#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:56:43 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179085 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/47/4304747.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_4304747
loop_
_publ_author_name
'Kwun-Chi Hwang'
'Jing-Lin Chen'
'Yun Chi'
'Chun-Wei Lin'
'Yi-Ming Cheng'
'Gene-Hsiang Lee'
'Pi-Tai Chou'
'Sue-Yi Lin'
'Ching-Fong Shu'
_publ_section_title
;
Luminescent Osmium(II) Complexes with Functionalized 2-Phenylpyridine
Chelating Ligands: Preparation, Structural Analyses, and Photophysical
Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3307
_journal_page_last               3317
_journal_paper_doi               10.1021/ic7023132
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C24 H12 F4 N2 O2 Os'
_chemical_formula_weight         626.56
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 105.757(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.7294(5)
_cell_length_b                   26.6052(16)
_cell_length_c                   8.9896(5)
_cell_measurement_reflns_used    total
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.00
_cell_volume                     2009.4(2)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'NONIUS COLLECT'
_computing_data_reduction        DENZO-SMN
_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      150(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'NONIUS KappaCCD'
_diffrn_measurement_method       'ω 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  0.0771
_diffrn_reflns_av_sigmaI/netI    0.0979
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            9858
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    6.409
_exptl_absorpt_correction_T_max  0.731
_exptl_absorpt_correction_T_min  0.566
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.071
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.057
_refine_diff_density_min         -0.707
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         3495
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0997
_refine_ls_R_factor_gt           0.0491
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0308P)²+7.2435P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0843
_refine_ls_wR_factor_ref         0.0962
_reflns_number_gt                2260
_reflns_number_total             3495
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic7023132-file003.cif
_cod_data_source_block           ic12594
_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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4304747
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.95939(5) 0.109249(15) 0.81792(4) 0.03690(16) Uani 1 1 d . . .
O1 O 1.2346(8) 0.1067(3) 1.1062(8) 0.0518(18) Uani 1 1 d . . .
O2 O 0.8094(9) 0.0164(3) 0.9262(8) 0.055(2) Uani 1 1 d . . .
N1 N 0.7953(9) 0.1084(3) 0.5922(8) 0.0381(19) Uani 1 1 d . . .
N2 N 0.8158(11) 0.1648(3) 0.8928(8) 0.045(2) Uani 1 1 d . . .
C1 C 1.1251(12) 0.1075(4) 0.9996(12) 0.041(2) Uani 1 1 d . . .
C2 C 0.8630(12) 0.0500(4) 0.8804(10) 0.037(3) Uani 1 1 d . . .
C3 C 0.6415(13) 0.1245(3) 0.5579(12) 0.042(3) Uani 1 1 d . . .
H3 H 0.6036 0.1384 0.6386 0.050 Uiso 1 1 calc R . .
C4 C 0.5381(13) 0.1217(4) 0.4119(11) 0.047(3) Uani 1 1 d . . .
H4 H 0.4318 0.1336 0.3904 0.056 Uiso 1 1 calc R . .
C5 C 0.5970(13) 0.1006(4) 0.2988(12) 0.049(3) Uani 1 1 d . . .
H5 H 0.5285 0.0975 0.1972 0.059 Uiso 1 1 calc R . .
C6 C 0.7509(13) 0.0839(4) 0.3276(11) 0.047(3) Uani 1 1 d . . .
H6 H 0.7882 0.0698 0.2468 0.056 Uiso 1 1 calc R . .
C7 C 0.8525(12) 0.0879(3) 0.4770(11) 0.037(2) Uani 1 1 d . . .
C8 C 1.0137(12) 0.0699(4) 0.5295(11) 0.042(3) Uani 1 1 d . . .
C9 C 1.1068(14) 0.0524(4) 0.4339(11) 0.046(3) Uani 1 1 d . . .
