#------------------------------------------------------------------------------
#$Date: 2018-05-02 15:32:12 +0300 (Wed, 02 May 2018) $
#$Revision: 207621 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/62/7046215.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_7046215
loop_
_publ_author_name
'Arikawa, Yasuhiro'
'Hiura, Junko'
'Tsuchii, Chika'
'Kodama, Mika'
'Matsumoto, Naoki'
'Umakoshi, Keisuke'
_publ_section_title
;
 Synthetic NO reduction cycle on a bis(pyrazolato)-bridged dinuclear
 ruthenium complex including photo-induced transformation
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C8DT01208C
_journal_year                    2018
_chemical_formula_moiety         'C24 H27 B2 N16 O Ru2, P F6, C4 H10 O'
_chemical_formula_sum            'C28 H37 B2 F6 N16 O2 P Ru2'
_chemical_formula_weight         998.43
_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
;
2018-04-23 deposited with the CCDC.
2018-04-30 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                   11.8607(8)
_cell_length_b                   15.0217(9)
_cell_length_c                   10.8179(7)
_cell_measurement_reflns_used    3182
_cell_measurement_temperature    296
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.21
_cell_volume                     1927.4(2)
_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  'SHELXL Version 2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla, et al., 2005)'
_diffrn_ambient_temperature      296
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            13785
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.241
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         3.302
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.907
_exptl_absorpt_correction_T_max  0.913
_exptl_absorpt_correction_T_min  0.815
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.720
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1000.00
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetone/ether'
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.31
_refine_diff_density_min         -0.88
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.299
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     149
_refine_ls_number_reflns         2382
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0740
_refine_ls_R_factor_gt           0.0666
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0375P)²+4.4427P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1278
_refine_ls_wR_factor_ref         0.1315
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2221
_reflns_number_total             2382
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            c8dt01208c2.cif
_cod_data_source_block           4'
_cod_database_code               7046215
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 0.7500 0.36003(4) 0.60457(5) 0.03209(18) Uani 1 2 d S T P
P1 P 0.2500 0.2500 0.9682(3) 0.0503(7) Uani 1 4 d S T P
F1 F 0.2500 0.3554(3) 0.9679(6) 0.0803(17) Uani 1 2 d S T P
F2 F 0.3434(6) 0.2500 0.8634(6) 0.109(2) Uani 1 2 d S T P
F3 F 0.3438(6) 0.2500 1.0707(6) 0.110(2) Uani 1 2 d S T P
O1 O 0.7500 0.2500 0.7048(6) 0.0344(14) Uani 1 4 d DS T P
H9 H 0.7500 0.2500 0.786(2) 0.08(4) Uiso 1 4 d DS . P
O2 O 0.7500 0.2500 0.9530(16) 0.140(5) Uiso 1 4 d S . P
N1 N 0.7500 0.4709(4) 0.4983(5) 0.0399(14) Uani 1 2 d S T P
N2 N 0.7500 0.5527(4) 0.5552(6) 0.0424(14) Uani 1 2 d S T P
N3 N 0.6297(3) 0.4229(3) 0.7111(4) 0.0377(9) Uani 1 1 d . . .
N4 N 0.6459(4) 0.5093(3) 0.7450(4) 0.0405(9) Uani 1 1 d . . .
N5 N 0.6306(3) 0.2957(2) 0.5014(3) 0.0349(9) Uani 1 1 d . . .
C1 C 0.7500 0.4865(5) 0.3772(7) 0.0477(18) Uani 1 2 d S T P
H1 H 0.7500 0.4424 0.3168 0.057 Uiso 1 2 calc R U P
C2 C 0.7500 0.5755(6) 0.3534(8) 0.060(2) Uani 1 2 d S T P
H2 H 0.7500 0.6034 0.2766 0.072 Uiso 1 2 calc R U P
C3 C 0.7500 0.6153(5) 0.4688(8) 0.054(2) Uani 1 2 d S T P
H3 H 0.7500 0.6763 0.4835 0.065 Uiso 1 2 calc R U P
C4 C 0.5352(4) 0.3957(4) 0.7658(5) 0.0478(13) Uani 1 1 d . . .
H4 H 0.5040 0.3393 0.7577 0.057 Uiso 1 1 calc R U .
C5 C 0.4903(5) 0.4637(4) 0.8363(6) 0.0591(16) Uani 1 1 d . . .
H5 H 0.4250 0.4621 0.8839 0.071 Uiso 1 1 calc R U .
C6 C 0.5621(5) 0.5340(4) 0.8212(5) 0.0502(14) Uani 1 1 d . . .
H6 H 0.5544 0.5897 0.8577 0.060 Uiso 1 1 calc R U .
