#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/36/7023684.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_7023684
loop_
_publ_author_name
'Chaudhuri, Satyabrata'
'Patra, Sarat Chandra'
'Saha, Pinaki'
'Saha Roy, Amit'
'Maity, Suvendu'
'Bera, Sachinath'
'Saha Sardar, Pinki'
'Ghosh, Sanjib'
'Weyhermüller, Thomas'
'Ghosh, Prasanta'
_publ_section_title
;
 Zinc(ii), iron(ii/iii) and ruthenium(ii) complexes of o-phenylenediamine
 derivatives: oxidative dehydrogenation and photoluminescence.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15028
_journal_page_last               15042
_journal_paper_doi               10.1039/c3dt51771c
_journal_volume                  42
_journal_year                    2013
_chemical_compound_source        'dichloromethane, n-hexane'
_chemical_formula_moiety         'C61 H48 N3 O P2 Ru, F6 P'
_chemical_formula_sum            'C61 H48 F6 N3 O P3 Ru'
_chemical_formula_weight         1147.00
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      62
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                WGT-PG-501-24
_audit_creation_date             2011-06-20
_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                   26.0925(12)
_cell_length_b                   14.8744(10)
_cell_length_c                   13.0900(7)
_cell_measurement_reflns_used    180172
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.0
_cell_measurement_theta_min      2.7108
_cell_volume                     5080.4(5)
_computing_cell_refinement       'DENZO (Bruker AXS, 2006)'
_computing_data_collection       'DATCOL (Bruker AXS, 2006)'
_computing_data_reduction        'DENZO (Bruker AXS, 2006)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 18.02
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker AXS Enraf-Nonius KappaCCD'
_diffrn_measurement_method       'CCD φ- and ω-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         '0.2 x 2mm^2^ focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_av_sigmaI/netI    0.0211
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            142738
_diffrn_reflns_theta_full        35.03
_diffrn_reflns_theta_max         35.03
_diffrn_reflns_theta_min         2.81
_exptl_absorpt_coefficient_mu    0.473
_exptl_absorpt_correction_T_max  0.94333
_exptl_absorpt_correction_T_min  0.89165
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2008)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2344
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.759
_refine_diff_density_min         -1.154
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         11532
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0285
_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)+(0.0269P)²+3.5020P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0649
_refine_ls_wR_factor_ref         0.0701
_reflns_number_gt                9495
_reflns_number_total             11532
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt51771c.txt
_cod_data_source_block           5PF6