C10 C 1.2605(15) 0.0364(4) 0.4863(13) 0.053(3) Uani 1 1 d . . .
H10 H 1.3198 0.0250 0.4185 0.064 Uiso 1 1 calc R . .
C11 C 1.3223(13) 0.0378(4) 0.6404(14) 0.051(3) Uani 1 1 d . . .
C12 C 1.2455(13) 0.0542(4) 0.7437(12) 0.047(3) Uani 1 1 d . . .
H12 H 1.2971 0.0537 0.8513 0.057 Uiso 1 1 calc R . .
C13 C 1.0901(11) 0.0719(4) 0.6901(11) 0.037(3) Uani 1 1 d . . .
C14 C 0.6911(14) 0.1535(4) 0.9513(11) 0.054(3) Uani 1 1 d . . .
H14 H 0.6734 0.1191 0.9702 0.065 Uiso 1 1 calc R . .
C15 C 0.5892(15) 0.1885(4) 0.9850(12) 0.060(3) Uani 1 1 d . . .
H15 H 0.5050 0.1789 1.0272 0.072 Uiso 1 1 calc R . .
C16 C 0.6148(15) 0.2373(5) 0.9549(12) 0.064(3) Uani 1 1 d . . .
H16 H 0.5458 0.2627 0.9739 0.076 Uiso 1 1 calc R . .
C17 C 0.7416(15) 0.2505(4) 0.8964(12) 0.059(3) Uani 1 1 d . . .
H17 H 0.7616 0.2848 0.8792 0.071 Uiso 1 1 calc R . .
C18 C 0.8386(14) 0.2132(4) 0.8633(11) 0.048(3) Uani 1 1 d . . .
C19 C 0.9742(13) 0.2219(4) 0.7961(11) 0.046(3) Uani 1 1 d . . .
C20 C 1.0308(15) 0.2682(4) 0.7699(13) 0.051(3) Uani 1 1 d . . .
C21 C 1.1561(16) 0.2743(5) 0.7085(14) 0.064(4) Uani 1 1 d . . .
H21 H 1.1919 0.3068 0.6895 0.077 Uiso 1 1 calc R . .
C22 C 1.2272(15) 0.2323(6) 0.6758(12) 0.062(4) Uani 1 1 d . . .
C23 C 1.1789(13) 0.1848(4) 0.6962(11) 0.051(3) Uani 1 1 d . . .
H23 H 1.2315 0.1564 0.6688 0.061 Uiso 1 1 calc R . .
C24 C 1.0484(12) 0.1788(4) 0.7591(11) 0.040(3) Uani 1 1 d . . .
F1 F 1.0366(8) 0.0512(3) 0.2780(7) 0.077(2) Uani 1 1 d . . .
F2 F 1.4766(8) 0.0221(3) 0.6990(8) 0.078(2) Uani 1 1 d . . .
F3 F 0.9593(9) 0.3115(2) 0.8038(8) 0.090(2) Uani 1 1 d . . .
F4 F 1.3498(9) 0.2376(3) 0.6120(9) 0.098(3) 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'
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
C1 Os C2 91.2(4) . . ?
C1 Os C13 93.5(4) . . ?
C2 Os C13 96.8(4) . . ?
C1 Os C24 89.4(4) . . ?
C2 Os C24 173.9(4) . . ?
C13 Os C24 89.2(4) . . ?
C1 Os N1 171.5(4) . . ?
C2 Os N1 92.0(3) . . ?
C13 Os N1 78.3(3) . . ?
C24 Os N1 88.2(3) . . ?
C1 Os N2 97.0(4) . . ?
C2 Os N2 97.6(4) . . ?
C13 Os N2 162.0(3) . . ?
C24 Os N2 76.4(4) . . ?
N1 Os N2 90.4(3) . . ?
C3 N1 C7 119.3(8) . . ?
C3 N1 Os 125.1(6) . . ?
C7 N1 Os 115.5(6) . . ?