C7 C 0.5442(5) 0.3229(4) 0.4325(5) 0.0466(13) Uani 1 1 d . . .
H7 H 0.5247 0.3819 0.4182 0.056 Uiso 1 1 calc R U .
C8 C 0.4881(7) 0.2500 0.3859(8) 0.057(2) Uani 1 2 d S T P
H8 H 0.4257 0.2500 0.3339 0.068 Uiso 1 2 calc R U P
C10 C 0.824(3) 0.306(3) 1.042(4) 0.30(2) Uiso 0.5 1 d . . P
C11 C 0.7500 0.379(2) 1.031(3) 0.253(13) Uiso 1 2 d S . P
B1 B 0.7500 0.5590(5) 0.6971(8) 0.0412(18) Uani 1 2 d S T P
H1A H 0.7500 0.6211 0.7245 0.049 Uiso 1 2 calc R U 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)
;
B B 0.0013 0.0007
;
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)
;
O O 0.0106 0.0060
;
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)
;
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
O1 Ru1 N1 178.6(2) . .
O1 Ru1 N5 84.51(15) . .
N1 Ru1 N5 94.52(15) . .
O1 Ru1 N5 84.51(15) . 2_655
N1 Ru1 N5 94.52(15) . 2_655
N5 Ru1 N5 87.6(2) . 2_655
O1 Ru1 N3 94.39(16) . .
N1 Ru1 N3 86.60(16) . .
N5 Ru1 N3 92.44(15) . .
N5 Ru1 N3 178.88(15) 2_655 .
O1 Ru1 N3 94.39(16) . 2_655
N1 Ru1 N3 86.60(16) . 2_655
N5 Ru1 N3 178.88(15) . 2_655
N5 Ru1 N3 92.44(15) 2_655 2_655
N3 Ru1 N3 87.5(2) . 2_655
F3 P1 F3 90.2(6) . 2
F3 P1 F1 90.08(18) . 3
F3 P1 F1 90.08(18) 2 3
F3 P1 F1 90.08(18) . .
F3 P1 F1 90.08(18) 2 .
F1 P1 F1 179.8(5) 3 .
F3 P1 F2 179.2(5) . 2
F3 P1 F2 90.5(4) 2 2
F1 P1 F2 89.92(18) 3 2
F1 P1 F2 89.92(18) . 2
F3 P1 F2 90.5(4) . .
F3 P1 F2 179.2(5) 2 .
F1 P1 F2 89.92(18) 3 .
F1 P1 F2 89.92(18) . .
F2 P1 F2 88.7(6) 2 .
Ru1 O1 Ru1 113.5(3) . 3
Ru1 O1 H9 123.26(15) . .
Ru1 O1 H9 123.26(15) 3 .
C10 O2 C10 103(3) 3 2_655
C10 O2 C10 69(3) 3 4_655
C10 O2 C10 65(3) 2_655 4_655
C10 O2 C10 65(3) 3 .
C10 O2 C10 69(3) 2_655 .
C10 O2 C10 103(3) 4_655 .
C1 N1 N2 106.5(6) . .
C1 N1 Ru1 134.8(5) . .
N2 N1 Ru1 118.8(4) . .
C3 N2 N1 108.6(6) . .
C3 N2 B1 131.3(7) . .
N1 N2 B1 120.1(6) . .
C4 N3 N4 107.0(4) . .
C4 N3 Ru1 133.6(4) . .
N4 N3 Ru1 119.3(3) . .
C6 N4 N3 108.9(4) . .
C6 N4 B1 132.0(5) . .
N3 N4 B1 119.1(4) . .
C7 N5 N5 107.8(3) . 3
C7 N5 Ru1 133.9(3) . .
N5 N5 Ru1 118.19(10) 3 .
N1 C1 C2 111.0(7) . .
N1 C1 H1 124.5 . .
C2 C1 H1 124.5 . .
C1 C2 C3 104.7(7) . .
C1 C2 H2 127.7 . .
C3 C2 H2 127.7 . .
N2 C3 C2 109.2(7) . .
N2 C3 H3 125.4 . .
C2 C3 H3 125.4 . .
N3 C4 C5 110.1(5) . .
N3 C4 H4 125.0 . .
C5 C4 H4 125.0 . .
C6 C5 C4 105.3(5) . .
C6 C5 H5 127.3 . .
C4 C5 H5 127.3 . .
N4 C6 C5 108.8(5) . .
N4 C6 H6 125.6 . .
C5 C6 H6 125.6 . .
N5 C7 C8 109.5(5) . .
N5 C7 H7 125.3 . .
C8 C7 H7 125.3 . .
C7 C8 C7 105.4(7) 3 .
C7 C8 H8 127.3 3 .
C7 C8 H8 127.3 . .
C11 C10 O2 91(3) . .
