#------------------------------------------------------------------------------
#$Date: 2018-11-01 02:10:04 +0200 (Thu, 01 Nov 2018) $
#$Revision: 211734 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/79/7047927.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_7047927
loop_
_publ_author_name
'Misawa-Suzuki, T.'
'Matsuya, K.'
'Watanabe, T.'
'Nagao, H.'
_publ_section_title
;
 Triply bridged dinuclear ruthenium complexes bearing
 alkylbis(2-pyridylmethyl)amine in the mixed-valence state of
 Ru(ii)--Ru(iii)
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C8DT03507E
_journal_year                    2018
_chemical_formula_moiety         'C31 H41 Br2 Cl F12 N6 O1.5 P2 Ru2'
_chemical_formula_sum            'C31 H41 Br2 Cl F12 N6 O1.5 P2 Ru2'
_chemical_formula_weight         1209.03
_space_group_crystal_system      orthorhombic
_space_group_IT_number           59
_space_group_name_Hall           '-P 2ab 2a'
_space_group_name_H-M_alt        'P m m n'
_symmetry_space_group_name_Hall  '-P 2ab 2a'
_symmetry_space_group_name_H-M   'P m m n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2018-08-28 deposited with the CCDC.
2018-10-23 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   13.913(3)
_cell_length_b                   15.805(4)
_cell_length_c                   9.095(2)
_cell_measurement_reflns_used    5444
_cell_measurement_temperature    93
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.20
_cell_volume                     1999.9(8)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.3'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2018)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            15087
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         3.415
_exptl_absorpt_coefficient_mu    3.001
_exptl_absorpt_correction_T_max  0.914
_exptl_absorpt_correction_T_min  0.715
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.008
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1188.00
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.86
_refine_diff_density_min         -0.67
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     183
_refine_ls_number_reflns         2465
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0300
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0264P)²+5.5777P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0700
_refine_ls_wR_factor_ref         0.0702
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2448
_reflns_number_total             2465
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            c8dt03507e2.cif
_cod_data_source_block           Ru2ClBr2ebpma2-low
_cod_original_cell_volume        2000.0(8)
_cod_database_code               7047927
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 1/2-X,+Y,+Z
3 +X,1/2-Y,+Z
4 1/2-X,1/2-Y,+Z
5 -X,-Y,-Z
6 -1/2+X,-Y,-Z
7 -X,-1/2+Y,-Z
8 -1/2+X,-1/2+Y,-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
Ru1 Ru 0.35407(2) 0.250000 1.02968(3) 0.01131(9) Uani 1 2 d S T P
Br1 Br 0.250000 0.13315(2) 1.13112(4) 0.01653(10) Uani 1 2 d S T P
Cl1 Cl 0.250000 0.250000 0.81757(13) 0.0114(2) Uani 1 4 d S T P
P4 P 0.750000 0.01471(7) 1.44592(11) 0.0219(2) Uani 1 2 d S T P
F6 F 0.750000 -0.0138(2) 1.2779(3) 0.0447(8) Uani 1 2 d S T P
F7 F 0.6694(2) -0.05393(17) 1.4842(3) 0.0593(7) Uani 1 1 d . . .
F8 F 0.6683(2) 0.08146(17) 1.4107(3) 0.0584(7) Uani 1 1 d . . .
F10 F 0.750000 0.0439(2) 1.6139(3) 0.0373(7) Uani 1 2 d S T P
O1 O 0.750000 0.250000 1.2390(16) 0.061(3) Uani 0.5 4 d S T P
O2 O 0.750000 0.250000 0.9444(7) 0.0618(18) Uani 1 4 d S T P
N1 N 0.4515(3) 0.250000 1.2087(4) 0.0222(7) Uani 1 2 d S T P
N2 N 0.44599(15) 0.15956(13) 0.9502(2) 0.0151(4) Uani 1 1 d . . .
C1 C 0.4040(4) 0.250000 1.3578(5) 0.0356(11) Uani 1 2 d S T P
H1 H 0.362326 0.199447 1.365489 0.043 Uiso 1 1 calc R U .
H2 H 0.362326 0.300553 1.365490 0.043 Uiso 1 1 calc R U .
C2 C 0.4736(6) 0.250000 1.4855(6) 0.0482(16) Uani 1 2 d S T P
H3 H 0.513(3) 0.300(3) 1.492(4) 0.042(11) Uiso 1 1 d . . .
