#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:43:41 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179761 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/57/7005728.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7005728
loop_
_publ_author_name
'Jakonen, Minna'
'Hirva, Pipsa'
'Haukka, Matti'
'Chardon-Noblat, Sylvie'
'Lafolet, Frédéric'
'Chauvin, Jérôme'
'Deronzier, Alain'
_publ_section_title
;
 An alternative synthesis method for [Os(NN)(CO)(2)X(2)] complexes (NN
 = 2,2'-bipyridine, 4,4'-dimethyl-2,2'-bipyridine; X = Cl, Br, I).
 Electrochemical and photochemical properties and behavior.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3314
_journal_page_last               3324
_journal_paper_doi               10.1039/b704931e
_journal_year                    2007
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C12 H8 Cl2 N2 O2 Os'
_chemical_formula_sum            'C12 H8 Cl2 N2 O2 Os'
_chemical_formula_weight         473.30
_chemical_name_systematic
;
?
;
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_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                 104.171(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.1820(6)
_cell_length_b                   6.8180(3)
_cell_length_c                   12.4450(8)
_cell_measurement_reflns_used    1916
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     673.12(7)
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Diamond v.3.1d (Brandenburg, 2006)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'φ scans and ω scans with κ offset'
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0432
_diffrn_reflns_av_sigmaI/netI    0.0540
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5285
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.71
_exptl_absorpt_coefficient_mu    9.866
_exptl_absorpt_correction_T_max  0.6129
_exptl_absorpt_correction_T_min  0.4183
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Xprep in Shelxtl v.6.14-1 (Sheldrick, 2005)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.335
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             440
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.065
_refine_diff_density_min         -1.482
_refine_diff_density_rms         0.186
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.008(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2498
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0307
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0224P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0625
_refine_ls_wR_factor_ref         0.0634
_reflns_number_gt                2344
_reflns_number_total             2498
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b704931e.txt
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P n'
_cod_database_code               7005728
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x+1/2, -y, z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Os1 Os 0.96217(6) 0.78237(4) 0.09967(6) 0.02121(9) Uani 1 1 d . . .
Cl1 Cl 1.1280(3) 0.5921(3) 0.24842(18) 0.0302(5) Uani 1 1 d . . .
Cl2 Cl 0.8220(3) 0.9627(3) -0.06130(17) 0.0289(5) Uani 1 1 d . . .
O1 O 0.8452(9) 1.0632(11) 0.2514(6) 0.0425(17) Uani 1 1 d . . .
O2 O 0.6599(11) 0.5348(11) 0.0905(6) 0.0475(19) Uani 1 1 d . . .
N1 N 1.0683(9) 0.6101(10) -0.0067(5) 0.0228(15) Uani 1 1 d . . .
N2 N 1.1837(9) 0.9406(10) 0.0970(5) 0.0225(15) Uani 1 1 d . . .
C1 C 0.8856(11) 0.9591(13) 0.1970(7) 0.0250(19) Uani 1 1 d . . .
C2 C 0.7671(12) 0.6213(15) 0.0927(7) 0.0259(19) Uani 1 1 d . . .
C10 C 1.0053(11) 0.4423(12) -0.0551(6) 0.0254(19) Uani 1 1 d . . .
H10 H 0.9015 0.3959 -0.0435 0.030 Uiso 1 1 calc R . .
C11 C 1.0858(12) 0.3313(13) -0.1225(7) 0.030(2) Uani 1 1 d . . .
H11 H 1.0387 0.2124 -0.1562 0.036 Uiso 1 1 calc R . .
C12 C 1.2364(13) 0.4030(13) -0.1375(8) 0.031(2) Uani 1 1 d . . .
H12 H 1.2960 0.3311 -0.1811 0.037 Uiso 1 1 calc R . .
C13 C 1.3004(12) 0.5757(13) -0.0905(7) 0.030(2) Uani 1 1 d . . .
H13 H 1.4022 0.6260 -0.1033 0.036 Uiso 1 1 calc R . .
C14 C 1.2177(11) 0.6768(12) -0.0245(7) 0.0231(18) Uani 1 1 d . . .
C15 C 1.2800(11) 0.8636(13) 0.0326(7) 0.0259(18) Uani 1 1 d . . .
C16 C 1.4261(10) 0.9530(13) 0.0231(8) 0.029(2) Uani 1 1 d . . .
H16 H 1.4927 0.8958 -0.0214 0.034 Uiso 1 1 calc R . .
