#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:58:48 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179402 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/99/4329992.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_4329992
loop_
_publ_author_name
'Lai-Hon Chung'
'Siu-Chung Chan'
'Wing-Chun Lee'
'Chun-Yuen Wong'
_publ_section_title
;
 Emissive Osmium(II) Complexes Supported by N-Heterocyclic Carbene-based
 CCC-Pincer Ligands and Aromatic Diimines
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8693
_journal_page_last               8703
_journal_paper_doi               10.1021/ic202726g
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C28 H23 Cl2 F6 N6 O Os P'
_chemical_formula_weight         865.59
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.6127(4)
_cell_length_b                   14.5454(6)
_cell_length_c                   17.8962(9)
_cell_measurement_reflns_used    7700
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      71.5105
_cell_measurement_theta_min      3.0356
_cell_volume                     3022.9(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_sigmaI/netI    0.0278
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11832
_diffrn_reflns_theta_full        67.48
_diffrn_reflns_theta_max         67.48
_diffrn_reflns_theta_min         3.92
_exptl_absorpt_coefficient_mu    10.748
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.15856
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro, Agilent Technologies,Version 1.171.35.11'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.902
_exptl_crystal_description       block
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.298
_refine_diff_density_min         -1.029
_refine_diff_density_rms         0.124
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.016(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         5057
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0330
_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)+(0.0753P)²+7.3266P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0989
_refine_ls_wR_factor_ref         0.1127
_reflns_number_gt                4939
_reflns_number_total             5057
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202726g_si_002_2.cif
_cod_data_source_block           Complex_1b
_cod_database_code               4329992
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
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
C1 C 0.5996(6) -0.0898(5) 0.5288(4) 0.0268(15) Uani 1 1 d .
C2 C 0.4367(7) -0.1390(6) 0.5862(5) 0.0342(18) Uani 1 1 d .
H2 H 0.3595 -0.1442 0.5993 0.041 Uiso 1 1 calc R
C3 C 0.5263(7) -0.1867(6) 0.6148(5) 0.0353(19) Uani 1 1 d .
H3 H 0.5215 -0.2321 0.6513 0.042 Uiso 1 1 calc R
C4 C 0.8085(6) -0.1405(4) 0.5341(4) 0.0245(15) Uani 1 1 d .
C5 C 0.7418(8) -0.1857(4) 0.5849(4) 0.0284(15) Uani 1 1 d .
C6 C 0.7867(7) -0.2504(5) 0.6353(5) 0.0335(18) Uani 1 1 d .
H6 H 0.7394 -0.2816 0.6687 0.040 Uiso 1 1 calc R
C7 C 0.9053(8) -0.2661(5) 0.6332(4) 0.0328(19) Uani 1 1 d .
H7 H 0.9375 -0.3086 0.6659 0.039 Uiso 1 1 calc R
C8 C 0.9766(7) -0.2198(5) 0.5832(5) 0.0315(17) Uani 1 1 d .
H8 H 1.0555 -0.2307 0.5824 0.038 Uiso 1 1 calc R
C9 C 0.9274(6) -0.1575(5) 0.5352(4) 0.0265(15) Uani 1 1 d .
C10 C 0.9177(6) -0.0397(5) 0.4417(4) 0.0235(14) Uani 1 1 d .
C11 C 1.0981(7) -0.1005(5) 0.4577(5) 0.0316(18) Uani 1 1 d .
H11 H 1.1587 -0.1359 0.4758 0.038 Uiso 1 1 calc R
C12 C 1.1019(7) -0.0372(6) 0.4018(5) 0.0363(18) Uani 1 1 d .
H12 H 1.1667 -0.0205 0.3744 0.044 Uiso 1 1 calc R
C13 C 0.4163(7) -0.0228(6) 0.4829(5) 0.039(2) Uani 1 1 d .
H13A H 0.4610 0.0296 0.4680 0.058 Uiso 1 1 calc R
H13B H 0.3480 -0.0025 0.5082 0.058 Uiso 1 1 calc R
H13C H 0.3952 -0.0577 0.4395 0.058 Uiso 1 1 calc R
C14 C 0.9619(8) 0.0682(6) 0.3376(6) 0.043(2) Uani 1 1 d .
H14A H 0.8796 0.0727 0.3342 0.064 Uiso 1 1 calc R
H14B H 0.9927 0.0512 0.2897 0.064 Uiso 1 1 calc R
H14C H 0.9932 0.1265 0.3525 0.064 Uiso 1 1 calc R
C15 C 0.6311(7) 0.0908(6) 0.3493(5) 0.0337(18) Uani 1 1 d .
H15 H 0.6215 0.0387 0.3198 0.040 Uiso 1 1 calc R
C16 C 0.5938(8) 0.1752(7) 0.3211(6) 0.047(2) Uani 1 1 d .
