#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:42:00 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179803 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/99/7009964.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_7009964
loop_
_publ_author_name
'Barthram, Anita M.'
'Reeves, Zöe R.'
'Jeffery, John C.'
'Ward, Michael D.'
_publ_section_title
;
 Polynuclear osmium--dioxolene complexes: comparison of electrochemical
 and spectroelectrochemical properties with those of their ruthenium
 analogues
;
_journal_issue                   18
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3162
_journal_paper_doi               10.1039/b004858p
_journal_year                    2000
_chemical_formula_sum            'C26 H20 F6 N4 O2 Os P'
_chemical_formula_weight         755.63
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(11)
_cell_angle_beta                 104.011(10)
_cell_angle_gamma                90.000(14)
_cell_formula_units_Z            4
_cell_length_a                   11.8056(14)
_cell_length_b                   14.869(3)
_cell_length_c                   14.909(3)
_cell_measurement_temperature    173(2)
_cell_volume                     2539.2(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'Siemens SMART Area Detector'
_diffrn_measurement_method
'ω rotation with narrow frames (0.3 degrees)'
_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  0.0253
_diffrn_reflns_av_sigmaI/netI    0.0328
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8036
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    5.163
_exptl_absorpt_correction_T_max  0.60
_exptl_absorpt_correction_T_min  0.08
_exptl_absorpt_correction_type   'Empirical, pseudo-azimuthal scan (SADABS)'
_exptl_crystal_colour            'dark green '
_exptl_crystal_density_diffrn    1.977
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1460
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.890
_refine_diff_density_min         -0.824
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         2910
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0252
_refine_ls_R_factor_gt           0.0224
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0311P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0545
_refine_ls_wR_factor_ref         0.0549
_reflns_number_gt                2647
_reflns_number_total             2910
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b004858p.txt
_cod_data_source_block           sad
_cod_original_cell_volume        2539.3(7)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7009964
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Os1 Os 0.5000 0.528215(13) 0.7500 0.02330(7) Uani 1 2 d S . .
O31 O 0.56508(19) 0.63105(16) 0.68970(14) 0.0286(5) Uani 1 1 d . . .
N11 N 0.3587(2) 0.51871(19) 0.63788(18) 0.0273(6) Uani 1 1 d . . .
N21 N 0.5586(2) 0.43573(19) 0.66887(17) 0.0240(5) Uani 1 1 d . . .
C22 C 0.4834(3) 0.4155(2) 0.5865(2) 0.0263(6) Uani 1 1 d . . .
C12 C 0.3701(3) 0.4607(2) 0.5700(2) 0.0289(7) Uani 1 1 d . . .
C26 C 0.6660(3) 0.3980(2) 0.6874(2) 0.0310(7) Uani 1 1 d . . .
H26 H 0.7194 0.4118 0.7444 0.037 Uiso 1 1 calc R . .
C32 C 0.5343(3) 0.7119(2) 0.7167(2) 0.0291(7) Uani 1 1 d . . .
C23 C 0.5149(3) 0.3572(2) 0.5241(2) 0.0315(7) Uani 1 1 d . . .
H23A H 0.4608 0.3436 0.4674 0.038 Uiso 1 1 calc R . .
C13 C 0.2795(3) 0.4478(3) 0.4916(3) 0.0372(8) Uani 1 1 d . . .
H13A H 0.2880 0.4066 0.4450 0.045 Uiso 1 1 calc R . .
C16 C 0.2578(3) 0.5651(3) 0.6282(2) 0.0336(8) Uani 1 1 d . . .
H16A H 0.2499 0.6058 0.6754 0.040 Uiso 1 1 calc R . .
C25 C 0.7012(3) 0.3401(3) 0.6270(2) 0.0340(8) Uani 1 1 d . . .
H25A H 0.7775 0.3150 0.6422 0.041 Uiso 1 1 calc R . .
C14 C 0.1770(4) 0.4959(3) 0.4826(3) 0.0446(10) Uani 1 1 d . . .
H14A H 0.1145 0.4884 0.4294 0.053 Uiso 1 1 calc R . .
C33 C 0.5650(3) 0.7930(3) 0.6829(2) 0.0363(8) Uani 1 1 d . . .
H33 H 0.6087 0.7933 0.6371 0.044 Uiso 1 1 calc R . .
C15 C 0.1660(3) 0.5548(3) 0.5515(3) 0.0418(9) Uani 1 1 d . . .
H15A H 0.0959 0.5880 0.5462 0.050 Uiso 1 1 calc R . .
C34 C 0.5320(3) 0.8734(3) 0.7157(3) 0.0406(9) Uani 1 1 d . . .
H34 H 0.5525 0.9288 0.6920 0.049 Uiso 1 1 calc R . .
C24 C 0.6242(3) 0.3192(3) 0.5443(2) 0.0348(8) Uani 1 1 d . . .
H24A H 0.6464 0.2792 0.5019 0.042 Uiso 1 1 calc R . .
