-[(C~5~H~5~ N)~2~CH~2~][OsBr~2~F~4~]
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              481
_journal_page_last               483
_journal_volume                  54
_journal_year                    1998
_chemical_formula_iupac          '(C11 H12 N2)[OsBr2 F4]'
_chemical_formula_structural
;
cis-[(C~5~H~5~N)~2~CH~2~][OsF~4~Br~2~]
;
_chemical_formula_sum            'C11 H12 Br2 F4 N2 Os'
_chemical_formula_weight         598.25
_chemical_name_systematic
;
Dipyridinomethane cis-Dibromotetrafluoroosmate(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           'manual editing of cif file (SHELX97)'
_cell_angle_alpha                90.000(8)
_cell_angle_beta                 90.32(3)
_cell_angle_gamma                90.00(2)
_cell_formula_units_Z            4
_cell_length_a                   7.080(3)
_cell_length_b                   6.8203(5)
_cell_length_c                   29.473(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    208(2)
_cell_measurement_theta_max      12.013
_cell_measurement_theta_min      6.336
_cell_volume                     1423.2(6)
_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  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1992)'
_diffrn_ambient_temperature      208(2)
_diffrn_measured_fraction_theta_full .903
_diffrn_measured_fraction_theta_max .903
_diffrn_measurement_device_type
;
Enraf-Nonius CAD4-Turbo four-circle diffractometer
;
_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  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0305
_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            2718
_diffrn_reflns_theta_full        25.07
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         2.76
_diffrn_standards_decay_%        4.5
_diffrn_standards_interval_time  250
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    14.610
_exptl_absorpt_correction_T_max  0.23
_exptl_absorpt_correction_T_min  0.17
_exptl_absorpt_correction_type   'psi-scan (North et al., 1968)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.792
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.036
_refine_diff_density_min         -1.453
_refine_ls_extinction_coef       0.0054(2)
_refine_ls_extinction_method     SHELXL97_(Sheldrick,_1997)
_refine_ls_goodness_of_fit_ref   1.170
_refine_ls_hydrogen_treatment    constr_(riding)
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         2501
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.170
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_obs          0.0261
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
'calc w  = 1/[\s^2^(Fo^2^)+(0.0313P)^2^+6.6890P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_wR_factor_obs         0.0616
_refine_ls_wR_factor_ref         0.0734
_reflns_number_gt                2084
_reflns_number_total             2501
_reflns_threshold_expression     I>2\s(I)
_[local]_cod_data_source_file    jz1245.cif
_[local]_cod_data_source_block   f4br2
_[local]_cod_cif_authors_sg_H-M  'P 2/n'
_cod_original_cell_volume        1423.1(6)
_cod_database_code               2007176
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_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
Os 0.89748(4) 0.35964(4) 0.362292(9) 0.02015(13) Uani d . 1 Os
Br1 1.04187(11) 0.2832(2) 0.43653(3) 0.0413(2) Uani d . 1 Br
Br2 0.57764(10) 0.37326(11) 0.39502(2) 0.0286(2) Uani d . 1 Br
