#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:48:10 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179129 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/91/4309142.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_4309142
loop_
_publ_author_name
'Yi-Ming Cheng'
'Yu-Shan Yeh'
'Mei-Lin Ho'
'Pi-Tai Chou'
'Po-Shen Chen'
'Yun Chi'
_publ_section_title
;
Dual Room-Temperature Fluorescent and Phosphorescent Emission in
8-Quinolinolate Osmium(II) Carbonyl Complexes: Rationalization and
Generalization of Intersystem Crossing Dynamics
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4594
_journal_page_last               4603
_journal_paper_doi               10.1021/ic0505347
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C15 H8 F3 N O6 Os'
_chemical_formula_weight         545.42
_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                90.00
_cell_angle_beta                 100.979(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.5579(5)
_cell_length_b                   9.3166(4)
_cell_length_c                   25.7751(10)
_cell_measurement_reflns_used    5205
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      24.76
_cell_measurement_theta_min      2.67
_cell_volume                     3196.2(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART ApexCCD area detector'
_diffrn_measurement_method       'omega scans'
_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  0.0406
_diffrn_reflns_av_sigmaI/netI    0.0294
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            20278
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.67
_exptl_absorpt_coefficient_mu    8.046
_exptl_absorpt_correction_T_max  0.5000
_exptl_absorpt_correction_T_min  0.2960
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.267
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         3679
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0239
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0209P)²+5.1823P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0507
_refine_ls_wR_factor_ref         0.0528
_reflns_number_gt                3270
_reflns_number_total             3679
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0505347si20050511_022616_2.cif
_cod_data_source_block           complex5
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4309142
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
Os Os 0.210046(11) 0.526941(16) 0.656726(5) 0.03094(6) Uani 1 1 d . . .
O1 O 0.1132(3) 0.4939(4) 0.75301(13) 0.0634(10) Uani 1 1 d . . .
O2 O 0.3837(2) 0.6641(4) 0.73301(12) 0.0572(8) Uani 1 1 d . . .
O3 O 0.3159(3) 0.2415(4) 0.67410(14) 0.0713(10) Uani 1 1 d . . .
O4 O 0.2761(2) 0.5675(3) 0.59290(10) 0.0389(6) Uani 1 1 d . . .
O5 O 0.1312(2) 0.7179(3) 0.63384(10) 0.0377(6) Uani 1 1 d . . .
O6 O 0.1794(3) 0.8374(4) 0.70904(14) 0.0886(14) Uani 1 1 d . . .
N1 N 0.1022(2) 0.4326(3) 0.59472(11) 0.0309(7) Uani 1 1 d . . .
C1 C 0.1476(3) 0.5038(4) 0.71688(17) 0.0414(10) Uani 1 1 d . . .
C2 C 0.3179(3) 0.6173(4) 0.70455(15) 0.0387(9) Uani 1 1 d . . .
C3 C 0.2767(3) 0.3476(5) 0.66884(15) 0.0451(10) Uani 1 1 d . . .
C4 C 0.2317(3) 0.4989(4) 0.54917(16) 0.0362(9) Uani 1 1 d . . .
C5 C 0.2717(4) 0.4954(5) 0.50400(18) 0.0488(11) Uani 1 1 d . . .
H5A H 0.3324 0.5417 0.5037 0.059 Uiso 1 1 calc R . .
C6 C 0.2235(4) 0.4245(6) 0.45883(17) 0.0554(12) Uani 1 1 d . . .
H6A H 0.2527 0.4231 0.4290 0.066 Uiso 1 1 calc R . .
C7 C 0.1337(4) 0.3568(5) 0.45766(16) 0.0503(11) Uani 1 1 d . . .
H7A H 0.1020 0.3108 0.4270 0.060 Uiso 1 1 calc R . .
C8 C 0.0888(3) 0.3561(4) 0.50287(15) 0.0397(9) Uani 1 1 d . . .
C9 C 0.1398(3) 0.4275(4) 0.54861(14) 0.0317(8) Uani 1 1 d . . .
C10 C -0.0039(3) 0.2924(5) 0.50550(15) 0.0451(10) Uani 1 1 d . . .
H10A H -0.0401 0.2446 0.4763 0.054 Uiso 1 1 calc R . .
C11 C -0.0404(3) 0.3008(4) 0.55081(16) 0.0444(10) Uani 1 1 d . . .
H11A H -0.1019 0.2583 0.5524 0.053 Uiso 1 1 calc R . .
C12 C 0.0129(3) 0.3725(4) 0.59547(15) 0.0363(8) Uani 1 1 d . . .
C13 C -0.0321(3) 0.3819(6) 0.64376(17) 0.0533(12) Uani 1 1 d . . .
H13A H 0.0126 0.4331 0.6708 0.080 Uiso 1 1 calc R . .
H13B H -0.0429 0.2869 0.6560 0.080 Uiso 1 1 calc R . .
H13C H -0.0952 0.4316 0.6355 0.080 Uiso 1 1 calc R . .
C14 C 0.1348(3) 0.8249(4) 0.66412(16) 0.0408(9) Uani 1 1 d . . .
C15 C 0.0712(4) 0.9520(5) 0.64070(19) 0.0493(11) Uani 1 1 d . . .
F1 F 0.0217(14) 0.9352(19) 0.5937(6) 0.111(8) Uani 0.50 1 d P . .
F2 F 0.0038(12) 0.9824(18) 0.6708(6) 0.091(4) Uani 0.50 1 d P . .
F3 F 0.1281(14) 1.0672(17) 0.6458(8) 0.091(5) Uani 0.50 1 d P . .
