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#$Date: 2016-03-21 09:02:51 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178616 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/27/4072736.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_4072736
loop_
_publ_author_name
'Gross, Christopher L.'
'Brumaghim, Julia L.'
'Girolami, Gregory S.'
_publ_section_title
;
 Synthesis and Reactivity of the Osmium(III) Pentamethylcyclopentadienyl
 Complex (C5Me5)2Os2Br4. X-ray Crystal Structures of (C5Me5)2Os2Br4,
 (C5Me5)2Os2(μ-O)Br4, and (C5Me5)2Os2(μ-NPh)2Br2
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2258
_journal_paper_doi               10.1021/om060983u
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C20 H30 Br4 O Os2'
_chemical_formula_weight         986.48
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/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                 93.9340(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.5196(4)
_cell_length_b                   13.7702(6)
_cell_length_c                   10.8259(5)
_cell_measurement_temperature    198(2)
_cell_volume                     1267.07(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      198(2)
_diffrn_measured_fraction_theta_full 0.663
_diffrn_measured_fraction_theta_max 0.663
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0701
_diffrn_reflns_av_sigmaI/netI    0.0629
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5476
_diffrn_reflns_theta_full        28.24
_diffrn_reflns_theta_max         28.24
_diffrn_reflns_theta_min         2.40
_exptl_absorpt_coefficient_mu    16.334
_exptl_crystal_density_diffrn    2.586
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             900
_refine_diff_density_max         3.321
_refine_diff_density_min         -1.642
_refine_diff_density_rms         0.378
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         2082
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0999
_refine_ls_R_factor_gt           0.0748
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0791P)²+81.1694P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1902
_refine_ls_wR_factor_ref         0.2084
_reflns_number_gt                1605
_reflns_number_total             2082
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060983usi20061024_064623.cif
_cod_data_source_block           ossmabs2
_cod_database_code               4072736
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_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
Os Os 0.56786(10) 0.46935(5) 0.65783(8) 0.0255(3) Uani 1 1 d .
Br1 Br 0.3213(3) 0.5254(2) 0.7509(3) 0.0474(7) Uani 1 1 d .
Br2 Br 0.6949(4) 0.63017(17) 0.7104(3) 0.0654(10) Uani 1 1 d .
O O 0.5000 0.5000 0.5000 0.026(4) Uani 1 2 d SU
C1 C 0.754(3) 0.3982(15) 0.798(2) 0.031(5) Uani 1 1 d U
C2 C 0.782(3) 0.3805(15) 0.672(2) 0.028(4) Uani 1 1 d U
C3 C 0.651(3) 0.3242(15) 0.610(2) 0.033(5) Uani 1 1 d U
C4 C 0.538(3) 0.3158(15) 0.702(2) 0.029(5) Uani 1 1 d U
C5 C 0.602(3) 0.3583(15) 0.816(2) 0.031(5) Uani 1 1 d U
C6 C 0.862(3) 0.4516(18) 0.890(2) 0.042(6) Uani 1 1 d .
H6A H 0.8090 0.4620 0.9667 0.063 Uiso 1 1 calc R
H6B H 0.8907 0.5144 0.8558 0.063 Uiso 1 1 calc R
H6C H 0.9578 0.4130 0.9089 0.063 Uiso 1 1 calc R
C7 C 0.938(3) 0.401(2) 0.611(3) 0.063(9) Uani 1 1 d .
H7A H 0.9142 0.4196 0.5237 0.095 Uiso 1 1 calc R
H7B H 1.0034 0.3429 0.6148 0.095 Uiso 1 1 calc R
H7C H 0.9935 0.4545 0.6545 0.095 Uiso 1 1 calc R
C8 C 0.646(3) 0.2797(18) 0.487(2) 0.044(6) Uani 1 1 d .