F1 0.7944(7) 0.4117(7) 0.3028(2) 0.0408(11) Uani d . 1 F
F2 1.1450(6) 0.3489(7) 0.3323(2) 0.0388(11) Uani d . 1 F
F3 0.9346(7) 0.6378(6) 0.3705(2) 0.0430(12) Uani d . 1 F
F4 0.8698(6) 0.0835(6) 0.3497(2) 0.0331(10) Uani d . 1 F
N1 0.3861(8) 0.8565(8) 0.4044(2) 0.0208(12) Uani d . 1 N
C11 0.2811(10) 0.7748(11) 0.4377(2) 0.026(2) Uani d . 1 C
H11 0.1516 0.7520 0.4329 0.032 Uiso calc R 1 H
C12 0.3631(13) 0.7254(12) 0.4784(3) 0.038(2) Uani d . 1 C
H12 0.2909 0.6685 0.5016 0.045 Uiso calc R 1 H
C13 0.5517(12) 0.7601(12) 0.4846(3) 0.036(2) Uani d . 1 C
H13 0.6086 0.7326 0.5128 0.043 Uiso calc R 1 H
C14 0.6581(11) 0.8350(10) 0.4500(3) 0.031(2) Uani d . 1 C
H14 0.7886 0.8537 0.4540 0.037 Uiso calc R 1 H
C15 0.5726(11) 0.8831(10) 0.4089(3) 0.027(2) Uani d . 1 C
H15 0.6443 0.9333 0.3848 0.032 Uiso calc R 1 H
N2 0.3827(8) 0.8934(8) 0.3216(2) 0.0222(13) Uani d . 1 N
C21 0.4422(11) 1.0458(11) 0.2964(2) 0.032(2) Uani d . 1 C
H21 0.4328 1.1739 0.3080 0.038 Uiso calc R 1 H
C22 0.5165(12) 1.0160(12) 0.2539(3) 0.037(2) Uani d . 1 C
H22 0.5547 1.1222 0.2359 0.044 Uiso calc R 1 H
C23 0.5335(11) 0.8264(12) 0.2387(3) 0.035(2) Uani d . 1 C
H23 0.5813 0.8025 0.2095 0.042 Uiso calc R 1 H
C24 0.4812(12) 0.6711(12) 0.2656(3) 0.037(2) Uani d . 1 C
H24 0.4983 0.5413 0.2557 0.044 Uiso calc R 1 H
C25 0.4034(11) 0.7094(11) 0.3074(3) 0.033(2) Uani d . 1 C
H25 0.3647 0.6051 0.3260 0.039 Uiso calc R 1 H
CM 0.2840(10) 0.9355(12) 0.3649(2) 0.029(2) Uani d . 1 C
HM1 0.2704 1.0777 0.3684 0.035 Uiso calc R 1 H
HM2 0.1571 0.8783 0.3637 0.035 Uiso calc R 1 H
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 0.02116(18) 0.01939(18) 0.01993(18) -0.00091(11) 0.00251(10) 0.00145(11)
Br1 0.0325(4) 0.0650(6) 0.0265(4) 0.0039(4) -0.0056(3) 0.0020(4)
Br2 0.0246(4) 0.0304(4) 0.0308(4) 0.0025(3) 0.0045(3) -0.0022(3)
F1 0.047(3) 0.053(3) 0.022(2) 0.007(2) -0.0059(19) 0.010(2)
F2 0.027(2) 0.042(3) 0.048(3) -0.001(2) 0.014(2) 0.004(2)
F3 0.049(3) 0.019(2) 0.061(3) -0.004(2) 0.005(2) 0.001(2)
F4 0.041(2) 0.018(2) 0.040(3) -0.0014(18) 0.009(2) -0.0073(19)
N1 0.023(3) 0.022(3) 0.017(3) 0.002(2) 0.002(2) -0.001(2)
C11 0.027(4) 0.029(4) 0.023(4) -0.005(3) 0.010(3) 0.003(3)
C12 0.053(5) 0.042(5) 0.019(4) -0.003(4) 0.016(3) 0.009(4)
C13 0.042(5) 0.042(5) 0.022(4) 0.009(4) -0.004(3) -0.002(4)
C14 0.027(4) 0.022(4) 0.043(5) 0.001(3) -0.004(3) -0.001(3)
C15 0.033(4) 0.018(4) 0.029(4) -0.004(3) 0.005(3) 0.000(3)
N2 0.023(3) 0.026(3) 0.017(3) 0.007(2) -0.002(2) 0.000(2)
C21 0.050(5) 0.019(4) 0.025(4) 0.000(3) -0.003(3) 0.006(3)
C22 0.043(5) 0.037(5) 0.030(4) 0.000(4) 0.005(4) 0.014(4)
C23 0.028(4) 0.048(5) 0.028(4) 0.008(4) -0.002(3) -0.003(4)
C24 0.044(5) 0.040(5) 0.026(4) 0.013(4) -0.003(4) -0.008(4)
C25 0.038(4) 0.025(4) 0.035(4) 0.012(3) -0.006(3) 0.002(3)
CM 0.026(4) 0.036(4) 0.026(4) 0.007(3) 0.006(3) 0.011(3)
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'
Br Br -.2901 2.4595 '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'
F F .0171 .0103 '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'
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 F4 88.1(2) y
F1 Os F3 89.1(2) y
F4 Os F3 175.6(2) y
F1 Os F2 86.1(2) y
F4 Os F2 88.1(2) y
F3 Os F2 88.4(2) y
F1 Os Br1 177.10(10) y
F4 Os Br1 90.40(10) y
F3 Os Br1 92.4(2) y
F2 Os Br1 91.4(2) y
F1 Os Br2 90.3(2) y
F4 Os Br2 91.10(10) y
F3 Os Br2 92.2(2) y
F2 Os Br2 176.40(10) y
Br1 Os Br2 92.18(4) y
C15 N1 C11 121.9(6) ?
