#------------------------------------------------------------------------------
#$Date: 2019-11-08 01:23:21 +0200 (Fri, 08 Nov 2019) $
#$Revision: 224489 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/05/7700578.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_7700578
loop_
_publ_author_name
'Kotani, Hiroaki'
'Shimomura, Hinatsu'
'Horimoto, Momoka'
'Ishizuka, Tomoya'
'Shiota, Yoshihito'
'Yoshizawa, Kazunari'
'Yanagisawa, Sachiko'
'Kawahara-Nakagawa, Yuka'
'Kubo, Minoru'
'Kojima, Takahiko'
_publ_section_title
;
 Fundamental electron-transfer and proton-coupled electron-transfer
 properties of Ru(iv)-oxo complexes.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13154
_journal_page_last               13161
_journal_paper_doi               10.1039/c9dt02734c
_journal_volume                  48
_journal_year                    2019
_chemical_formula_sum            'C23 H25 F12 N5 O P2 Ru'
_chemical_formula_weight         778.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2019-07-03 deposited with the CCDC.    2019-07-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.214(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.0227(16)
_cell_length_b                   17.867(4)
_cell_length_c                   10.601(2)
_cell_measurement_reflns_used    6554
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.33
_cell_volume                     1434.9(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoKa
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0135
_diffrn_reflns_av_unetI/netI     0.0159
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.906
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8273
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.906
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.644
_diffrn_reflns_theta_min         2.034
_exptl_absorpt_coefficient_mu    0.765
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.802
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.560
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.720
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         3452
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0234
_refine_ls_R_factor_gt           0.0223
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[?s²(Fo²)+(0.0281P)²+0.9532P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0571
_refine_ls_wR_factor_ref         0.0578
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3302
_reflns_number_total             3452
_reflns_threshold_expression     'I > 2?s(I)'
_cod_data_source_file            c9dt02734c2.cif
_cod_data_source_block           Momoka2
_cod_depositor_comments
'Adding full bibliography for 7700578--7700580.cif.'
_cod_database_code               7700578
_shelx_shelxl_version_number     2017/1
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.674
_shelx_estimated_absorpt_t_max   0.921
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.44538(2) 0.250000 0.37548(2) 0.01610(6) Uani 1 2 d S T P . .
P1 P 0.48254(6) 0.41649(3) 0.79256(4) 0.02917(11) Uani 1 1 d D . . . .
F1 F 0.5667(17) 0.4286(8) 0.9485(10) 0.0448(18) Uani 0.636(15) 1 d . . P A 1
F2 F 0.6168(9) 0.3559(4) 0.7973(8) 0.101(3) Uani 0.636(15) 1 d . . P A 1
F3 F 0.3384(6) 0.3609(4) 0.8066(6) 0.0583(13) Uani 0.636(15) 1 d . . P A 1
F4 F 0.3490(7) 0.4864(2) 0.7810(4) 0.0450(9) Uani 0.636(15) 1 d D . P A 1
F5 F 0.6170(4) 0.4790(2) 0.7641(5) 0.0401(9) Uani 0.636(15) 1 d D . P A 1
F6 F 0.381(3) 0.4069(13) 0.6316(11) 0.042(3) Uani 0.636(15) 1 d . . P A 1
F7 F 0.576(3) 0.4122(14) 0.9506(15) 0.047(4) Uani 0.364(15) 1 d D . P A 2
F8 F 0.6162(9) 0.3485(3) 0.7725(9) 0.0362(15) Uani 0.364(15) 1 d D . P A 2
F9 F 0.378(2) 0.3404(11) 0.8123(10) 0.108(5) Uani 0.364(15) 1 d D . P A 2
F10 F 0.3311(14) 0.4603(13) 0.8117(14) 0.123(6) Uani 0.364(15) 1 d . . P A 2
F11 F 0.5979(16) 0.4740(6) 0.7852(11) 0.117(5) Uani 0.364(15) 1 d D . P A 2
F12 F 0.409(5) 0.408(2) 0.6337(18) 0.034(3) Uani 0.364(15) 1 d D . P A 2
O1 O 0.3809(2) 0.250000 0.55852(17) 0.0268(3) Uani 1 2 d DS T P . .