H8A H 0.6749 0.2110 0.4951 0.067 Uiso 1 1 calc R
H8B H 0.7198 0.3131 0.4363 0.067 Uiso 1 1 calc R
H8C H 0.5391 0.2851 0.4480 0.067 Uiso 1 1 calc R
C9 C 0.391(3) 0.2585(19) 0.690(3) 0.050(7) Uani 1 1 d .
H9A H 0.4170 0.1892 0.6955 0.075 Uiso 1 1 calc R
H9B H 0.3350 0.2724 0.6104 0.075 Uiso 1 1 calc R
H9C H 0.3250 0.2758 0.7575 0.075 Uiso 1 1 calc R
C10 C 0.529(4) 0.358(2) 0.934(3) 0.047(7) Uani 1 1 d .
H10A H 0.5726 0.4115 0.9859 0.071 Uiso 1 1 calc R
H10B H 0.5494 0.2963 0.9763 0.071 Uiso 1 1 calc R
H10C H 0.4148 0.3675 0.9192 0.071 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 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'
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
O Os C4 113.4(7) .
O Os C2 113.8(6) .
C4 Os C2 63.6(8) .
O Os C3 94.5(7) .
C4 Os C3 38.3(8) .
C2 Os C3 39.3(9) .
O Os C5 150.5(6) .
C4 Os C5 37.2(8) .
C2 Os C5 61.0(8) .
C3 Os C5 62.7(8) .
O Os C1 150.2(5) .
C4 Os C1 62.4(8) .
C2 Os C1 36.5(8) .
C3 Os C1 63.4(9) .
C5 Os C1 36.0(8) .
O Os Br1 94.86(8) .
C4 Os Br1 95.5(6) .
C2 Os Br1 149.1(5) .
C3 Os Br1 131.8(6) .
C5 Os Br1 88.5(6) .
C1 Os Br1 114.7(5) .
O Os Br2 96.47(8) .
C4 Os Br2 149.0(7) .
C2 Os Br2 97.7(6) .
C3 Os Br2 135.6(7) .
C5 Os Br2 112.8(6) .
C1 Os Br2 87.7(5) .
Br1 Os Br2 89.84(12) .
Os O Os 180.0 3_666
C2 C1 C5 106(2) .
C2 C1 C6 126(2) .
C5 C1 C6 128(2) .
C2 C1 Os 66.2(12) .
C5 C1 Os 70.5(14) .
C6 C1 Os 125.8(15) .
C1 C2 C3 110.7(19) .
C1 C2 C7 125(2) .
C3 C2 C7 123(2) .
C1 C2 Os 77.3(12) .
C3 C2 Os 70.5(12) .
C7 C2 Os 126.9(18) .
C4 C3 C8 128(2) .
C4 C3 C2 105(2) .
C8 C3 C2 127(2) .
C4 C3 Os 70.6(12) .
C8 C3 Os 127.1(16) .
C2 C3 Os 70.2(12) .
C3 C4 C5 109(2) .
C3 C4 C9 126(2) .
C5 C4 C9 124(2) .
C3 C4 Os 71.1(12) .
C5 C4 Os 75.5(12) .
C9 C4 Os 127.6(17) .
C1 C5 C4 110(2) .
C1 C5 C10 124(2) .
C4 C5 C10 126(2) .
C1 C5 Os 73.4(14) .
C4 C5 Os 67.3(12) .
C10 C5 Os 127.6(15) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Os O 1.8156(9) .
Os C4 2.19(2) .
Os C2 2.19(2) .
Os C3 2.19(2) .
Os C5 2.30(2) .
Os C1 2.33(2) .
Os Br1 2.513(3) .
Os Br2 2.513(3) .
O Os 1.8155(9) 3_666
C1 C2 1.42(3) .
C1 C5 1.43(3) .
C1 C6 1.50(3) .
C2 C3 1.47(3) .
C2 C7 1.55(3) .
C3 C4 1.44(3) .
C3 C8 1.47(3) .
C4 C5 1.43(3) .
C4 C9 1.47(3) .
C5 C10 1.46(4) .