C11 C10 C10 141(2) . 3
O2 C10 C10 57.4(16) . 3
C11 C10 C10 52(2) . 2_655
O2 C10 C10 55.4(16) . 2_655
C10 C10 C10 89.999(17) 3 2_655
C10 C11 C10 77(4) . 2_655
N4 B1 N4 107.3(6) 2_655 .
N4 B1 N2 107.9(4) 2_655 .
N4 B1 N2 107.9(4) . .
N4 B1 H1A 111.2 2_655 .
N4 B1 H1A 111.2 . .
N2 B1 H1A 111.2 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru1 O1 1.977(3) .
Ru1 N1 2.024(6) .
Ru1 N5 2.046(4) .
Ru1 N5 2.046(4) 2_655
Ru1 N3 2.063(4) .
Ru1 N3 2.063(4) 2_655
P1 F3 1.571(6) .
P1 F3 1.571(6) 2
P1 F1 1.583(5) 3
P1 F1 1.583(5) .
P1 F2 1.585(6) 2
P1 F2 1.585(6) .
O1 Ru1 1.977(3) 3
O1 H9 0.88(2) .
O2 C10 1.55(4) 3
O2 C10 1.55(4) 2_655
O2 C10 1.55(4) 4_655
O2 C10 1.55(4) .
N1 C1 1.331(9) .
N1 N2 1.374(8) .
N2 C3 1.326(9) .
N2 B1 1.538(10) .
N3 C4 1.331(6) .
N3 N4 1.362(5) .
N4 C6 1.343(6) .
N4 B1 1.533(6) .
N5 C7 1.331(6) .
N5 N5 1.373(7) 3
C1 C2 1.361(11) .
C1 H1 0.9300 .
C2 C3 1.384(12) .
C2 H2 0.9300 .
C3 H3 0.9300 .
C4 C5 1.382(7) .
C4 H4 0.9300 .
C5 C6 1.366(8) .
C5 H5 0.9300 .
C6 H6 0.9300 .
C7 C8 1.376(7) .
C7 H7 0.9300 .
C8 C7 1.376(7) 3
C8 H8 0.9300 .
C10 C11 1.42(4) .
C10 C10 1.67(8) 3
C10 C10 1.76(8) 2_655
C11 C10 1.42(4) 2_655
B1 N4 1.533(6) 2_655
B1 H1A 0.9800 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O(1) H(9) O(2) 2.685(18) 0.880 1.805 180.0 no
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
C1 N1 N2 C3 0.000(3) . .
Ru1 N1 N2 C3 180.000(3) . .
C1 N1 N2 B1 180.000(3) . .
Ru1 N1 N2 B1 0.000(3) . .
C4 N3 N4 C6 0.8(5) . .
Ru1 N3 N4 C6 -175.3(3) . .
C4 N3 N4 B1 179.3(5) . .
Ru1 N3 N4 B1 3.3(6) . .
N2 N1 C1 C2 0.000(2) . .
Ru1 N1 C1 C2 180.000(3) . .
N1 C1 C2 C3 0.000(4) . .
N1 N2 C3 C2 0.000(3) . .
B1 N2 C3 C2 180.000(3) . .
C1 C2 C3 N2 0.000(3) . .
N4 N3 C4 C5 -0.7(6) . .
Ru1 N3 C4 C5 174.6(4) . .
N3 C4 C5 C6 0.3(7) . .
N3 N4 C6 C5 -0.6(6) . .
B1 N4 C6 C5 -178.9(6) . .
C4 C5 C6 N4 0.2(7) . .
N5 N5 C7 C8 -0.8(6) 3 .
Ru1 N5 C7 C8 -178.0(5) . .
N5 C7 C8 C7 1.2(9) . 3
C10 O2 C10 C11 -156.4(16) 3 .
C10 O2 C10 C11 -40(3) 2_655 .
C10 O2 C10 C11 -97(3) 4_655 .
C10 O2 C10 C10 116.2(17) 2_655 3
C10 O2 C10 C10 59.4(19) 4_655 3
C10 O2 C10 C10 -116.2(17) 3 2_655
C10 O2 C10 C10 -57(2) 4_655 2_655
O2 C10 C11 C10 43(3) . 2_655
C10 C10 C11 C10 10(5) 3 2_655
C6 N4 B1 N4 117.1(6) . 2_655
N3 N4 B1 N4 -61.0(7) . 2_655
C6 N4 B1 N2 -126.8(6) . .
N3 N4 B1 N2 55.0(6) . .
C3 N2 B1 N4 -122.2(4) . 2_655
N1 N2 B1 N4 57.8(4) . 2_655
C3 N2 B1 N4 122.2(4) . .
N1 N2 B1 N4 -57.8(4) . .
