#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:56:43 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179085 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/47/4304745.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_4304745
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            'C36 H25 F4 N2 O Os P'
_chemical_formula_weight         798.75
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 93.203(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.7517(5)
_cell_length_b                   17.2482(9)
_cell_length_c                   19.8393(10)
_cell_measurement_reflns_used    3218
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      21.86
_cell_measurement_theta_min      2.36
_cell_volume                     2990.1(3)
_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  0.0581
_diffrn_reflns_av_sigmaI/netI    0.0642
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            19394
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.36
_exptl_absorpt_coefficient_mu    4.377
_exptl_absorpt_correction_T_max  0.7492
_exptl_absorpt_correction_T_min  0.3845
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.774
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.186
_refine_diff_density_min         -1.225
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         6874
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0432
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0219P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0756
_refine_ls_wR_factor_ref         0.0813
_reflns_number_gt                5468
_reflns_number_total             6874
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic7023132-file001.cif
_cod_data_source_block           ic12149
_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               4304745
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Os Os 0.36702(2) 0.198662(12) 0.041326(9) 0.03152(7) Uani 1 1 d . . .
P1 P 0.48325(16) 0.24934(8) -0.05429(6) 0.0339(3) Uani 1 1 d . . .
O1 O 0.5722(4) 0.0600(2) 0.04496(19) 0.0479(10) Uani 1 1 d . . .
N1 N 0.2503(5) 0.3058(3) 0.0592(2) 0.0394(11) Uani 1 1 d . . .
N2 N 0.1589(5) 0.1503(3) -0.0062(2) 0.0396(11) Uani 1 1 d . . .
C1 C 0.4879(6) 0.1124(3) 0.0411(2) 0.0330(12) Uani 1 1 d . . .
C2 C 0.5230(6) 0.2555(3) 0.1038(2) 0.0310(11) Uani 1 1 d . . .
C3 C 0.6676(6) 0.2296(3) 0.1274(2) 0.0403(13) Uani 1 1 d . . .
H3 H 0.7057 0.1833 0.1111 0.048 Uiso 1 1 calc R . .
C4 C 0.7529(7) 0.2709(3) 0.1735(3) 0.0495(15) Uani 1 1 d . . .
C5 C 0.7045(7) 0.3369(3) 0.2037(3) 0.0528(16) Uani 1 1 d . . .
H5 H 0.7631 0.3624 0.2374 0.063 Uiso 1 1 calc R . .
C6 C 0.5631(7) 0.3628(3) 0.1806(3) 0.0465(15) Uani 1 1 d . . .
C7 C 0.4709(6) 0.3265(3) 0.1308(2) 0.0339(12) Uani 1 1 d . . .
C8 C 0.3249(6) 0.3559(3) 0.1029(2) 0.0360(12) Uani 1 1 d . . .
C9 C 0.2628(7) 0.4288(3) 0.1146(3) 0.0521(16) Uani 1 1 d . . .
H9 H 0.3155 0.4641 0.1426 0.063 Uiso 1 1 calc R . .
C10 C 0.1232(8) 0.4480(4) 0.0842(3) 0.0604(18) Uani 1 1 d . . .
H10 H 0.0808 0.4964 0.0922 0.072 Uiso 1 1 calc R . .
C11 C 0.0463(8) 0.3970(4) 0.0426(3) 0.0642(19) Uani 1 1 d . . .
H11 H -0.0497 0.4093 0.0231 0.077 Uiso 1 1 calc R . .
C12 C 0.1135(7) 0.3266(4) 0.0300(3) 0.0502(15) Uani 1 1 d . . .
H12 H 0.0629 0.2923 0.0004 0.060 Uiso 1 1 calc R . .
C13 C 0.2567(6) 0.1517(3) 0.1232(3) 0.0386(13) Uani 1 1 d . . .
C14 C 0.3150(7) 0.1509(3) 0.1903(3) 0.0437(14) Uani 1 1 d . . .
H14 H 0.4094 0.1732 0.2021 0.052 Uiso 1 1 calc R . .
C15 C 0.2309(8) 0.1165(3) 0.2386(3) 0.0535(17) Uani 1 1 d . . .
C16 C 0.0898(8) 0.0845(3) 0.2249(3) 0.0589(18) Uani 1 1 d . . .
H16 H 0.0341 0.0629 0.2588 0.071 Uiso 1 1 calc R . .
C17 C 0.0347(7) 0.0858(4) 0.1598(4) 0.0553(16) Uani 1 1 d . . .
C18 C 0.1138(6) 0.1170(3) 0.1077(3) 0.0413(13) Uani 1 1 d . . .
C19 C 0.0600(6) 0.1171(3) 0.0364(3) 0.0410(13) Uani 1 1 d . . .
C20 C -0.0784(7) 0.0864(4) 0.0109(4) 0.0579(17) Uani 1 1 d . . .
H20 H -0.1452 0.0639 0.0400 0.069 Uiso 1 1 calc R . .
C21 C -0.1170(7) 0.0894(4) -0.0576(4) 0.066(2) Uani 1 1 d . . .
