#------------------------------------------------------------------------------
#$Date: 2019-11-07 23:17:12 +0200 (Thu, 07 Nov 2019) $
#$Revision: 223979 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/03/7700333.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_7700333
loop_
_publ_author_name
'Kataoka, Yusuke'
'Imasaki, Nanako'
'Arakawa, Kazuki'
'Yano, Natsumi'
'Sakiyama, Hiroshi'
'Sugimori, Tamotsu'
'Mitsumi, Minoru'
'Handa, Makoto'
_publ_section_title
;
 Paddlewheel-type diruthenium(iii,iii) tetrakis(2-aminopyridinate)
 complexes with NIR absorption features: combined experimental and
 theoretical study.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12421
_journal_page_last               12429
_journal_paper_doi               10.1039/c9dt02271f
_journal_volume                  48
_journal_year                    2019
_chemical_formula_sum            'C30 H40 Cl2 N8 O2 Ru2'
_chemical_formula_weight         817.74
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-05-17 deposited with the CCDC.    2019-06-24 downloaded from the CCDC.
;
_cell_angle_alpha                85.558(3)
_cell_angle_beta                 85.197(3)
_cell_angle_gamma                65.274(3)
_cell_formula_units_Z            1
_cell_length_a                   8.8746(3)
_cell_length_b                   9.9417(3)
_cell_length_c                   10.5840(4)
_cell_measurement_reflns_used    6733
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.0410
_cell_measurement_theta_min      2.2200
_cell_volume                     844.29(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_molecular_graphics    'CrystalStructure 4.3 (Rigaku, 2018)'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2018)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SIR2004 (Burla, et al., 2005)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1053
_diffrn_reflns_av_unetI/netI     0.0899
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9038
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.933
_diffrn_source                   'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    1.093
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.20045
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.43a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             414
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.176
_exptl_crystal_size_min          0.105
_refine_diff_density_max         1.867
_refine_diff_density_min         -2.071
_refine_diff_density_rms         0.275
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         3311
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0546
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0938P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1446
_refine_ls_wR_factor_ref         0.1500
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2887
_reflns_number_total             3311
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt02271f2.cif
_cod_data_source_block           complex2-[Ru2(ammp)4Cl2]
_cod_depositor_comments
'Adding full bibliography for 7700332--7700333.cif.'
_cod_database_code               7700333
_shelx_shelxl_version_number     2014/7
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -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
Ru1 Ru 0.07403(3) 0.07316(3) 0.47848(3) 0.01576(18) Uani 1 1 d . .
Cl1 Cl 0.27246(13) 0.19502(12) 0.42800(11) 0.0250(3) Uani 1 1 d . .
O16 O 0.3210(5) 0.0889(5) 0.0980(3) 0.0492(11) Uani 1 1 d . .
N1 N -0.1370(4) 0.2546(4) 0.4213(3) 0.0157(7) Uani 1 1 d . .
N2 N -0.2732(4) 0.1027(4) 0.4614(3) 0.0178(7) Uani 1 1 d . .
H2A H -0.3643 0.0916 0.4622 0.021 Uiso 1 1 calc R U
N3 N -0.0139(4) -0.1500(4) 0.3391(3) 0.0170(7) Uani 1 1 d . .
N4 N 0.1136(4) 0.0093(4) 0.2997(3) 0.0183(7) Uani 1 1 d . .
H4A H 0.1646 0.0486 0.2470 0.022 Uiso 1 1 calc R U
C1 C -0.2792(5) 0.2334(5) 0.4208(4) 0.0193(9) Uani 1 1 d . .
C2 C -0.4258(5) 0.3518(4) 0.3771(4) 0.0188(9) Uani 1 1 d . .
H2 H -0.5233 0.3381 0.3775 0.023 Uiso 1 1 calc R U
C3 C -0.4258(5) 0.4847(4) 0.3347(4) 0.0239(9) Uani 1 1 d . .
C4 C -0.2777(5) 0.5031(5) 0.3381(4) 0.0226(10) Uani 1 1 d . .
H4 H -0.2739 0.5930 0.3111 0.027 Uiso 1 1 calc R U
C5 C -0.1392(5) 0.3881(5) 0.3814(4) 0.0249(10) Uani 1 1 d . .
H5 H -0.0422 0.4021 0.3836 0.030 Uiso 1 1 calc R U
C6 C -0.5785(5) 0.6080(5) 0.2857(5) 0.0317(11) Uani 1 1 d . .
