#------------------------------------------------------------------------------
#$Date: 2016-03-23 23:40:49 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179511 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/08/4340880.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_4340880
loop_
_publ_author_name
'Liao, Jia-Ling'
'Chi, Yun'
'Liu, Shih-Hung'
'Lee, Gene-Hsiang'
'Chou, Pi-Tai'
'Huang, Hao-Xiang'
'Su, Yu-De'
'Chang, Chih-Hao'
'Lin, Jin-Sheng'
'Tseng, Meu-Rurng'
_publ_section_title
;
 Os(II) Phosphors with Near-Infrared Emission Induced by Ligand-to-Ligand
 Charge Transfer Transition.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9366
_journal_page_last               9374
_journal_paper_doi               10.1021/ic501474r
_journal_volume                  53
_journal_year                    2014
_chemical_formula_sum            'C21 H14 F6 N8 O3 Os'
_chemical_formula_weight         730.60
_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                 97.8898(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.3471(6)
_cell_length_b                   17.0368(9)
_cell_length_c                   12.9426(7)
_cell_measurement_reflns_used    3004
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      21.80
_cell_measurement_theta_min      2.24
_cell_volume                     2478.4(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      200(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  0.0593
_diffrn_reflns_av_sigmaI/netI    0.0560
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18957
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    5.231
_exptl_absorpt_correction_T_max  0.5969
_exptl_absorpt_correction_T_min  0.3546
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.958
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.453
_refine_diff_density_min         -0.966
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         5695
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0389
_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)+(0.0309P)²+3.2940P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0784
_refine_ls_wR_factor_ref         0.0847
_reflns_number_gt                4493
_reflns_number_total             5695
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic501474r_si_001.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4340879--4340881.cif.

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_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4340880
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 0.036892(19) 0.627400(12) 0.355564(15) 0.02076(7) Uani 1 1 d . . .
N1 N -0.0550(4) 0.7280(3) 0.2979(3) 0.0227(10) Uani 1 1 d . . .
N2 N 0.1673(4) 0.7154(3) 0.3874(3) 0.0234(10) Uani 1 1 d . . .
N3 N 0.0805(5) 0.6399(3) 0.1150(4) 0.0318(12) Uani 1 1 d . A .
N4 N 0.1033(4) 0.6097(2) 0.2133(3) 0.0220(10) Uani 1 1 d . A .
N5 N 0.2207(5) 0.5440(3) 0.1199(4) 0.0341(12) Uani 1 1 d . A .
N6 N 0.1648(4) 0.5403(3) 0.3891(3) 0.0238(10) Uani 1 1 d . . .
N7 N 0.2113(4) 0.5034(3) 0.4782(4) 0.0282(11) Uani 1 1 d . . .
N8 N 0.3077(5) 0.4651(3) 0.3436(4) 0.0325(12) Uani 1 1 d . . .
C1 C -0.0867(6) 0.5557(3) 0.3161(4) 0.0289(13) Uani 1 1 d . . .
C2 C -0.0039(5) 0.6318(3) 0.4925(5) 0.0290(13) Uani 1 1 d . . .
C3 C -0.1691(5) 0.7307(4) 0.2529(4) 0.0316(14) Uani 1 1 d . . .
H3 H -0.2161 0.6845 0.2528 0.038 Uiso 1 1 calc R . .
C4 C -0.2202(6) 0.7972(4) 0.2072(5) 0.0376(15) Uani 1 1 d . . .
H4 H -0.3019 0.7978 0.1786 0.045 Uiso 1 1 calc R . .
C5 C -0.1507(6) 0.8638(4) 0.2034(5) 0.0374(15) Uani 1 1 d . . .
H5 H -0.1831 0.9101 0.1697 0.045 Uiso 1 1 calc R . .
C6 C -0.0348(6) 0.8617(3) 0.2491(5) 0.0346(14) Uani 1 1 d . . .
H6 H 0.0141 0.9068 0.2475 0.041 Uiso 1 1 calc R . .
C7 C 0.0116(5) 0.7933(3) 0.2980(4) 0.0267(13) Uani 1 1 d . . .
C8 C 0.1333(5) 0.7881(3) 0.3525(4) 0.0263(13) Uani 1 1 d . . .
C9 C 0.2079(6) 0.8518(3) 0.3738(5) 0.0329(14) Uani 1 1 d . . .
H9 H 0.1832 0.9024 0.3485 0.039 Uiso 1 1 calc R . .
C10 C 0.3182(6) 0.8422(4) 0.4318(5) 0.0378(15) Uani 1 1 d . . .
H10 H 0.3695 0.8859 0.4478 0.045 Uiso 1 1 calc R . .
C11 C 0.3532(6) 0.7675(4) 0.4665(5) 0.0356(15) Uani 1 1 d . . .