_cod_original_sg_symbol_Hall     '-p 2ac 2n'
_cod_database_code               7023684
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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
Ru1 Ru 0.143417(4) 0.7500 0.060577(8) 0.00827(3) Uani 1 2 d S
O1 O 0.14893(4) 0.7500 0.21856(8) 0.01278(18) Uani 1 2 d S
C2 C 0.19224(6) 0.7500 0.26823(12) 0.0171(3) Uani 1 2 d S
C3 C 0.18917(8) 0.7500 0.37604(15) 0.0468(7) Uani 1 2 d S
H3 H 0.1564 0.7500 0.4076 0.056 Uiso 1 2 calc SR
C4 C 0.23206(10) 0.7500 0.43637(18) 0.0757(14) Uani 1 2 d S
H4 H 0.2283 0.7500 0.5086 0.091 Uiso 1 2 calc SR
C5 C 0.28123(9) 0.7500 0.39389(17) 0.0519(8) Uani 1 2 d S
H5 H 0.3108 0.7500 0.4363 0.062 Uiso 1 2 calc SR
C6 C 0.28575(7) 0.7500 0.28957(14) 0.0246(3) Uani 1 2 d S
H6 H 0.3190 0.7500 0.2601 0.030 Uiso 1 2 calc SR
C7 C 0.24244(6) 0.7500 0.22411(12) 0.0152(3) Uani 1 2 d S
C8 C 0.25395(6) 0.7500 0.11703(12) 0.0137(2) Uani 1 2 d S
H8 H 0.2890 0.7500 0.0977 0.016 Uiso 1 2 calc SR
N9 N 0.21985(5) 0.7500 0.04408(10) 0.0112(2) Uani 1 2 d S
C10 C 0.23393(5) 0.7500 -0.06123(11) 0.0126(2) Uani 1 2 d S
C11 C 0.28478(6) 0.7500 -0.09502(13) 0.0182(3) Uani 1 2 d S
H11 H 0.3120 0.7500 -0.0468 0.022 Uiso 1 2 calc SR
C12 C 0.29550(6) 0.7500 -0.19826(14) 0.0243(3) Uani 1 2 d S
H12 H 0.3301 0.7500 -0.2207 0.029 Uiso 1 2 calc SR
C13 C 0.25624(7) 0.7500 -0.26927(14) 0.0290(4) Uani 1 2 d S
H13 H 0.2641 0.7500 -0.3401 0.035 Uiso 1 2 calc SR
C14 C 0.20533(6) 0.7500 -0.23776(12) 0.0214(3) Uani 1 2 d S
H14 H 0.1786 0.7500 -0.2870 0.026 Uiso 1 2 calc SR
C15 C 0.19360(5) 0.7500 -0.13370(11) 0.0126(2) Uani 1 2 d S
N16 N 0.14298(5) 0.7500 -0.09036(9) 0.01025(19) Uani 1 2 d S
C17 C 0.09874(5) 0.7500 -0.13810(11) 0.0107(2) Uani 1 2 d S
C18 C 0.05426(5) 0.7500 -0.06985(11) 0.0106(2) Uani 1 2 d S
C19 C 0.00401(5) 0.7500 -0.10646(12) 0.0141(2) Uani 1 2 d S
H19 H -0.0024 0.7500 -0.1779 0.017 Uiso 1 2 calc SR
C20 C -0.03641(6) 0.7500 -0.03790(13) 0.0167(3) Uani 1 2 d S
H20 H -0.0708 0.7500 -0.0617 0.020 Uiso 1 2 calc SR
C21 C -0.02594(6) 0.7500 0.06637(12) 0.0156(3) Uani 1 2 d S
H21 H -0.0530 0.7500 0.1149 0.019 Uiso 1 2 calc SR
C22 C 0.02476(5) 0.7500 0.09819(12) 0.0127(2) Uani 1 2 d S
H22 H 0.0316 0.7500 0.1695 0.015 Uiso 1 2 calc SR
N23 N 0.06479(5) 0.7500 0.03293(9) 0.0103(2) Uani 1 2 d S
C24 C 0.08956(5) 0.7500 -0.25023(11) 0.0125(2) Uani 1 2 d S
C25 C 0.08399(5) 0.66899(8) -0.30198(9) 0.0191(2) Uani 1 1 d .
H25 H 0.0877 0.6137 -0.2665 0.023 Uiso 1 1 calc R
C26 C 0.07296(5) 0.66924(9) -0.40607(10) 0.0240(2) Uani 1 1 d .
H26 H 0.0691 0.6140 -0.4416 0.029 Uiso 1 1 calc R
C27 C 0.06752(6) 0.7500 -0.45800(13) 0.0228(3) Uani 1 2 d S
H27 H 0.0601 0.7500 -0.5290 0.027 Uiso 1 2 calc SR
P30 P 0.144866(10) 0.587734(17) 0.070048(19) 0.01000(5) Uani 1 1 d .
C31 C 0.20976(4) 0.54219(7) 0.07721(8) 0.01312(17) Uani 1 1 d .
C32 C 0.24222(4) 0.54729(7) -0.00780(9) 0.01597(18) Uani 1 1 d .
H32 H 0.2292 0.5688 -0.0710 0.019 Uiso 1 1 calc R
C33 C 0.29330(4) 0.52124(9) -0.00095(11) 0.0231(2) Uani 1 1 d .
