#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:48:10 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179129 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/91/4309141.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_4309141
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            'C14 H5 F4 N O6 Os'
_chemical_formula_weight         549.39
_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                 117.088(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.2840(6)
_cell_length_b                   10.5425(3)
_cell_length_c                   16.8868(5)
_cell_measurement_reflns_used    5577
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.17
_cell_measurement_theta_min      2.35
_cell_volume                     3056.53(16)
_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  0.0332
_diffrn_reflns_av_sigmaI/netI    0.0294
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14920
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.27
_exptl_absorpt_coefficient_mu    8.424
_exptl_absorpt_correction_T_max  0.2475
_exptl_absorpt_correction_T_min  0.2014
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            deep-yellow
_exptl_crystal_density_diffrn    2.388
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.512
_refine_diff_density_min         -0.703
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       0.00119(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         3511
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0245
_refine_ls_R_factor_gt           0.0206
_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)+(0.0148P)²+2.6549P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0429
_refine_ls_wR_factor_ref         0.0441
_reflns_number_gt                3183
_reflns_number_total             3511
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0505347si20050511_022616_1.cif
_cod_data_source_block           complex4
_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               4309141
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 0.745671(7) 0.631266(11) 0.863338(8) 0.02592(6) Uani 1 1 d . . .
O5 O 0.82588(13) 0.7727(2) 0.93567(15) 0.0316(5) Uani 1 1 d . . .
O2 O 0.72353(17) 0.7322(2) 0.68498(17) 0.0484(7) Uani 1 1 d . . .
O4 O 0.77267(13) 0.5646(2) 0.98825(15) 0.0328(5) Uani 1 1 d . . .
F3 F 0.84219(15) 1.0825(2) 0.98467(18) 0.0620(7) Uani 1 1 d . . .
C1 C 0.6580(2) 0.7293(3) 0.8535(2) 0.0354(8) Uani 1 1 d . . .
C12 C 0.87025(19) 0.4547(3) 0.9681(2) 0.0274(7) Uani 1 1 d . . .
F1 F 1.01422(15) 0.2264(2) 1.10705(18) 0.0661(7) Uani 1 1 d . . .
N1 N 0.84463(15) 0.5196(2) 0.88886(17) 0.0267(6) Uani 1 1 d . . .
O6 O 0.76441(15) 0.9298(2) 0.83870(16) 0.0398(6) Uani 1 1 d . . .
F4 F 0.91881(15) 1.0231(3) 0.93440(19) 0.0715(8) Uani 1 1 d . . .
O1 O 0.60377(16) 0.7833(3) 0.84314(19) 0.0494(7) Uani 1 1 d . . .
F2 F 0.92195(17) 0.9331(2) 1.04898(17) 0.0770(9) Uani 1 1 d . . .
C13 C 0.8148(2) 0.8873(3) 0.9082(2) 0.0301(7) Uani 1 1 d . . .
C7 C 0.9329(2) 0.3684(3) 0.9956(2) 0.0337(8) Uani 1 1 d . . .
C4 C 0.8805(2) 0.5006(3) 0.8392(2) 0.0339(8) Uani 1 1 d . . .
H4A H 0.8633 0.5449 0.7860 0.041 Uiso 1 1 calc R . .
C2 C 0.7311(2) 0.6958(3) 0.7512(2) 0.0325(7) Uani 1 1 d . . .
O3 O 0.63565(18) 0.4133(3) 0.7744(2) 0.0603(8) Uani 1 1 d . . .
C14 C 0.8748(2) 0.9805(4) 0.9706(3) 0.0405(8) Uani 1 1 d . . .
C6 C 0.9693(2) 0.3507(3) 0.9409(3) 0.0414(9) Uani 1 1 d . . .
H6A H 1.0108 0.2947 0.9574 0.050 Uiso 1 1 calc R . .
C11 C 0.8298(2) 0.4797(3) 1.0183(2) 0.0296(7) Uani 1 1 d . . .
C5 C 0.9428(2) 0.4171(4) 0.8633(3) 0.0409(9) Uani 1 1 d . . .
H5A H 0.9663 0.4066 0.8264 0.049 Uiso 1 1 calc R . .
C8 C 0.9531(2) 0.3081(3) 1.0773(3) 0.0426(9) Uani 1 1 d . . .