H11 H 0.4288 0.7592 0.5065 0.043 Uiso 1 1 calc R . .
C12 C 0.2759(5) 0.7055(3) 0.4417(4) 0.0293(13) Uani 1 1 d . . .
H12 H 0.3004 0.6541 0.4638 0.035 Uiso 1 1 calc R . .
C13 C 0.1513(11) 0.6055(7) -0.0520(8) 0.053(3) Uani 0.768(7) 1 d PD A 1
F1 F 0.1148(10) 0.6737(8) -0.0912(12) 0.079(3) Uani 0.768(7) 1 d PD A 1
F2 F 0.0766(8) 0.5526(5) -0.1061(5) 0.090(3) Uani 0.768(7) 1 d PD A 1
F3 F 0.2559(6) 0.5887(5) -0.0789(5) 0.076(3) Uani 0.768(7) 1 d PD A 1
C13' C 0.184(3) 0.626(2) -0.036(3) 0.053(3) Uani 0.232(7) 1 d PD A 2
F1' F 0.093(4) 0.667(3) -0.080(5) 0.079(3) Uani 0.232(7) 1 d PD A 2
F2' F 0.190(3) 0.5623(17) -0.0979(19) 0.090(3) Uani 0.232(7) 1 d PD A 2
F3' F 0.2839(19) 0.6611(15) -0.0438(14) 0.076(3) Uani 0.232(7) 1 d PD A 2
C14 C 0.1530(6) 0.5983(4) 0.0638(5) 0.0352(15) Uani 1 1 d . . .
C15 C 0.1865(5) 0.5541(3) 0.2118(4) 0.0249(12) Uani 1 1 d . . .
C16 C 0.2227(5) 0.5169(3) 0.3117(4) 0.0242(12) Uani 1 1 d . A .
C17 C 0.2942(6) 0.4591(4) 0.4444(5) 0.0336(14) Uani 1 1 d . B .
O1 O -0.1632(4) 0.5138(3) 0.2882(4) 0.0464(12) Uani 1 1 d . . .
O2 O -0.0237(4) 0.6288(3) 0.5760(3) 0.0471(12) Uani 1 1 d . . .
C18 C 0.3678(7) 0.4070(5) 0.5170(6) 0.054(2) Uani 1 1 d . . .
F4 F 0.3112(11) 0.3494(6) 0.5536(10) 0.092(4) Uani 0.579(6) 1 d PU B 1
F5 F 0.4650(12) 0.3856(7) 0.4866(8) 0.083(3) Uani 0.579(6) 1 d P B 1
F6 F 0.4112(10) 0.4479(6) 0.6091(7) 0.091(3) Uani 0.579(6) 1 d P B 1
F4' F 0.3307(16) 0.3913(9) 0.6011(14) 0.092(4) Uani 0.421(6) 1 d P B 2
F5' F 0.3680(13) 0.3312(8) 0.4681(10) 0.083(3) Uani 0.421(6) 1 d P B 2
F6' F 0.4817(18) 0.4197(9) 0.5264(13) 0.091(3) Uani 0.421(6) 1 d P B 2
O3 O 0.4406(8) 0.3021(4) 0.9302(6) 0.107(3) Uani 1 1 d . . .
C19 C 0.4871(8) 0.3449(5) 0.8716(7) 0.058(2) Uani 1 1 d . . .
C20 C 0.5576(9) 0.3096(6) 0.7951(7) 0.082(3) Uani 1 1 d . . .
H20A H 0.6424 0.3186 0.8178 0.123 Uiso 1 1 calc R . .
H20B H 0.5347 0.3337 0.7265 0.123 Uiso 1 1 calc R . .
H20C H 0.5422 0.2530 0.7903 0.123 Uiso 1 1 calc R . .
C21 C 0.4668(9) 0.4298(5) 0.8744(8) 0.083(3) Uani 1 1 d . . .
H21A H 0.4298 0.4430 0.9363 0.125 Uiso 1 1 calc R . .
H21B H 0.4141 0.4458 0.8115 0.125 Uiso 1 1 calc R . .