C18 N2 C14 117.7(9) . . ?
C18 N2 Os 117.7(7) . . ?
C14 N2 Os 124.1(7) . . ?
O1 C1 Os 175.5(8) . . ?
O2 C2 Os 175.7(8) . . ?
N1 C3 C4 123.3(9) . . ?
C5 C4 C3 116.5(10) . . ?
C6 C5 C4 122.4(10) . . ?
C5 C6 C7 119.4(10) . . ?
N1 C7 C6 119.1(9) . . ?
N1 C7 C8 114.0(8) . . ?
C6 C7 C8 126.8(9) . . ?
C9 C8 C13 116.3(10) . . ?
C9 C8 C7 125.6(9) . . ?
C13 C8 C7 118.0(9) . . ?
C10 C9 F1 118.1(10) . . ?
C10 C9 C8 124.6(10) . . ?
F1 C9 C8 117.3(10) . . ?
C11 C10 C9 115.4(10) . . ?
C10 C11 C12 125.4(11) . . ?
C10 C11 F2 117.7(10) . . ?
C12 C11 F2 116.8(10) . . ?
C11 C12 C13 119.2(10) . . ?
C12 C13 C8 119.0(9) . . ?
C12 C13 Os 126.9(8) . . ?
C8 C13 Os 113.8(7) . . ?
N2 C14 C15 124.5(10) . . ?
C16 C15 C14 116.9(12) . . ?
C15 C16 C17 120.3(11) . . ?
C18 C17 C16 119.7(11) . . ?
N2 C18 C17 120.8(11) . . ?
N2 C18 C19 114.1(10) . . ?
C17 C18 C19 125.1(11) . . ?
C20 C19 C24 118.9(10) . . ?
C20 C19 C18 125.0(10) . . ?
C24 C19 C18 116.1(9) . . ?
C21 C20 C19 122.8(11) . . ?
C21 C20 F3 116.8(11) . . ?
C19 C20 F3 120.4(11) . . ?
C22 C21 C20 117.2(11) . . ?
C21 C22 F4 118.1(12) . . ?
C21 C22 C23 124.2(12) . . ?
F4 C22 C23 117.6(14) . . ?
C22 C23 C24 118.1(11) . . ?
C19 C24 C23 118.7(9) . . ?
C19 C24 Os 115.4(7) . . ?
C23 C24 Os 125.8(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 C1 1.865(11) . ?
Os C2 1.940(12) . ?
Os C13 2.078(9) . ?
Os C24 2.129(9) . ?
Os N1 2.142(7) . ?
Os N2 2.159(8) . ?
O1 C1 1.155(11) . ?
O2 C2 1.137(11) . ?
N1 C3 1.363(12) . ?
N1 C7 1.379(11) . ?
N2 C18 1.340(12) . ?
N2 C14 1.365(13) . ?
C3 C4 1.378(13) . ?
C4 C5 1.377(14) . ?
C5 C6 1.371(14) . ?
C6 C7 1.398(13) . ?
C7 C8 1.438(13) . ?
C8 C9 1.413(13) . ?
C8 C13 1.418(13) . ?
C9 C10 1.364(14) . ?
C9 F1 1.369(11) . ?
C10 C11 1.343(14) . ?
C11 C12 1.357(14) . ?
C11 F2 1.372(12) . ?
C12 C13 1.392(13) . ?
C14 C15 1.376(14) . ?
C15 C16 1.359(15) . ?
C16 C17 1.393(15) . ?
C17 C18 1.389(15) . ?
C18 C19 1.485(15) . ?
C19 C20 1.373(14) . ?
C19 C24 1.400(14) . ?
C20 C21 1.362(16) . ?
C20 F3 1.382(12) . ?
C21 C22 1.349(16) . ?
C22 F4 1.351(13) . ?
C22 C23 1.362(15) . ?
C23 C24 1.412(14) . ?