H21 H -0.2098 0.0691 -0.0747 0.080 Uiso 1 1 calc R . .
C22 C -0.0171(7) 0.1225(4) -0.1003(4) 0.065(2) Uani 1 1 d . . .
H22 H -0.0396 0.1248 -0.1466 0.079 Uiso 1 1 calc R . .
C23 C 0.1176(7) 0.1520(4) -0.0717(3) 0.0548(16) Uani 1 1 d . . .
H23 H 0.1849 0.1749 -0.1004 0.066 Uiso 1 1 calc R . .
C24 C 0.6755(7) 0.2891(4) -0.0367(3) 0.0533(16) Uani 1 1 d . . .
H24A H 0.7111 0.3121 -0.0770 0.080 Uiso 1 1 calc R . .
H24B H 0.7438 0.2483 -0.0218 0.080 Uiso 1 1 calc R . .
H24C H 0.6722 0.3278 -0.0020 0.080 Uiso 1 1 calc R . .
C25 C 0.5187(6) 0.1827(3) -0.1236(2) 0.0363(12) Uani 1 1 d . . .
C26 C 0.6022(7) 0.2073(3) -0.1773(3) 0.0473(15) Uani 1 1 d . . .
H26 H 0.6333 0.2587 -0.1800 0.057 Uiso 1 1 calc R . .
C27 C 0.6386(7) 0.1552(4) -0.2266(3) 0.0522(16) Uani 1 1 d . . .
H27 H 0.6942 0.1719 -0.2625 0.063 Uiso 1 1 calc R . .
C28 C 0.5945(8) 0.0795(4) -0.2237(3) 0.0602(19) Uani 1 1 d . . .
H28 H 0.6218 0.0448 -0.2569 0.072 Uiso 1 1 calc R . .
C29 C 0.5100(7) 0.0545(4) -0.1717(3) 0.0514(16) Uani 1 1 d . . .
H29 H 0.4783 0.0031 -0.1699 0.062 Uiso 1 1 calc R . .
C30 C 0.4723(6) 0.1061(3) -0.1220(3) 0.0428(14) Uani 1 1 d . . .
H30 H 0.4147 0.0890 -0.0869 0.051 Uiso 1 1 calc R . .
C31 C 0.3865(6) 0.3316(3) -0.0963(3) 0.0405(13) Uani 1 1 d . . .
C32 C 0.2931(7) 0.3229(4) -0.1551(3) 0.0555(17) Uani 1 1 d . . .
H32 H 0.2847 0.2746 -0.1759 0.067 Uiso 1 1 calc R . .
C33 C 0.2127(8) 0.3857(5) -0.1827(4) 0.075(2) Uani 1 1 d . . .
H33 H 0.1499 0.3795 -0.2216 0.089 Uiso 1 1 calc R . .
C34 C 0.2262(8) 0.4566(5) -0.1524(4) 0.075(2) Uani 1 1 d . . .
H34 H 0.1732 0.4987 -0.1712 0.090 Uiso 1 1 calc R . .
C35 C 0.3156(9) 0.4661(4) -0.0955(4) 0.073(2) Uani 1 1 d . . .
H35 H 0.3238 0.5147 -0.0753 0.088 Uiso 1 1 calc R . .
C36 C 0.3950(8) 0.4040(4) -0.0669(3) 0.0597(17) Uani 1 1 d . . .
H36 H 0.4552 0.4111 -0.0273 0.072 Uiso 1 1 calc R . .
F1 F 0.8939(4) 0.2437(2) 0.19357(18) 0.0774(12) Uani 1 1 d . . .
F2 F 0.5103(4) 0.4269(2) 0.21155(17) 0.0692(11) Uani 1 1 d . . .
F3 F 0.2914(5) 0.1143(2) 0.30357(17) 0.0746(12) Uani 1 1 d . . .
F4 F -0.1066(4) 0.0544(2) 0.1483(2) 0.0797(12) 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'
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'
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 91.4(2) . . ?
C1 Os C13 88.8(2) . . ?
C2 Os C13 92.1(2) . . ?
C1 Os N1 168.91(18) . . ?
C2 Os N1 78.18(18) . . ?
C13 Os N1 87.74(18) . . ?
C1 Os N2 99.09(18) . . ?
C2 Os N2 164.65(18) . . ?
C13 Os N2 77.08(19) . . ?
N1 Os N2 90.40(17) . . ?
C1 Os P1 91.38(16) . . ?
C2 Os P1 90.36(13) . . ?
C13 Os P1 177.53(16) . . ?
N1 Os P1 92.52(12) . . ?
N2 Os P1 100.46(12) . . ?
C31 P1 C25 103.8(2) . . ?
C31 P1 C24 101.1(3) . . ?
C25 P1 C24 100.7(3) . . ?
C31 P1 Os 116.25(18) . . ?
C25 P1 Os 117.90(18) . . ?
C24 P1 Os 114.58(18) . . ?
C12 N1 C8 119.1(5) . . ?
C12 N1 Os 125.2(4) . . ?
C8 N1 Os 115.7(3) . . ?
C23 N2 C19 117.8(5) . . ?