H4 H 0.436(5) 0.250000 1.578(9) 0.07(2) Uiso 1 2 d S . P
C3 C 0.5106(3) 0.1712(2) 1.1966(4) 0.0326(7) Uani 1 1 d . . .
H5 H 0.570(3) 0.182(3) 1.230(5) 0.047(12) Uiso 1 1 d . . .
H6 H 0.475(3) 0.126(3) 1.255(5) 0.048(12) Uiso 1 1 d . . .
C4 C 0.5194(2) 0.13952(17) 1.0418(3) 0.0226(6) Uani 1 1 d . . .
C5 C 0.5927(2) 0.0860(2) 0.9965(4) 0.0314(7) Uani 1 1 d . . .
H7 H 0.636(3) 0.072(2) 1.057(4) 0.031(10) Uiso 1 1 d . . .
C6 C 0.5896(2) 0.0512(2) 0.8581(4) 0.0341(8) Uani 1 1 d . . .
H8 H 0.637(3) 0.011(3) 0.820(5) 0.052(12) Uiso 1 1 d . . .
C7 C 0.5125(2) 0.06906(19) 0.7677(4) 0.0290(7) Uani 1 1 d . . .
H9 H 0.506(3) 0.045(3) 0.673(5) 0.042(11) Uiso 1 1 d . . .
C8 C 0.4419(2) 0.12383(16) 0.8163(3) 0.0198(5) Uani 1 1 d . . .
H10 H 0.388(3) 0.138(2) 0.760(4) 0.024(9) Uiso 1 1 d . . .
C9 C 0.750000 0.250000 0.8096(9) 0.0357(15) Uani 1 4 d S T P
C10 C 0.8408(4) 0.250000 0.7219(7) 0.0380(11) Uani 1 2 d S T P
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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
Br Br -0.2901 2.4595
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Cl Cl 0.1484 0.1585
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
F F 0.0171 0.0103
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
P P 0.1023 0.0942
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Ru Ru -1.2594 0.8363
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(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
N2 Ru1 N2 88.43(12) . 3
N2 Ru1 N1 82.63(10) . .
N2 Ru1 N1 82.63(10) 3 .
N2 Ru1 Cl1 95.31(7) . .
N2 Ru1 Cl1 95.31(7) 3 .
N1 Ru1 Cl1 177.11(11) . .
N2 Ru1 Br1 88.66(6) . .
N2 Ru1 Br1 176.43(6) 3 .
N1 Ru1 Br1 94.95(7) . .
Cl1 Ru1 Br1 87.013(19) . .
N2 Ru1 Br1 176.43(6) . 3
N2 Ru1 Br1 88.66(6) 3 3
N1 Ru1 Br1 94.95(7) . 3
Cl1 Ru1 Br1 87.013(19) . 3
Br1 Ru1 Br1 94.17(2) . 3
N2 Ru1 Ru1 128.61(6) . 2
N2 Ru1 Ru1 128.61(6) 3 2
N1 Ru1 Ru1 129.78(11) . 2
Cl1 Ru1 Ru1 53.11(2) . 2
Br1 Ru1 Ru1 54.953(11) . 2
Br1 Ru1 Ru1 54.954(11) 3 2
Ru1 Br1 Ru1 70.09(2) . 2
Ru1 Cl1 Ru1 73.78(4) . 2
F8 P4 F8 91.7(2) 2_655 .
F8 P4 F6 89.66(13) 2_655 .
F8 P4 F6 89.66(13) . .
F8 P4 F10 90.08(13) 2_655 .
F8 P4 F10 90.08(13) . .
F6 P4 F10 179.63(18) . .
F8 P4 F7 89.59(16) 2_655 2_655
F8 P4 F7 178.53(16) . 2_655
F6 P4 F7 90.98(13) . 2_655
F10 P4 F7 89.28(13) . 2_655
F8 P4 F7 178.53(16) 2_655 .
F8 P4 F7 89.60(16) . .
F6 P4 F7 90.98(14) . .
F10 P4 F7 89.28(13) . .
F7 P4 F7 89.1(2) 2_655 .
C3 N1 C3 112.7(4) . 3
C3 N1 C1 107.9(2) . .
C3 N1 C1 107.9(2) 3 .