H13 H 0.408(3) 0.2892(9) 0.606(2) 0.061(8) Uiso 1 1 d D . . . .
N1 N 0.4767(3) 0.250000 0.1873(2) 0.0270(4) Uani 1 2 d S T P . .
N2 N 0.25123(16) 0.17305(7) 0.28391(13) 0.0215(3) Uani 1 1 d . . . . .
N3 N 0.64739(16) 0.32325(7) 0.46593(13) 0.0201(2) Uani 1 1 d . . . . .
C1 C 0.3917(3) 0.18049(12) 0.11647(19) 0.0418(5) Uani 1 1 d . . . . .
H1 H 0.480802 0.139994 0.135162 0.050 Uiso 1 1 calc R U . . .
H2 H 0.349869 0.189788 0.018983 0.050 Uiso 1 1 calc R U . . .
C2 C 0.2392(2) 0.15527(10) 0.15783(17) 0.0310(4) Uani 1 1 d . . . . .
C3 C 0.1011(3) 0.11158(12) 0.0773(2) 0.0459(5) Uani 1 1 d . . . . .
H3 H 0.093438 0.100706 -0.012144 0.055 Uiso 1 1 calc R U . . .
C4 C -0.0240(3) 0.08430(12) 0.1282(3) 0.0504(6) Uani 1 1 d . . . . .
H4 H -0.118154 0.053979 0.074840 0.060 Uiso 1 1 calc R U . . .
C5 C -0.0104(2) 0.10170(10) 0.2576(2) 0.0408(5) Uani 1 1 d . . . . .
H5 H -0.094506 0.082913 0.295149 0.049 Uiso 1 1 calc R U . . .
C6 C 0.1263(2) 0.14664(9) 0.33255(19) 0.0290(4) Uani 1 1 d . . . . .
H6 H 0.132875 0.159460 0.421038 0.035 Uiso 1 1 calc R U . . .
C7 C 0.6620(4) 0.250000 0.1860(3) 0.0485(8) Uani 1 2 d DS T P . .
H7 H 0.662(4) 0.250000 0.0964(12) 0.045(9) Uiso 1 2 d DS . P . .
C8 C 0.6389(2) 0.39871(9) 0.45949(16) 0.0244(3) Uani 1 1 d . . . . .
H9 H 0.532967 0.421504 0.404349 0.029 Uiso 1 1 calc R U . . .
C9 C 0.7782(2) 0.44430(9) 0.52999(18) 0.0297(3) Uani 1 1 d . . . . .
H10 H 0.767464 0.497221 0.523139 0.036 Uiso 1 1 calc R U . . .
C10 C 0.9331(2) 0.41175(10) 0.61039(19) 0.0312(4) Uani 1 1 d . . . . .
H11 H 1.030062 0.441931 0.659893 0.037 Uiso 1 1 calc R U . . .
C11 C 0.9447(2) 0.33424(10) 0.61761(17) 0.0274(3) Uani 1 1 d . . . . .
H12 H 1.050179 0.310758 0.671813 0.033 Uiso 1 1 calc R U . . .
C12 C 0.80052(19) 0.29123(8) 0.54483(15) 0.0213(3) Uani 1 1 d . . . . .
H8 H 0.721(3) 0.2931(9) 0.232(2) 0.058(8) Uiso 1 1 d 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'
Ru Ru -1.2594 0.8363 '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
N3 Ru1 N3 78.97(7) 4_565 .
N3 Ru1 N2 98.75(5) 4_565 .
N3 Ru1 N2 177.37(5) . .
N3 Ru1 N2 177.37(5) 4_565 4_565
N3 Ru1 N2 98.75(5) . 4_565
N2 Ru1 N2 83.49(7) . 4_565
N3 Ru1 N1 96.95(6) 4_565 .