C17 C 1.4749(17) 1.1250(14) 0.0779(9) 0.034(3) Uani 1 1 d . . .
H17 H 1.5737 1.1904 0.0698 0.041 Uiso 1 1 calc R . .
C18 C 1.3805(13) 1.2030(14) 0.1449(8) 0.032(2) Uani 1 1 d . . .
H18 H 1.4148 1.3202 0.1854 0.039 Uiso 1 1 calc R . .
C19 C 1.2351(12) 1.1075(13) 0.1522(7) 0.030(2) Uani 1 1 d . . .
H19 H 1.1690 1.1617 0.1978 0.036 Uiso 1 1 calc R . .
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'
H H 0.0000 0.0000 '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'
Cl Cl 0.1484 0.1585 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Os1 C2 89.5(4) . . yes
C1 Os1 N1 173.7(3) . . ?
C2 Os1 N1 96.8(3) . . ?
C1 Os1 N2 95.9(3) . . ?
C2 Os1 N2 174.6(3) . . ?
N1 Os1 N2 77.8(3) . . yes
C1 Os1 Cl2 92.4(2) . . ?
C2 Os1 Cl2 91.9(2) . . ?
N1 Os1 Cl2 86.98(19) . . ?
N2 Os1 Cl2 87.81(18) . . ?
C1 Os1 Cl1 93.6(3) . . ?
C2 Os1 Cl1 91.9(2) . . ?
N1 Os1 Cl1 86.61(18) . . ?
N2 Os1 Cl1 87.87(19) . . ?
Cl2 Os1 Cl1 172.91(8) . . yes
C10 N1 C14 118.1(7) . . ?
C10 N1 Os1 126.0(6) . . ?
C14 N1 Os1 115.9(5) . . ?
C19 N2 C15 118.4(8) . . ?
C19 N2 Os1 125.9(6) . . ?
C15 N2 Os1 115.7(6) . . ?
O1 C1 Os1 178.0(8) . . ?
O2 C2 Os1 178.7(9) . . ?
N1 C10 C11 123.0(8) . . ?
N1 C10 H10 118.5 . . ?
C11 C10 H10 118.5 . . ?
C12 C11 C10 117.0(8) . . ?
C12 C11 H11 121.5 . . ?
C10 C11 H11 121.5 . . ?
C13 C12 C11 120.7(8) . . ?
C13 C12 H12 119.7 . . ?
C11 C12 H12 119.7 . . ?
C12 C13 C14 119.9(8) . . ?
C12 C13 H13 120.1 . . ?
C14 C13 H13 120.1 . . ?
C13 C14 N1 121.3(8) . . ?
C13 C14 C15 123.8(8) . . ?
N1 C14 C15 114.9(7) . . ?
N2 C15 C16 121.5(8) . . ?
N2 C15 C14 115.7(7) . . ?
C16 C15 C14 122.9(8) . . ?
C17 C16 C15 119.5(9) . . ?
C17 C16 H16 120.3 . . ?
C15 C16 H16 120.3 . . ?
C16 C17 C18 119.7(10) . . ?
C16 C17 H17 120.1 . . ?
C18 C17 H17 120.1 . . ?
C17 C18 C19 118.6(9) . . ?
C17 C18 H18 120.7 . . ?
C19 C18 H18 120.7 . . ?
N2 C19 C18 122.3(9) . . ?
N2 C19 H19 118.9 . . ?
C18 C19 H19 118.9 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Os1 C1 1.919(10) . yes
Os1 C2 1.922(11) . yes
Os1 N1 2.109(7) . yes
Os1 N2 2.117(7) . yes
Os1 Cl2 2.391(2) . yes
Os1 Cl1 2.392(2) . yes
O1 C1 1.087(11) . ?
O2 C2 1.052(11) . ?
N1 C10 1.336(11) . ?
N1 C14 1.373(11) . ?
N2 C19 1.342(11) . ?
N2 C15 1.359(11) . ?
C10 C11 1.408(12) . ?
C10 H10 0.9500 . ?
C11 C12 1.379(13) . ?
C11 H11 0.9500 . ?
C12 C13 1.361(13) . ?
C12 H12 0.9500 . ?
C13 C14 1.371(12) . ?
C13 H13 0.9500 . ?
C14 C15 1.487(12) . ?
C15 C16 1.373(12) . ?
C16 C17 1.366(14) . ?
C16 H16 0.9500 . ?
C17 C18 1.374(15) . ?
C17 H17 0.9500 . ?
C18 C19 1.379(14) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