C3 N1 Ru1 107.13(18) . .
C3 N1 Ru1 107.12(18) 3 .
C1 N1 Ru1 114.2(3) . .
C8 N2 C4 119.4(2) . .
C8 N2 Ru1 125.90(18) . .
C4 N2 Ru1 114.62(19) . .
N1 C1 C2 114.2(5) . .
N1 C1 H1 108.7 . .
C2 C1 H1 108.7 . .
N1 C1 H2 108.7 . .
C2 C1 H2 108.7 . .
H1 C1 H2 107.6 . .
C1 C2 H3 114(3) . .
C1 C2 H4 108(4) . .
H3 C2 H4 105(3) . .
C1 C2 H3 114(3) . 3
H3 C2 H3 109(5) . 3
H4 C2 H3 105(3) . 3
N1 C3 C4 113.1(3) . .
N1 C3 H5 109(3) . .
C4 C3 H5 108(3) . .
N1 C3 H6 106(2) . .
C4 C3 H6 107(2) . .
H5 C3 H6 114(4) . .
N2 C4 C5 120.9(3) . .
N2 C4 C3 115.9(3) . .
C5 C4 C3 122.9(3) . .
C6 C5 C4 119.5(3) . .
C6 C5 H7 121(3) . .
C4 C5 H7 119(3) . .
C5 C6 C7 119.3(3) . .
C5 C6 H8 124(3) . .
C7 C6 H8 117(3) . .
C6 C7 C8 119.3(3) . .
C6 C7 H9 122(3) . .
C8 C7 H9 118(3) . .
N2 C8 C7 121.6(3) . .
N2 C8 H10 116(2) . .
C7 C8 H10 123(2) . .
O2 C9 C10 122.3(3) . 2_655
O2 C9 C10 122.3(3) . .
C10 C9 C10 115.5(7) 2_655 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru1 N2 2.050(2) .
Ru1 N2 2.050(2) 3
Ru1 N1 2.119(3) .
Ru1 Cl1 2.4121(10) .
Ru1 Br1 2.5216(5) .
Ru1 Br1 2.5216(5) 3
Ru1 Ru1 2.8961(9) 2
P4 F8 1.583(2) 2_655
P4 F8 1.583(2) .
P4 F6 1.593(3) .
P4 F10 1.596(3) .
P4 F7 1.598(2) 2_655
P4 F7 1.598(2) .
O2 C9 1.226(10) .
N1 C3 1.496(4) .
N1 C3 1.496(4) 3
N1 C1 1.508(6) .
N2 C8 1.344(4) .
N2 C4 1.356(3) .
C1 C2 1.512(7) .
C1 H1 0.9900 .
C1 H2 0.9900 .
C2 H3 0.96(4) .
C2 H4 0.99(8) .
C2 H3 0.96(4) 3
C3 C4 1.499(5) .
C3 H5 0.90(4) .
C3 H6 1.02(4) .
C4 C5 1.388(4) .
C5 C6 1.374(5) .
C5 H7 0.84(4) .
C6 C7 1.381(5) .
C6 H8 0.98(4) .
C7 C8 1.382(4) .
C7 H9 0.94(4) .
C8 H10 0.94(4) .
C9 C10 1.494(7) 2_655
C9 C10 1.494(7) .
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
C3 N1 C1 C2 61.0(2) .
C3 N1 C1 C2 -61.0(2) 3
Ru1 N1 C1 C2 180.000(1) .
C3 N1 C3 C4 -90.8(3) 3
C1 N1 C3 C4 150.2(3) .
Ru1 N1 C3 C4 26.8(3) .
C8 N2 C4 C5 3.2(4) .
Ru1 N2 C4 C5 -173.2(2) .
C8 N2 C4 C3 -170.8(3) .
Ru1 N2 C4 C3 12.9(3) .
N1 C3 C4 N2 -27.4(4) .
N1 C3 C4 C5 158.7(3) .
N2 C4 C5 C6 -1.6(4) .
C3 C4 C5 C6 171.9(3) .
C4 C5 C6 C7 -1.1(5) .
C5 C6 C7 C8 2.2(5) .
C4 N2 C8 C7 -2.1(4) .
Ru1 N2 C8 C7 173.9(2) .
C6 C7 C8 N2 -0.7(4) .