N3 Ru1 N1 96.95(6) . .
N2 Ru1 N1 81.98(6) . .
N2 Ru1 N1 81.98(6) 4_565 .
N3 Ru1 O1 88.07(5) 4_565 .
N3 Ru1 O1 88.06(5) . .
N2 Ru1 O1 93.19(5) . .
N2 Ru1 O1 93.19(5) 4_565 .
N1 Ru1 O1 173.49(7) . .
F11 P1 F10 101.7(9) . .
F2 P1 F3 94.8(4) . .
F2 P1 F1 90.5(6) . .
F3 P1 F1 93.6(5) . .
F11 P1 F7 90.2(9) . .
F10 P1 F7 90.2(9) . .
F11 P1 F12 92.0(13) . .
F10 P1 F12 99.2(15) . .
F7 P1 F12 169.7(17) . .
F2 P1 F4 174.6(3) . .
F3 P1 F4 90.3(3) . .
F1 P1 F4 91.1(5) . .
F2 P1 F6 93.6(9) . .
F3 P1 F6 84.4(8) . .
F1 P1 F6 175.6(9) . .
F4 P1 F6 85.0(8) . .
F2 P1 F5 89.4(3) . .
F3 P1 F5 173.8(2) . .
F1 P1 F5 91.1(5) . .
F4 P1 F5 85.44(19) . .
F6 P1 F5 90.7(7) . .
F11 P1 F9 170.2(8) . .
F10 P1 F9 86.7(8) . .
F7 P1 F9 84.8(9) . .
F12 P1 F9 91.5(13) . .
F11 P1 F8 93.5(6) . .
F10 P1 F8 164.8(10) . .
F7 P1 F8 90.0(9) . .
F12 P1 F8 79.8(14) . .
F9 P1 F8 78.1(8) . .
Ru1 O1 H13 116.0(19) . .
Ru1 O1 H13 116.0(18) . 4_565
H13 O1 H13 111(4) . 4_565
C7 N1 C1 106.68(14) . .
C7 N1 C1 106.68(14) . 4_565
C1 N1 C1 112.4(2) . 4_565
C7 N1 Ru1 116.22(17) . .
C1 N1 Ru1 107.51(11) . .
C1 N1 Ru1 107.51(11) 4_565 .
C2 N2 C6 118.42(15) . .
C2 N2 Ru1 114.86(11) . .
C6 N2 Ru1 126.26(12) . .
C8 N3 C12 118.05(13) . .
C8 N3 Ru1 126.32(11) . .
C12 N3 Ru1 115.55(10) . .
N1 C1 C2 112.61(16) . .
N1 C1 H1 109.1 . .
C2 C1 H1 109.1 . .
N1 C1 H2 109.1 . .
C2 C1 H2 109.1 . .
H1 C1 H2 107.8 . .
N2 C2 C3 121.52(18) . .
N2 C2 C1 114.91(15) . .
C3 C2 C1 123.39(18) . .
C4 C3 C2 119.6(2) . .
C4 C3 H3 120.2 . .
C2 C3 H3 120.2 . .
C3 C4 C5 118.84(17) . .
C3 C4 H4 120.6 . .
C5 C4 H4 120.6 . .
C4 C5 C6 119.51(19) . .
C4 C5 H5 120.2 . .
C6 C5 H5 120.2 . .
N2 C6 C5 122.08(18) . .
N2 C6 H6 119.0 . .
C5 C6 H6 119.0 . .
N1 C7 H7 110(2) . .
N1 C7 H8 109.3(16) . .
H7 C7 H8 110.2(19) . .
N1 C7 H8 109.3(16) . 4_565
H7 C7 H8 110.2(19) . 4_565
H8 C7 H8 108(3) . 4_565
N3 C8 C9 122.74(15) . .
N3 C8 H9 118.6 . .