H6A H -0.5549 0.6924 0.2603 0.038 Uiso 1 1 calc R U
H6B H -0.6125 0.5762 0.2140 0.038 Uiso 1 1 calc R U
H6C H -0.6661 0.6347 0.3512 0.038 Uiso 1 1 calc R U
C7 C 0.0680(5) -0.0883(4) 0.2553(4) 0.0166(9) Uani 1 1 d . .
C8 C 0.1023(5) -0.1299(5) 0.1271(4) 0.0214(9) Uani 1 1 d . .
H8 H 0.1503 -0.0818 0.0692 0.026 Uiso 1 1 calc R U
C9 C 0.0654(5) -0.2401(4) 0.0879(4) 0.0234(9) Uani 1 1 d . .
C10 C -0.0074(5) -0.3096(5) 0.1779(4) 0.0269(10) Uani 1 1 d . .
H10 H -0.0297 -0.3877 0.1553 0.032 Uiso 1 1 calc R U
C11 C -0.0452(5) -0.2618(5) 0.2985(4) 0.0232(10) Uani 1 1 d . .
H11 H -0.0952 -0.3082 0.3563 0.028 Uiso 1 1 calc R U
C12 C 0.1068(6) -0.2882(5) -0.0468(4) 0.0319(11) Uani 1 1 d . .
H12A H 0.0724 -0.3661 -0.0573 0.038 Uiso 1 1 calc R U
H12B H 0.0499 -0.2056 -0.1038 0.038 Uiso 1 1 calc R U
H12C H 0.2245 -0.3238 -0.0652 0.038 Uiso 1 1 calc R U
C13 C 0.4316(6) 0.1222(7) 0.1183(5) 0.0411(13) Uani 1 1 d . .
C14 C 0.4336(10) 0.2609(8) 0.0730(8) 0.078(2) Uani 1 1 d . .
H14A H 0.5319 0.2666 0.0990 0.094 Uiso 1 1 calc R U
H14B H 0.4334 0.2686 -0.0179 0.094 Uiso 1 1 calc R U
H14C H 0.3371 0.3406 0.1078 0.094 Uiso 1 1 calc R U
C15 C 0.5796(7) 0.0185(8) 0.1881(5) 0.067(2) Uani 1 1 d . .
H15A H 0.6539 0.0651 0.1948 0.080 Uiso 1 1 calc R U
H15B H 0.5437 -0.0053 0.2716 0.080 Uiso 1 1 calc R U
H15C H 0.6360 -0.0707 0.1428 0.080 Uiso 1 1 calc R U
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'
Cl Cl 0.1484 0.1585 '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'
Ru Ru -1.2594 0.8363 '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'
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
N4 Ru1 N2 93.38(13) . 2_556
N4 Ru1 N3 175.52(11) . 2_556
N2 Ru1 N3 90.86(13) 2_556 2_556
N4 Ru1 N1 87.92(13) . .
N2 Ru1 N1 178.16(12) 2_556 .
N3 Ru1 N1 87.81(13) 2_556 .
N4 Ru1 Ru1 88.19(11) . 2_556
N2 Ru1 Ru1 86.82(10) 2_556 2_556
N3 Ru1 Ru1 90.57(10) 2_556 2_556
N1 Ru1 Ru1 91.93(10) . 2_556
N4 Ru1 Cl1 88.58(11) . .
N2 Ru1 Cl1 85.36(10) 2_556 .
N3 Ru1 Cl1 93.24(10) 2_556 .
N1 Ru1 Cl1 95.97(10) . .
Ru1 Ru1 Cl1 171.35(3) 2_556 .
C5 N1 C1 119.2(3) . .
C5 N1 Ru1 124.1(3) . .
C1 N1 Ru1 116.7(3) . .
C1 N2 Ru1 126.9(3) . 2_556
C1 N2 H2A 116.6 . .
Ru1 N2 H2A 116.6 2_556 .
C11 N3 C7 117.6(4) . .
C11 N3 Ru1 124.2(3) . 2_556
C7 N3 Ru1 118.1(3) . 2_556
C7 N4 Ru1 125.6(3) . .
C7 N4 H4A 117.2 . .
Ru1 N4 H4A 117.2 . .
N2 C1 N1 117.6(3) . .
N2 C1 C2 123.2(4) . .
N1 C1 C2 119.2(4) . .
C3 C2 C1 121.2(4) . .
C3 C2 H2 119.4 . .
C1 C2 H2 119.4 . .
C2 C3 C4 118.1(4) . .
C2 C3 C6 121.3(4) . .
C4 C3 C6 120.6(4) . .
C5 C4 C3 119.5(4) . .
C5 C4 H4 120.2 . .