C15 N1 CM 120.7(6) ?
C11 N1 CM 117.1(6) ?
N1 C11 C12 120.2(7) ?
N1 C11 H11 119.9 ?
C12 C11 H11 119.9 ?
C13 C12 C11 118.9(7) ?
C13 C12 H12 120.6 ?
C11 C12 H12 120.6 ?
C12 C13 C14 120.3(7) ?
C12 C13 H13 119.8 ?
C14 C13 H13 119.8 ?
C13 C14 C15 119.9(7) ?
C13 C14 H14 120.1 ?
C15 C14 H14 120.1 ?
N1 C15 C14 118.6(7) ?
N1 C15 H15 120.7 ?
C14 C15 H15 120.7 ?
C25 N2 C21 121.3(6) ?
C25 N2 CM 120.3(6) ?
C21 N2 CM 118.3(6) ?
N2 C21 C22 120.6(7) ?
N2 C21 H21 119.7 ?
C22 C21 H21 119.7 ?
C23 C22 C21 118.1(7) ?
C23 C22 H22 120.9 ?
C21 C22 H22 120.9 ?
C22 C23 C24 120.7(7) ?
C22 C23 H23 119.6 ?
C24 C23 H23 119.6 ?
C25 C24 C23 118.7(8) ?
C25 C24 H24 120.6 ?
C23 C24 H24 120.6 ?
N2 C25 C24 120.3(7) ?
N2 C25 H25 119.8 ?
C24 C25 H25 119.8 ?
N1 CM N2 112.2(6) y
N1 CM HM1 109.2 ?
N2 CM HM1 109.2 ?
N1 CM HM2 109.2 ?
N2 CM HM2 109.2 ?
HM1 CM HM2 107.9 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Os F1 1.928(4) y
Os F4 1.929(4) y
Os F3 1.930(4) y
Os F2 1.968(4) y
Os Br1 2.4660(10) y
Os Br2 2.4680(10) y
N1 C15 1.338(10) ?
N1 C11 1.355(9) ?
N1 CM 1.469(9) ?
C11 C12 1.371(11) ?
C11 H11 0.9400 ?
C12 C13 1.367(12) ?
C12 H12 0.9400 ?
C13 C14 1.371(11) ?
C13 H13 0.9400 ?
C14 C15 1.389(11) ?
C14 H14 0.9400 ?
C15 H15 0.9400 ?
N2 C25 1.331(9) ?
N2 C21 1.346(9) ?
N2 CM 1.487(9) ?
C21 C22 1.376(11) ?
C21 H21 0.9400 ?
C22 C23 1.374(12) ?
C22 H22 0.9400 ?
C23 C24 1.376(12) ?
C23 H23 0.9400 ?
C24 C25 1.376(11) ?
C24 H24 0.9400 ?
C25 H25 0.9400 ?
CM HM1 0.9800 ?
CM HM2 0.9800 ?