H16 H 0.5600 0.1781 0.2741 0.056 Uiso 1 1 calc R
C17 C 0.6068(8) 0.2535(7) 0.3623(7) 0.052(3) Uani 1 1 d .
H17 H 0.5847 0.3101 0.3429 0.062 Uiso 1 1 calc R
C18 C 0.6539(7) 0.2473(6) 0.4342(5) 0.0348(19) Uani 1 1 d .
C19 C 0.6892(6) 0.1595(5) 0.4587(5) 0.0324(18) Uani 1 1 d .
C20 C 0.7416(6) 0.1484(4) 0.5309(4) 0.0244(13) Uani 1 1 d .
C21 C 0.7582(7) 0.2259(5) 0.5777(5) 0.0376(18) Uani 1 1 d .
C22 C 0.8079(7) 0.2108(6) 0.6479(5) 0.041(2) Uani 1 1 d .
H22 H 0.8173 0.2594 0.6811 0.049 Uiso 1 1 calc R
C23 C 0.8424(8) 0.1249(7) 0.6670(5) 0.043(2) Uani 1 1 d .
H23 H 0.8775 0.1141 0.7129 0.052 Uiso 1 1 calc R
C24 C 0.8242(7) 0.0519(6) 0.6162(5) 0.0367(19) Uani 1 1 d .
H24 H 0.8491 -0.0066 0.6296 0.044 Uiso 1 1 calc R
C25 C 0.7194(8) 0.3140(5) 0.5507(6) 0.048(2) Uani 1 1 d .
H25 H 0.7289 0.3656 0.5808 0.057 Uiso 1 1 calc R
C26 C 0.6700(8) 0.3237(6) 0.4834(6) 0.050(2) Uani 1 1 d .
H26 H 0.6456 0.3816 0.4683 0.060 Uiso 1 1 calc R
C27 C 0.7154(7) -0.1200(5) 0.3899(4) 0.0311(17) Uani 1 1 d .
C28 C 0.944(2) 0.3756(16) 0.3399(10) 0.187(14) Uani 1 1 d .
H28A H 0.9549 0.4388 0.3558 0.225 Uiso 1 1 calc R
H28B H 0.8670 0.3707 0.3196 0.225 Uiso 1 1 calc R
Cl1 Cl 0.9532(2) 0.3056(2) 0.4177(2) 0.0749(9) Uani 1 1 d .
Cl2 Cl 1.0416(4) 0.3527(2) 0.26892(19) 0.0840(10) Uani 1 1 d .
F1 F 0.6510(7) 0.6328(4) 0.2935(4) 0.074(2) Uani 1 1 d .
F2 F 0.6532(5) 0.5472(4) 0.1883(3) 0.0518(13) Uani 1 1 d .
F3 F 0.6944(6) 0.5093(4) 0.3625(3) 0.0603(16) Uani 1 1 d .
F4 F 0.8062(5) 0.5476(6) 0.2647(3) 0.0682(19) Uani 1 1 d .
F5 F 0.6957(8) 0.4234(4) 0.2574(4) 0.078(2) Uani 1 1 d .
F6 F 0.5415(6) 0.5069(6) 0.2862(4) 0.083(3) Uani 1 1 d .
N1 N 0.4843(5) -0.0803(5) 0.5330(4) 0.0333(14) Uani 1 1 d .
N2 N 0.6245(6) -0.1572(4) 0.5814(4) 0.0299(14) Uani 1 1 d .
N3 N 0.9842(5) -0.1012(4) 0.4821(4) 0.0283(14) Uani 1 1 d .
N4 N 0.9929(6) -0.0023(4) 0.3933(4) 0.0330(15) Uani 1 1 d .
N5 N 0.6798(5) 0.0812(4) 0.4164(4) 0.0275(14) Uani 1 1 d .
N6 N 0.7734(5) 0.0627(4) 0.5505(3) 0.0260(13) Uani 1 1 d .
O1 O 0.6996(6) -0.1667(4) 0.3382(3) 0.0480(17) Uani 1 1 d .
Os1 Os 0.74260(2) -0.041523(18) 0.468295(15) 0.02290(12) Uani 1 1 d .