H33 H 0.3150 0.5249 -0.0591 0.028 Uiso 1 1 calc R
C34 C 0.31243(5) 0.48992(10) 0.09132(13) 0.0289(3) Uani 1 1 d .
H34 H 0.3473 0.4722 0.0965 0.035 Uiso 1 1 calc R
C35 C 0.28074(5) 0.48453(10) 0.17571(12) 0.0280(3) Uani 1 1 d .
H35 H 0.2940 0.4625 0.2385 0.034 Uiso 1 1 calc R
C36 C 0.22964(4) 0.51101(8) 0.16959(10) 0.0199(2) Uani 1 1 d .
H36 H 0.2083 0.5078 0.2283 0.024 Uiso 1 1 calc R
C41 C 0.11214(4) 0.53391(7) 0.17781(8) 0.01265(17) Uani 1 1 d .
C42 C 0.11047(4) 0.43950(7) 0.18256(9) 0.01742(19) Uani 1 1 d .
H42 H 0.1263 0.4048 0.1305 0.021 Uiso 1 1 calc R
C43 C 0.08579(4) 0.39691(8) 0.26291(10) 0.0198(2) Uani 1 1 d .
H43 H 0.0854 0.3331 0.2661 0.024 Uiso 1 1 calc R
C44 C 0.06154(4) 0.44671(8) 0.33897(9) 0.0192(2) Uani 1 1 d .
H44 H 0.0447 0.4172 0.3939 0.023 Uiso 1 1 calc R
C45 C 0.06220(4) 0.54008(8) 0.33370(9) 0.01758(19) Uani 1 1 d .
H45 H 0.0452 0.5745 0.3845 0.021 Uiso 1 1 calc R
C46 C 0.08785(4) 0.58353(7) 0.25398(8) 0.01474(18) Uani 1 1 d .
H46 H 0.0887 0.6473 0.2517 0.018 Uiso 1 1 calc R
C51 C 0.11398(4) 0.52804(7) -0.03638(8) 0.01202(16) Uani 1 1 d .
C52 C 0.13876(4) 0.46870(8) -0.10269(9) 0.01707(19) Uani 1 1 d .
H52 H 0.1742 0.4562 -0.0935 0.020 Uiso 1 1 calc R
C53 C 0.11197(4) 0.42763(8) -0.18241(9) 0.0193(2) Uani 1 1 d .
H53 H 0.1294 0.3879 -0.2274 0.023 Uiso 1 1 calc R
C54 C 0.06003(4) 0.44437(8) -0.19635(9) 0.01716(19) Uani 1 1 d .
H54 H 0.0420 0.4171 -0.2513 0.021 Uiso 1 1 calc R
C55 C 0.03473(4) 0.50150(7) -0.12908(9) 0.01513(18) Uani 1 1 d .
H55 H -0.0009 0.5125 -0.1374 0.018 Uiso 1 1 calc R
C56 C 0.06130(4) 0.54261(7) -0.04975(8) 0.01296(17) Uani 1 1 d .
H56 H 0.0435 0.5811 -0.0040 0.016 Uiso 1 1 calc R
P60 P 0.075035(15) 0.2500 0.57296(3) 0.01274(7) Uani 1 2 d S
F61 F 0.11851(3) 0.32619(6) 0.57582(7) 0.02972(18) Uani 1 1 d .
F62 F 0.07683(6) 0.2500 0.45097(8) 0.0310(3) Uani 1 2 d S
F63 F 0.03197(3) 0.32669(5) 0.57116(6) 0.02526(16) Uani 1 1 d .
F64 F 0.07352(5) 0.2500 0.69580(8) 0.0268(2) Uani 1 2 d S
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'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 -1.00 0.00 0.0650
0.00 1.00 0.00 0.0650
1.00 0.00 -1.00 0.1400
-1.00 0.00 1.00 0.1000
-1.00 0.00 -1.00 0.1200
1.00 0.00 1.00 0.1400
-1.00 0.00 0.00 0.1300
4.00 0.00 -1.00 0.1400
-4.00 0.00 -1.00 0.1300
1.00 -2.00 -1.00 0.0850
1.00 0.00 0.00 0.1500
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
N16 Ru1 N9 84.15(5) . .