C9 C8 H9 118.6 . .
C10 C9 C8 119.14(16) . .
C10 C9 H10 120.4 . .
C8 C9 H10 120.4 . .
C9 C10 C11 118.93(16) . .
C9 C10 H11 120.5 . .
C11 C10 H11 120.5 . .
C10 C11 C12 119.47(15) . .
C10 C11 H12 120.3 . .
C12 C11 H12 120.3 . .
N3 C12 C11 121.67(14) . .
N3 C12 C12 114.80(8) . 4_565
C11 C12 C12 123.52(9) . 4_565
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru1 N3 2.0581(13) 4_565
Ru1 N3 2.0582(13) .
Ru1 N2 2.0648(13) .
Ru1 N2 2.0648(13) 4_565
Ru1 N1 2.092(2) .
Ru1 O1 2.1663(17) .
P1 F11 1.402(10) .
P1 F10 1.514(9) .
P1 F2 1.516(6) .
P1 F3 1.568(5) .
P1 F1 1.581(10) .
P1 F7 1.597(16) .
P1 F12 1.598(18) .
P1 F4 1.624(4) .
P1 F6 1.640(12) .
P1 F5 1.647(4) .
P1 F9 1.648(12) .
P1 F8 1.679(7) .
O1 H13 0.847(5) .
O1 H13 0.847(5) 4_565
N1 C7 1.490(3) .
N1 C1 1.495(2) .
N1 C1 1.495(2) 4_565
N2 C2 1.346(2) .
N2 C6 1.354(2) .
N3 C8 1.351(2) .
N3 C12 1.3637(19) .
C1 C2 1.498(3) .
C1 H1 0.9900 .
C1 H2 0.9900 .
C2 C3 1.394(3) .
C3 C4 1.375(4) .
C3 H3 0.9500 .
C4 C5 1.376(4) .
C4 H4 0.9500 .
C5 C6 1.380(2) .
C5 H5 0.9500 .
C6 H6 0.9500 .
C7 H7 0.950(5) .
C7 H8 0.951(5) .
C7 H8 0.951(5) 4_565
C8 C9 1.386(2) .
C8 H9 0.9500 .
C9 C10 1.383(2) .
C9 H10 0.9500 .
C10 C11 1.388(2) .
C10 H11 0.9500 .
C11 C12 1.391(2) .
C11 H12 0.9500 .
C12 C12 1.473(3) 4_565
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
C7 N1 C1 C2 155.51(19) . .
C1 N1 C1 C2 -87.9(2) 4_565 .
Ru1 N1 C1 C2 30.2(2) . .
C6 N2 C2 C3 0.8(2) . .
Ru1 N2 C2 C3 -171.82(15) . .
C6 N2 C2 C1 -174.38(16) . .
Ru1 N2 C2 C1 13.0(2) . .
N1 C1 C2 N2 -29.6(2) . .
N1 C1 C2 C3 155.36(18) . .
N2 C2 C3 C4 -1.6(3) . .
C1 C2 C3 C4 173.2(2) . .
C2 C3 C4 C5 0.7(3) . .
C3 C4 C5 C6 0.8(3) . .
C2 N2 C6 C5 0.8(2) . .
Ru1 N2 C6 C5 172.50(13) . .
C4 C5 C6 N2 -1.6(3) . .
C12 N3 C8 C9 -0.4(2) . .
Ru1 N3 C8 C9 176.03(12) . .
N3 C8 C9 C10 0.1(3) . .
C8 C9 C10 C11 0.3(3) . .
C9 C10 C11 C12 -0.4(3) . .
C8 N3 C12 C11 0.3(2) . .
Ru1 N3 C12 C11 -176.53(12) . .
C8 N3 C12 C12 -179.02(11) . 4_565
Ru1 N3 C12 C12 4.19(11) . 4_565
C10 C11 C12 N3 0.1(3) . .
C10 C11 C12 C12 179.35(12) . 4_565