P3 P 0.67326(18) 0.52851(17) 0.27605(12) 0.0313(4) 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 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Os Os -4.9801 6.2216 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 '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
N1 C1 N2 103.9(7)
N1 C1 Os1 141.2(6)
N2 C1 Os1 114.8(5)
C3 C2 N1 105.6(7)
C2 C3 N2 108.5(7)
C5 C4 C9 117.7(7)
C5 C4 Os1 121.3(6)
C9 C4 Os1 120.6(5)
C4 C5 C6 122.7(8)
C4 C5 N2 111.9(6)
C6 C5 N2 125.3(7)
C7 C6 C5 117.3(8)
C8 C7 C6 121.6(7)
C9 C8 C7 118.3(7)
C8 C9 C4 122.3(8)
C8 C9 N3 127.4(7)
C4 C9 N3 110.3(6)
N4 C10 N3 103.6(6)
N4 C10 Os1 141.7(6)
N3 C10 Os1 114.6(5)
C12 C11 N3 105.5(7)
C11 C12 N4 107.6(7)
N5 C15 C16 123.2(8)
C17 C16 C15 120.3(9)
C16 C17 C18 119.1(9)
C17 C18 C19 117.2(9)
C17 C18 C26 124.5(8)
C19 C18 C26 118.3(8)
N5 C19 C18 123.8(8)
N5 C19 C20 115.9(6)
C18 C19 C20 120.2(8)
N6 C20 C21 123.1(7)
N6 C20 C19 116.9(6)
C21 C20 C19 119.9(6)
C22 C21 C20 117.4(7)
C22 C21 C25 124.6(8)
C20 C21 C25 117.9(8)
C23 C22 C21 119.5(8)
C22 C23 C24 119.0(9)
N6 C24 C23 123.3(8)
C26 C25 C21 121.8(8)
C25 C26 C18 121.9(8)
O1 C27 Os1 177.2(7)
Cl1 C28 Cl2 115.9(9)
C1 N1 C2 111.7(7)
C1 N1 C13 124.2(7)
C2 N1 C13 123.8(7)
C3 N2 C1 110.3(7)
C3 N2 C5 133.8(7)
C1 N2 C5 115.7(6)
C10 N3 C11 111.1(6)
C10 N3 C9 117.6(6)
C11 N3 C9 131.1(7)
C10 N4 C12 112.2(7)
C10 N4 C14 123.9(7)
C12 N4 C14 123.9(7)
C15 N5 C19 116.3(7)
C15 N5 Os1 128.4(6)
C19 N5 Os1 115.2(5)
C24 N6 C20 117.5(7)
C24 N6 Os1 126.9(5)
C20 N6 Os1 115.5(5)
C27 Os1 C4 93.9(3)
C27 Os1 C10 90.1(3)
C4 Os1 C10 76.8(3)
C27 Os1 C1 92.9(3)
C4 Os1 C1 76.1(3)
C10 Os1 C1 152.9(3)
C27 Os1 N5 97.4(3)
C4 Os1 N5 168.7(3)
C10 Os1 N5 102.8(3)
C1 Os1 N5 103.5(3)
C27 Os1 N6 173.4(3)
C4 Os1 N6 92.3(2)
C10 Os1 N6 89.1(2)
C1 Os1 N6 90.8(3)
N5 Os1 N6 76.4(2)
F1 P3 F6 90.6(5)
F1 P3 F4 90.9(5)
F6 P3 F4 178.4(5)
F1 P3 F5 179.3(4)
F6 P3 F5 89.5(5)
F4 P3 F5 89.0(5)
F1 P3 F3 90.1(4)
F6 P3 F3 90.2(4)
F4 P3 F3 90.3(4)
F5 P3 F3 90.6(4)
F1 P3 F2 90.4(4)
F6 P3 F2 90.3(3)
F4 P3 F2 89.2(3)
F5 P3 F2 88.9(3)
F3 P3 F2 179.3(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 N1 1.349(9)
C1 N2 1.390(10)
C1 Os1 2.103(7)
C2 C3 1.352(12)
C2 N1 1.393(11)
C3 N2 1.357(11)
C4 C5 1.363(11)
C4 C9 1.403(10)
C4 Os1 2.011(7)
C5 C6 1.404(11)
C5 N2 1.425(10)
C6 C7 1.397(12)
C7 C8 1.392(12)
C8 C9 1.373(11)
C9 N3 1.417(10)
C10 N4 1.346(10)
C10 N3 1.387(10)
C10 Os1 2.088(7)
C11 C12 1.361(12)
C11 N3 1.392(10)
C12 N4 1.372(11)
C13 N1 1.459(11)
C14 N4 1.474(11)
C15 N5 1.336(10)
C15 C16 1.396(12)
C16 C17 1.365(15)
C17 C18 1.401(14)
C18 C19 1.412(11)
C18 C26 1.429(14)
C19 N5 1.371(10)
C19 C20 1.438(11)
C20 N6 1.347(9)
C20 C21 1.417(10)
C21 C22 1.400(13)
C21 C25 1.441(12)
C22 C23 1.357(13)
C23 C24 1.414(12)
C24 N6 1.325(11)
C25 C26 1.343(14)
C27 O1 1.162(9)
C27 Os1 1.836(8)
C28 Cl1 1.73(2)
C28 Cl2 1.73(2)
F1 P3 1.571(6)
F2 P3 1.610(6)
F3 P3 1.592(6)
F4 P3 1.582(6)
F5 P3 1.587(6)
F6 P3 1.573(7)
N5 Os1 2.141(6)
N6 Os1 2.142(6)