N16 Ru1 O1 176.35(5) . .
N9 Ru1 O1 92.20(5) . .
N16 Ru1 N23 79.67(5) . .
N9 Ru1 N23 163.82(5) . .
O1 Ru1 N23 103.98(4) . .
N16 Ru1 P30 92.945(7) . 7_575
N9 Ru1 P30 89.424(7) . 7_575
O1 Ru1 P30 87.005(7) . 7_575
N23 Ru1 P30 91.394(7) . 7_575
N16 Ru1 P30 92.945(6) . .
N9 Ru1 P30 89.425(7) . .
O1 Ru1 P30 87.004(7) . .
N23 Ru1 P30 91.393(7) . .
P30 Ru1 P30 173.852(13) 7_575 .
C2 O1 Ru1 123.90(10) . .
O1 C2 C3 116.66(16) . .
O1 C2 C7 126.29(14) . .
C3 C2 C7 117.04(15) . .
C4 C3 C2 122.0(2) . .
C3 C4 C5 121.4(2) . .
C6 C5 C4 118.37(19) . .
C5 C6 C7 122.23(18) . .
C6 C7 C2 119.04(15) . .
C6 C7 C8 115.07(14) . .
C2 C7 C8 125.89(13) . .
N9 C8 C7 124.92(14) . .
C8 N9 C10 122.09(13) . .
C8 N9 Ru1 126.80(11) . .
C10 N9 Ru1 111.11(9) . .
C11 C10 C15 119.53(14) . .
C11 C10 N9 123.37(13) . .
C15 C10 N9 117.10(12) . .
C12 C11 C10 120.13(15) . .
C11 C12 C13 120.53(15) . .
C12 C13 C14 120.52(16) . .
C13 C14 C15 119.91(15) . .
C14 C15 C10 119.37(13) . .
C14 C15 N16 125.90(13) . .
C10 C15 N16 114.73(13) . .
C17 N16 C15 128.33(12) . .
C17 N16 Ru1 118.76(10) . .
C15 N16 Ru1 112.91(9) . .
N16 C17 C18 113.99(12) . .
N16 C17 C24 127.69(13) . .
C18 C17 C24 118.32(12) . .
N23 C18 C19 121.61(13) . .
N23 C18 C17 116.05(12) . .
C19 C18 C17 122.34(13) . .
C20 C19 C18 119.52(14) . .
C19 C20 C21 119.08(14) . .
C22 C21 C20 118.80(14) . .
N23 C22 C21 123.24(14) . .
C22 N23 C18 117.74(12) . .
C22 N23 Ru1 130.72(10) . .
C18 N23 Ru1 111.54(9) . .
C25 C24 C25 120.20(14) . 7_575
C25 C24 C17 119.86(7) . .
C25 C24 C17 119.86(7) 7_575 .
C24 C25 C26 119.74(12) . .
C27 C26 C25 120.19(12) . .
C26 C27 C26 119.94(15) 7_575 .
C31 P30 C41 103.32(5) . .
C31 P30 C51 105.44(5) . .
C41 P30 C51 99.67(5) . .
C31 P30 Ru1 112.80(3) . .
C41 P30 Ru1 117.93(3) . .
C51 P30 Ru1 115.89(3) . .
C36 C31 C32 118.81(10) . .
C36 C31 P30 120.83(9) . .
C32 C31 P30 119.99(8) . .
C33 C32 C31 120.87(11) . .
C34 C33 C32 119.63(12) . .
C35 C34 C33 120.01(11) . .
C34 C35 C36 120.68(12) . .
C35 C36 C31 119.99(12) . .