F1' F 0.0680(13) 0.9618(19) 0.5884(6) 0.090(6) Uani 0.50 1 d P . .
F2' F -0.0175(11) 0.936(2) 0.6457(7) 0.129(6) Uani 0.50 1 d P . .
F3' F 0.1012(14) 1.0736(19) 0.6569(7) 0.108(7) Uani 0.50 1 d P . .
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'
F F 0.0171 0.0103 '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
C3 Os C1 92.15(18) . . ?
C3 Os C2 90.00(17) . . ?
C1 Os C2 85.97(17) . . ?
C3 Os O4 91.57(15) . . ?
C1 Os O4 175.86(15) . . ?
C2 Os O4 92.22(14) . . ?
C3 Os O5 173.15(13) . . ?
C1 Os O5 92.47(15) . . ?
C2 Os O5 95.36(14) . . ?
O4 Os O5 83.99(11) . . ?
C3 Os N1 89.84(15) . . ?
C1 Os N1 102.35(15) . . ?
C2 Os N1 171.68(14) . . ?
O4 Os N1 79.47(11) . . ?
O5 Os N1 84.23(11) . . ?
C4 O4 Os 113.2(2) . . ?
C14 O5 Os 122.5(2) . . ?
C12 N1 C9 118.8(3) . . ?
C12 N1 Os 130.8(2) . . ?
C9 N1 Os 110.2(2) . . ?
O1 C1 Os 177.5(4) . . ?
O2 C2 Os 176.6(4) . . ?
O3 C3 Os 177.5(4) . . ?
O4 C4 C5 122.6(4) . . ?
O4 C4 C9 119.3(3) . . ?
C5 C4 C9 118.1(4) . . ?
C4 C5 C6 121.5(4) . . ?
C7 C6 C5 120.9(4) . . ?
C6 C7 C8 120.4(4) . . ?
C10 C8 C7 124.9(4) . . ?
C10 C8 C9 117.3(4) . . ?
C7 C8 C9 117.8(4) . . ?
N1 C9 C4 116.5(3) . . ?
N1 C9 C8 122.1(3) . . ?
C4 C9 C8 121.4(3) . . ?
C11 C10 C8 119.7(4) . . ?
C10 C11 C12 121.2(4) . . ?
N1 C12 C11 120.9(4) . . ?
N1 C12 C13 120.3(3) . . ?
C11 C12 C13 118.9(4) . . ?
O6 C14 O5 128.6(4) . . ?
O6 C14 C15 116.7(4) . . ?
O5 C14 C15 114.7(3) . . ?
F2' C15 F3' 109.4(13) . . ?
F2' C15 F1 74.9(11) . . ?
F3' C15 F1 120.4(12) . . ?
F2' C15 F3 130.3(12) . . ?
F3' C15 F3 22.7(14) . . ?
F1 C15 F3 112.7(13) . . ?
F2' C15 F2 35.2(9) . . ?
F3' C15 F2 80.1(11) . . ?
F1 C15 F2 106.4(11) . . ?
F3 C15 F2 102.8(10) . . ?
F2' C15 F1' 105.4(11) . . ?
F3' C15 F1' 102.7(12) . . ?
F1 C15 F1' 31.4(12) . . ?
F3 C15 F1' 87.2(12) . . ?
F2 C15 F1' 132.3(10) . . ?
F2' C15 C14 110.8(9) . . ?
F3' C15 C14 116.7(9) . . ?
F1 C15 C14 115.9(8) . . ?
F3 C15 C14 108.6(10) . . ?
F2 C15 C14 109.5(9) . . ?
F1' C15 C14 111.0(9) . . ?
F1' F1 C15 79(2) . . ?
F1' F1 F2' 129(3) . . ?
C15 F1 F2' 51.5(8) . . ?
F2' F2 C15 65.8(18) . . ?
F2' F2 F3' 106(3) . . ?
C15 F2 F3' 47.6(8) . . ?
F3' F3 C15 71(3) . . ?
F1 F1' C15 69(2) . . ?
F2 F2' C15 79(2) . . ?
F2 F2' F1 126(3) . . ?
C15 F2' F1 53.6(9) . . ?
F3 F3' C15 86(4) . . ?
F3 F3' F2 138(4) . . ?
C15 F3' F2 52.3(8) . . ?
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
Os C3 1.897(5) . ?
Os C1 1.915(4) . ?
Os C2 1.919(4) . ?
Os O4 2.052(2) . ?
Os O5 2.102(3) . ?
Os N1 2.139(3) . ?
O1 C1 1.122(5) . ?
O2 C2 1.128(5) . ?
O3 C3 1.118(5) . ?
O4 C4 1.335(5) . ?
O5 C14 1.261(5) . ?
O6 C14 1.205(5) . ?
N1 C12 1.336(5) . ?
N1 C9 1.381(4) . ?
C4 C5 1.375(6) . ?
C4 C9 1.410(5) . ?
C5 C6 1.389(6) . ?
C6 C7 1.366(7) . ?
C7 C8 1.414(6) . ?
C8 C10 1.404(6) . ?
C8 C9 1.414(5) . ?
C10 C11 1.355(5) . ?
C11 C12 1.407(5) . ?
C12 C13 1.490(5) . ?
C14 C15 1.520(6) . ?
C15 F2' 1.241(15) . ?
C15 F3' 1.248(17) . ?
C15 F1 1.277(16) . ?
C15 F3 1.314(15) . ?
C15 F2 1.337(16) . ?
C15 F1' 1.343(16) . ?
F1 F1' 0.71(3) . ?
F1 F2' 1.53(2) . ?
F2 F2' 0.78(2) . ?
F2 F3' 1.67(3) . ?
F3 F3' 0.51(3) . ?