P1 P 0.5000 0.16809(12) 0.7500 0.0878(9) Uani 1 2 d S . .
F1 F 0.5069(4) 0.1671(2) 0.6454(3) 0.1144(15) Uani 1 1 d . . .
F3 F 0.4051(4) 0.0914(4) 0.7269(3) 0.1318(16) Uani 1 1 d . . .
F2 F 0.4078(8) 0.2395(4) 0.7269(4) 0.324(7) Uani 1 1 d . . .
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'
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'
H H 0.0000 0.0000 '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
O31 Os1 O31 81.46(13) 2_656 . ?
O31 Os1 N21 170.54(9) 2_656 . ?
O31 Os1 N21 91.50(10) . . ?
O31 Os1 N21 91.50(10) 2_656 2_656 ?
O31 Os1 N21 170.55(9) . 2_656 ?
N21 Os1 N21 96.16(15) . 2_656 ?
O31 Os1 N11 95.32(10) 2_656 . ?
O31 Os1 N11 90.65(10) . . ?
N21 Os1 N11 78.38(11) . . ?
N21 Os1 N11 96.31(10) 2_656 . ?
O31 Os1 N11 90.65(10) 2_656 2_656 ?
O31 Os1 N11 95.32(10) . 2_656 ?
N21 Os1 N11 96.30(10) . 2_656 ?
N21 Os1 N11 78.38(11) 2_656 2_656 ?
N11 Os1 N11 172.13(16) . 2_656 ?
C32 O31 Os1 112.6(2) . . ?
C16 N11 C12 119.1(3) . . ?
C16 N11 Os1 124.8(2) . . ?
C12 N11 Os1 116.1(2) . . ?
C26 N21 C22 117.8(3) . . ?
C26 N21 Os1 126.1(2) . . ?
C22 N21 Os1 116.0(2) . . ?
N21 C22 C23 121.3(3) . . ?
N21 C22 C12 114.8(3) . . ?
C23 C22 C12 123.8(3) . . ?
N11 C12 C13 121.1(3) . . ?
N11 C12 C22 114.6(3) . . ?
C13 C12 C22 124.2(3) . . ?
N21 C26 C25 122.8(3) . . ?
O31 C32 C33 123.7(3) . . ?
O31 C32 C32 116.67(18) . 2_656 ?
C33 C32 C32 119.7(2) . 2_656 ?
C24 C23 C22 120.1(3) . . ?
C14 C13 C12 119.0(4) . . ?
N11 C16 C15 121.7(3) . . ?
C24 C25 C26 119.1(3) . . ?
C15 C14 C13 119.6(4) . . ?
C34 C33 C32 120.1(4) . . ?
C14 C15 C16 119.4(4) . . ?
C33 C34 C34 120.2(2) . 2_656 ?
C23 C24 C25 118.9(3) . . ?
F2 P1 F2 89.9(7) 2_656 . ?
F2 P1 F3 91.4(4) 2_656 2_656 ?
F2 P1 F3 178.7(4) . 2_656 ?
F2 P1 F3 178.7(4) 2_656 . ?
F2 P1 F3 91.4(4) . . ?
F3 P1 F3 87.4(4) 2_656 . ?
F2 P1 F1 89.3(3) 2_656 2_656 ?
F2 P1 F1 91.4(3) . 2_656 ?
F3 P1 F1 88.9(2) 2_656 2_656 ?
F3 P1 F1 90.3(2) . 2_656 ?
F2 P1 F1 91.4(3) 2_656 . ?
F2 P1 F1 89.3(3) . . ?
F3 P1 F1 90.3(2) 2_656 . ?
F3 P1 F1 88.9(2) . . ?
F1 P1 F1 178.9(3) 2_656 . ?
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 O31 2.018(2) 2_656 ?
Os1 O31 2.018(2) . ?
Os1 N21 2.058(3) . ?
Os1 N21 2.058(3) 2_656 ?
Os1 N11 2.061(3) . ?
Os1 N11 2.061(3) 2_656 ?
O31 C32 1.345(4) . ?
N11 C16 1.354(4) . ?
N11 C12 1.361(4) . ?
N21 C26 1.353(4) . ?
N21 C22 1.363(4) . ?
C22 C23 1.387(5) . ?
C22 C12 1.463(5) . ?
C12 C13 1.393(5) . ?
C26 C25 1.380(5) . ?
C32 C33 1.389(5) . ?
C32 C32 1.425(7) 2_656 ?
C23 C24 1.374(5) . ?
C13 C14 1.385(6) . ?
C16 C15 1.380(5) . ?
C25 C24 1.379(5) . ?
C14 C15 1.379(6) . ?
C33 C34 1.383(6) . ?
C34 C34 1.410(8) 2_656 ?
P1 F2 1.499(6) 2_656 ?
P1 F2 1.499(5) . ?
P1 F3 1.577(5) 2_656 ?
P1 F3 1.577(5) . ?
P1 F1 1.582(3) 2_656 ?
P1 F1 1.582(3) . ?