C23 N2 Os 126.2(4) . . ?
C19 N2 Os 115.9(3) . . ?
O1 C1 Os 174.6(4) . . ?
C3 C2 C7 116.8(4) . . ?
C3 C2 Os 127.8(4) . . ?
C7 C2 Os 115.1(4) . . ?
C4 C3 C2 120.9(5) . . ?
C3 C4 F1 118.3(5) . . ?
C3 C4 C5 124.3(6) . . ?
F1 C4 C5 117.3(5) . . ?
C4 C5 C6 115.0(5) . . ?
F2 C6 C5 116.0(5) . . ?
F2 C6 C7 119.3(5) . . ?
C5 C6 C7 124.6(5) . . ?
C6 C7 C2 118.1(5) . . ?
C6 C7 C8 125.2(5) . . ?
C2 C7 C8 116.7(4) . . ?
N1 C8 C9 120.0(5) . . ?
N1 C8 C7 113.6(4) . . ?
C9 C8 C7 126.3(5) . . ?
C10 C9 C8 119.3(6) . . ?
C11 C10 C9 120.6(6) . . ?
C10 C11 C12 118.6(6) . . ?
N1 C12 C11 122.3(6) . . ?
C14 C13 C18 118.5(5) . . ?
C14 C13 Os 125.6(4) . . ?
C18 C13 Os 115.9(4) . . ?
C15 C14 C13 119.1(6) . . ?
C16 C15 F3 118.3(6) . . ?
C16 C15 C14 123.3(6) . . ?
F3 C15 C14 118.4(6) . . ?
C17 C16 C15 116.9(6) . . ?
C16 C17 F4 115.2(6) . . ?
C16 C17 C18 123.5(6) . . ?
F4 C17 C18 121.3(6) . . ?
C17 C18 C13 118.6(5) . . ?
C17 C18 C19 125.0(6) . . ?
C13 C18 C19 116.4(5) . . ?
N2 C19 C20 120.1(5) . . ?
N2 C19 C18 114.6(5) . . ?
C20 C19 C18 125.3(6) . . ?
C21 C20 C19 120.3(6) . . ?
C22 C21 C20 119.4(6) . . ?
C21 C22 C23 117.4(6) . . ?
N2 C23 C22 125.0(6) . . ?
C30 C25 C26 118.4(5) . . ?
C30 C25 P1 121.3(4) . . ?
C26 C25 P1 120.2(4) . . ?
C27 C26 C25 119.8(6) . . ?
C28 C27 C26 121.1(6) . . ?
C27 C28 C29 119.9(6) . . ?
C28 C29 C30 119.6(6) . . ?
C29 C30 C25 121.1(5) . . ?
C36 C31 C32 117.9(6) . . ?
C36 C31 P1 119.8(4) . . ?
C32 C31 P1 122.1(4) . . ?
C33 C32 C31 120.4(6) . . ?
C34 C33 C32 119.8(7) . . ?
C35 C34 C33 120.7(7) . . ?
C34 C35 C36 120.3(7) . . ?
C31 C36 C35 121.0(6) . . ?
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 1.826(6) . ?
Os C2 2.041(5) . ?
Os C13 2.098(5) . ?
Os N1 2.151(4) . ?
Os N2 2.170(4) . ?
Os P1 2.3691(14) . ?
P1 C31 1.829(6) . ?
P1 C25 1.832(5) . ?
P1 C24 1.832(6) . ?
O1 C1 1.166(6) . ?
N1 C12 1.349(7) . ?
N1 C8 1.363(6) . ?
N2 C23 1.330(7) . ?
N2 C19 1.369(7) . ?
C2 C3 1.398(7) . ?
C2 C7 1.423(7) . ?
C3 C4 1.352(7) . ?
C4 F1 1.359(6) . ?
C4 C5 1.365(8) . ?
C5 C6 1.370(8) . ?
C6 F2 1.358(6) . ?
C6 C7 1.390(7) . ?
C7 C8 1.455(7) . ?
C8 C9 1.395(7) . ?
C9 C10 1.373(8) . ?
C10 C11 1.358(9) . ?
C11 C12 1.378(8) . ?
C13 C14 1.398(7) . ?
C13 C18 1.405(7) . ?
C14 C15 1.374(8) . ?
C15 C16 1.366(9) . ?
C15 F3 1.367(7) . ?
C16 C17 1.354(8) . ?
C17 F4 1.357(7) . ?
C17 C18 1.385(8) . ?
C18 C19 1.465(7) . ?
C19 C20 1.391(7) . ?
C20 C21 1.383(9) . ?
C21 C22 1.374(9) . ?
C22 C23 1.377(8) . ?
C25 C30 1.384(7) . ?
C25 C26 1.391(7) . ?
C26 C27 1.378(8) . ?
C27 C28 1.364(8) . ?
C28 C29 1.371(8) . ?
C29 C30 1.382(7) . ?
C31 C36 1.378(8) . ?
C31 C32 1.394(8) . ?
C32 C33 1.388(8) . ?
C33 C34 1.364(10) . ?
C34 C35 1.347(10) . ?
C35 C36 1.382(9) . ?