C46 C41 C42 118.90(10) . .
C46 C41 P30 122.10(8) . .
C42 C41 P30 118.99(8) . .
C43 C42 C41 120.28(11) . .
C42 C43 C44 120.68(10) . .
C45 C44 C43 119.34(10) . .
C44 C45 C46 120.31(11) . .
C41 C46 C45 120.47(10) . .
C52 C51 C56 118.28(9) . .
C52 C51 P30 124.98(8) . .
C56 C51 P30 116.73(8) . .
C53 C52 C51 120.61(10) . .
C54 C53 C52 120.51(10) . .
C53 C54 C55 119.29(10) . .
C56 C55 C54 120.33(10) . .
C55 C56 C51 120.93(9) . .
F62 P60 F63 90.34(5) . .
F62 P60 F63 90.34(5) . 7_565
F63 P60 F63 90.85(6) . 7_565
F62 P60 F61 90.15(5) . .
F63 P60 F61 89.62(4) . .
F63 P60 F61 179.33(5) 7_565 .
F62 P60 F61 90.15(5) . 7_565
F63 P60 F61 179.32(5) . 7_565
F63 P60 F61 89.62(4) 7_565 7_565
F61 P60 F61 89.91(7) . 7_565
F62 P60 F64 179.72(8) . .
F63 P60 F64 89.86(5) . .
F63 P60 F64 89.86(5) 7_565 .
F61 P60 F64 89.66(5) . .
F61 P60 F64 89.66(5) 7_565 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru1 N16 1.9758(12) .
Ru1 N9 2.0059(12) .
Ru1 O1 2.0730(11) .
Ru1 N23 2.0833(12) .
Ru1 P30 2.4170(3) 7_575
Ru1 P30 2.4171(3) .
O1 C2 1.3036(18) .
C2 C3 1.413(3) .
C2 C7 1.431(2) .
C3 C4 1.370(3) .
C4 C5 1.398(4) .
C5 C6 1.371(3) .
C6 C7 1.418(2) .
C7 C8 1.434(2) .
C8 N9 1.3053(18) .
N9 C10 1.4267(19) .
C10 C11 1.398(2) .
C10 C15 1.417(2) .
C11 C12 1.380(2) .
C12 C13 1.383(3) .
C13 C14 1.391(2) .
C14 C15 1.396(2) .
C15 N16 1.4375(18) .
N16 C17 1.3126(18) .
C17 C18 1.4645(19) .
C17 C24 1.487(2) .
C18 N23 1.3732(18) .
C18 C19 1.3960(19) .
C19 C20 1.385(2) .
C20 C21 1.392(2) .
C21 C22 1.387(2) .
C22 N23 1.3492(18) .
C24 C25 1.3900(13) .
C24 C25 1.3900(13) 7_575
C25 C26 1.3926(17) .
C26 C27 1.3875(16) .
C27 C26 1.3875(16) 7_575
P30 C31 1.8263(10) .
P30 C41 1.8330(10) .
P30 C51 1.8381(10) .
C31 C36 1.3951(15) .
C31 C32 1.4004(15) .
C32 C33 1.3909(15) .
C33 C34 1.387(2) .
C34 C35 1.382(2) .
C35 C36 1.3927(17) .
C41 C46 1.3931(15) .
C41 C42 1.4063(14) .
C42 C43 1.3865(16) .
C43 C44 1.3929(18) .
C44 C45 1.3907(16) .
C45 C46 1.3980(15) .
C51 C52 1.3967(14) .
C51 C56 1.4025(14) .
C52 C53 1.3966(15) .
C53 C54 1.3899(16) .
C54 C55 1.3905(16) .
C55 C56 1.3902(15) .
P60 F62 1.5976(12) .
P60 F63 1.6013(8) .
P60 F63 1.6013(8) 7_565
P60 F61 1.6039(8) .
P60 F61 1.6040(8) 7_565
P60 F64 1.6084(11) .