C3 C4 H4 120.2 . .
N1 C5 C4 122.9(4) . .
N1 C5 H5 118.6 . .
C4 C5 H5 118.6 . .
C3 C6 H6A 109.5 . .
C3 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
C3 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
N4 C7 N3 117.1(4) . .
N4 C7 C8 122.6(4) . .
N3 C7 C8 120.3(4) . .
C9 C8 C7 120.5(4) . .
C9 C8 H8 119.7 . .
C7 C8 H8 119.7 . .
C8 C9 C10 118.1(4) . .
C8 C9 C12 120.8(4) . .
C10 C9 C12 121.1(4) . .
C11 C10 C9 119.6(4) . .
C11 C10 H10 120.2 . .
C9 C10 H10 120.2 . .
N3 C11 C10 123.6(4) . .
N3 C11 H11 118.2 . .
C10 C11 H11 118.2 . .
C9 C12 H12A 109.5 . .
C9 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C9 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
O16 C13 C14 122.1(6) . .
O16 C13 C15 122.0(6) . .
C14 C13 C15 115.9(5) . .
C13 C14 H14A 109.5 . .
C13 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C13 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C13 C15 H15A 109.5 . .
C13 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
C13 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru1 N4 1.999(3) .
Ru1 N2 2.004(3) 2_556
Ru1 N3 2.076(4) 2_556
Ru1 N1 2.079(3) .
Ru1 Ru1 2.3336(6) 2_556
Ru1 Cl1 2.5262(11) .
O16 C13 1.199(6) .
N1 C5 1.354(5) .
N1 C1 1.364(5) .
N2 C1 1.318(5) .
N2 Ru1 2.004(3) 2_556
N2 H2A 0.8600 .
N3 C11 1.360(5) .
N3 C7 1.368(6) .
N3 Ru1 2.076(4) 2_556
N4 C7 1.325(5) .
N4 H4A 0.8600 .
C1 C2 1.424(5) .
C2 C3 1.362(6) .
C2 H2 0.9300 .
C3 C4 1.405(6) .
C3 C6 1.496(5) .
C4 C5 1.365(6) .
C4 H4 0.9300 .
C5 H5 0.9300 .
C6 H6A 0.9600 .
C6 H6B 0.9600 .
C6 H6C 0.9600 .
C7 C8 1.421(6) .
C8 C9 1.368(6) .
C8 H8 0.9300 .
C9 C10 1.403(6) .
C9 C12 1.506(6) .
C10 C11 1.363(6) .
C10 H10 0.9300 .
C11 H11 0.9300 .
C12 H12A 0.9600 .
C12 H12B 0.9600 .
C12 H12C 0.9600 .
C13 C14 1.431(9) .
C13 C15 1.499(7) .
C14 H14A 0.9600 .
C14 H14B 0.9600 .
C14 H14C 0.9600 .
C15 H15A 0.9600 .
C15 H15B 0.9600 .
C15 H15C 0.9600 .
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
Ru1 N2 C1 N1 -1.4(6) 2_556
Ru1 N2 C1 C2 178.6(3) 2_556
C5 N1 C1 N2 -179.3(3) .
Ru1 N1 C1 N2 2.8(5) .
C5 N1 C1 C2 0.7(6) .
Ru1 N1 C1 C2 -177.2(3) .
N2 C1 C2 C3 -179.3(4) .
N1 C1 C2 C3 0.7(6) .
C1 C2 C3 C4 -1.5(7) .
C1 C2 C3 C6 178.4(4) .
C2 C3 C4 C5 1.0(7) .
C6 C3 C4 C5 -178.9(4) .
C1 N1 C5 C4 -1.2(7) .
Ru1 N1 C5 C4 176.5(3) .
C3 C4 C5 N1 0.4(7) .
Ru1 N4 C7 N3 0.4(5) .
Ru1 N4 C7 C8 -179.2(2) .
C11 N3 C7 N4 -173.0(3) .
Ru1 N3 C7 N4 4.6(4) 2_556
C11 N3 C7 C8 6.5(5) .
Ru1 N3 C7 C8 -175.8(2) 2_556
N4 C7 C8 C9 174.5(3) .
N3 C7 C8 C9 -5.0(5) .
C7 C8 C9 C10 0.2(5) .
C7 C8 C9 C12 -177.9(3) .
C8 C9 C10 C11 2.7(6) .
C12 C9 C10 C11 -179.1(4) .
C7 N3 C11 C10 -3.6(6) .
Ru1 N3 C11 C10 178.9(3) 2_556
C9 C10 C11 N3 -1.1(6) .