H21C H 0.5430 0.4574 0.8773 0.125 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
C1 Os C2 90.6(2)
C1 Os N6 93.8(2)
C2 Os N6 94.9(2)
C1 Os N1 96.8(2)
C2 Os N1 97.3(2)
N6 Os N1 163.62(18)
C1 Os N4 90.7(2)
C2 Os N4 170.9(2)
N6 Os N4 75.96(17)
N1 Os N4 91.47(16)
C1 Os N2 174.1(2)
C2 Os N2 92.5(2)
N6 Os N2 90.90(17)
N1 Os N2 77.79(18)
N4 Os N2 86.95(17)
C7 N1 C3 118.7(5)
C7 N1 Os 115.2(4)
C3 N1 Os 125.8(4)
C12 N2 C8 119.3(5)
C12 N2 Os 125.6(4)
C8 N2 Os 115.1(4)
C14 N3 N4 102.4(4)
C15 N4 N3 107.3(4)
C15 N4 Os 116.8(3)
N3 N4 Os 135.9(4)
C15 N5 C14 100.5(5)
C16 N6 N7 109.0(4)
C16 N6 Os 117.3(4)
N7 N6 Os 133.5(4)
C17 N7 N6 101.3(5)
C16 N8 C17 100.3(5)
O1 C1 Os 177.0(5)
O2 C2 Os 174.4(6)
N1 C3 C4 122.7(6)
C3 C4 C5 118.9(6)
C6 C5 C4 118.8(6)
C5 C6 C7 120.0(6)
N1 C7 C6 120.9(6)
N1 C7 C8 116.4(5)
C6 C7 C8 122.7(5)
N2 C8 C9 120.8(5)
N2 C8 C7 114.9(5)
C9 C8 C7 124.1(5)
C10 C9 C8 120.1(6)
C9 C10 C11 118.9(6)
C12 C11 C10 118.7(6)
N2 C12 C11 122.2(5)
F3 C13 F1 109.9(11)
F3 C13 F2 104.0(8)
F1 C13 F2 104.2(11)
F3 C13 C14 111.0(9)
F1 C13 C14 114.7(10)
F2 C13 C14 112.4(10)
F3' C13' F1' 112(3)
F3' C13' F2' 101(2)
F1' C13' F2' 106(3)
F3' C13' C14 122(3)
F1' C13' C14 107(3)
F2' C13' C14 107(3)
N3 C14 N5 116.2(5)
N3 C14 C13' 120.3(16)
N5 C14 C13' 120.9(15)
N3 C14 C13 122.1(6)
N5 C14 C13 121.5(6)
C13' C14 C13 20.6(12)
N5 C15 N4 113.7(5)
N5 C15 C16 132.1(5)
N4 C15 C16 114.2(5)
N8 C16 N6 112.1(5)
N8 C16 C15 132.2(5)
N6 C16 C15 115.6(5)
N7 C17 N8 117.3(5)
N7 C17 C18 120.0(6)
N8 C17 C18 122.7(6)
F4' C18 F5 128.2(10)
F4' C18 F4 43.7(9)
F5 C18 F4 112.9(10)
F4' C18 F6' 113.9(13)
F5 C18 F6' 35.4(7)
F4 C18 F6' 128.9(10)
F4' C18 F6 59.3(9)
F5 C18 F6 100.8(10)
F4 C18 F6 101.4(9)
F6' C18 F6 67.2(10)
F4' C18 F5' 102.2(11)
F5 C18 F5' 63.5(8)
F4 C18 F5' 60.8(9)
F6' C18 F5' 97.4(10)
F6 C18 F5' 142.6(8)
F4' C18 C17 117.2(10)
F5 C18 C17 114.6(7)
F4 C18 C17 115.1(8)
F6' C18 C17 115.5(9)
F6 C18 C17 110.1(7)
F5' C18 C17 107.2(8)
O3 C19 C21 119.4(8)
O3 C19 C20 119.4(8)
C21 C19 C20 121.2(8)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Os C1 1.877(6)
Os C2 1.894(6)
Os N6 2.079(4)
Os N1 2.090(4)
Os N4 2.105(4)
Os N2 2.107(5)
N1 C7 1.344(7)
N1 C3 1.346(7)
N2 C12 1.343(7)
N2 C8 1.356(7)
N3 C14 1.329(7)
N3 N4 1.363(6)
N4 C15 1.341(7)
N5 C15 1.312(7)
N5 C14 1.349(7)
N6 C16 1.332(7)
N6 N7 1.355(6)
N7 C17 1.326(7)
N8 C16 1.330(7)
N8 C17 1.339(8)
C1 O1 1.143(7)
C2 O2 1.135(7)
C3 C4 1.371(8)
C4 C5 1.386(9)
C5 C6 1.366(9)
C6 C7 1.395(8)
C7 C8 1.464(8)
C8 C9 1.382(8)
C9 C10 1.378(9)
C10 C11 1.389(9)
C11 C12 1.383(8)
C13 F3 1.313(12)
C13 F1 1.313(12)
C13 F2 1.364(13)
C13 C14 1.501(12)
C13' F3' 1.30(2)
C13' F1' 1.30(2)
C13' F2' 1.36(2)
C13' C14 1.46(4)
C15 C16 1.448(7)
C17 C18 1.467(9)
C18 F4' 1.248(18)
C18 F5 1.274(13)
C18 F4 1.298(13)
C18 F6' 1.30(2)
C18 F6 1.409(12)
C18 F5' 1.439(16)
O3 C19 1.223(9)
C19 C21 1.466(11)
C19 C20 1.483(12)