C10 C 0.8528(2) 0.4145(3) 1.0966(2) 0.0398(8) Uani 1 1 d . . .
H10A H 0.8266 0.4278 1.1306 0.048 Uiso 1 1 calc R . .
C3 C 0.6780(2) 0.4939(3) 0.8072(2) 0.0370(8) Uani 1 1 d . . .
C9 C 0.9149(2) 0.3283(4) 1.1264(3) 0.0450(9) Uani 1 1 d . . .
H9A H 0.9298 0.2852 1.1797 0.054 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'
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 Os1 C2 91.09(15) . . ?
C3 Os1 C1 89.36(15) . . ?
C2 Os1 C1 89.78(15) . . ?
C3 Os1 O4 92.72(13) . . ?
C2 Os1 O4 174.47(12) . . ?
C1 Os1 O4 94.26(12) . . ?
C3 Os1 O5 174.77(12) . . ?
C2 Os1 O5 93.51(12) . . ?
C1 Os1 O5 93.15(13) . . ?
O4 Os1 O5 82.52(9) . . ?
C3 Os1 N1 91.64(13) . . ?
C2 Os1 N1 96.45(12) . . ?
C1 Os1 N1 173.66(12) . . ?
O4 Os1 N1 79.44(9) . . ?
O5 Os1 N1 85.36(9) . . ?
C13 O5 Os1 120.3(2) . . ?
C11 O4 Os1 113.66(19) . . ?
O1 C1 Os1 176.0(3) . . ?
N1 C12 C7 120.9(3) . . ?
N1 C12 C11 115.9(3) . . ?
C7 C12 C11 123.2(3) . . ?
C4 N1 C12 118.7(3) . . ?
C4 N1 Os1 129.7(2) . . ?
C12 N1 Os1 111.4(2) . . ?
O6 C13 O5 128.7(3) . . ?
O6 C13 C14 116.9(3) . . ?
O5 C13 C14 114.3(3) . . ?
C8 C7 C6 126.1(3) . . ?
C8 C7 C12 115.4(3) . . ?
C6 C7 C12 118.6(3) . . ?
N1 C4 C5 122.8(3) . . ?
O2 C2 Os1 178.6(3) . . ?
F2 C14 F3 107.2(3) . . ?
F2 C14 F4 107.3(3) . . ?
F3 C14 F4 105.3(3) . . ?
F2 C14 C13 114.3(3) . . ?
F3 C14 C13 112.2(3) . . ?
F4 C14 C13 110.1(3) . . ?
C5 C6 C7 118.9(3) . . ?
O4 C11 C10 123.6(3) . . ?
O4 C11 C12 119.0(3) . . ?
C10 C11 C12 117.4(3) . . ?
C6 C5 C4 120.1(3) . . ?
C9 C8 F1 119.7(3) . . ?
C9 C8 C7 123.1(3) . . ?
F1 C8 C7 117.2(4) . . ?
C11 C10 C9 121.2(3) . . ?
O3 C3 Os1 177.7(3) . . ?
C8 C9 C10 119.8(3) . . ?
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 C3 1.891(4) . ?
Os1 C2 1.908(4) . ?
Os1 C1 1.924(4) . ?
Os1 O4 2.053(2) . ?
Os1 O5 2.094(2) . ?
Os1 N1 2.113(3) . ?
O5 C13 1.277(4) . ?
O2 C2 1.127(4) . ?
O4 C11 1.328(4) . ?
F3 C14 1.320(4) . ?
C1 O1 1.132(4) . ?
C12 N1 1.379(4) . ?
C12 C7 1.411(4) . ?
C12 C11 1.413(4) . ?
F1 C8 1.358(4) . ?
N1 C4 1.322(4) . ?
O6 C13 1.218(4) . ?
F4 C14 1.330(4) . ?
F2 C14 1.316(4) . ?
C13 C14 1.518(5) . ?
C7 C8 1.403(5) . ?
C7 C6 1.403(5) . ?
C4 C5 1.392(5) . ?
O3 C3 1.133(4) . ?
C6 C5 1.364(5) . ?
C11 C10 1.373(5) . ?
C8 C9 1.355(6) . ?
C10 C9 1.401(5) . ?
