#------------------------------------------------------------------------------
#$Date: 2015-10-06 15:57:01 +0300 (Tue, 06 Oct 2015) $
#$Revision: 160520 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/40/4344065.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_4344065
loop_
_publ_author_name
'Brown, Tristan R.'
'Dolinar, Brian S.'
'Hillard, Elizabeth A.'
'Clérac, Rodolphe'
'Berry, John F.'
_publ_section_title
;
 Electronic Structure of Ru2(II,II) Oxypyridinates: Synthetic, Structural,
 and Theoretical Insights into Axial Ligand Binding.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8571
_journal_page_last               8589
_journal_paper_doi               10.1021/acs.inorgchem.5b01241
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C25 H17 Cl4 N5 O4 Ru2'
_chemical_formula_sum            'C25 H17 Cl4 N5 O4 Ru2'
_chemical_formula_weight         795.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 107.8400(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.5485(5)
_cell_length_b                   12.1926(4)
_cell_length_c                   13.7919(4)
_cell_measurement_reflns_used    9976
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      30.52
_cell_measurement_theta_min      2.37
_cell_volume                     2648.97(14)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'APEX2 Ver. 2013.2-0 (Bruker-AXS, 2013)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4102
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         30.533
_diffrn_reflns_theta_min         2.112
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.588
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.363075
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0580 before and 0.0426 after correction.
 The Ratio of minimum to maximum transmission is 0.84.
 The λ/2 correction factor is Not present

Final HKLF 4 output contains 72448 reflections, Rint = 0.0358
 (37211 with I > 3sig(I), Rint = 0.0324)
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.994
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.184
_exptl_crystal_size_mid          0.118
_exptl_crystal_size_min          0.094
_refine_diff_density_max         1.616
_refine_diff_density_min         -0.911
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         4102
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0231
_refine_ls_R_factor_gt           0.0213
_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/[σ²(Fo²)+(0.0181P)²+6.9044P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0534
_refine_ls_wR_factor_ref         0.0544
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3863
_reflns_number_total             4102
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic5b01241_si_002.cif
_cod_data_source_block           berry339
_cod_depositor_comments
'Adding full bibliography for 4344062--4344067.cif.'
_cod_database_code               4344065
_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_max   0.865
_shelx_estimated_absorpt_t_min   0.759
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12), C13(H13)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Ru1 Ru 0.5000 0.94087(2) 0.2500 0.01305(5) Uani 1 2 d S T P
Ru2 Ru 0.5000 0.75512(2) 0.2500 0.01036(5) Uani 1 2 d S T P
Cl1 Cl 0.57230(3) 0.56332(3) 0.12088(3) 0.01906(8) Uani 1 1 d . . .
Cl2 Cl 0.63381(3) 0.56380(3) 0.38468(3) 0.01720(8) Uani 1 1 d . . .
O1 O 0.62430(8) 0.94074(10) 0.25175(10) 0.0172(2) Uani 1 1 d . . .
O2 O 0.53650(8) 0.94172(10) 0.40506(10) 0.0170(2) Uani 1 1 d . . .
N1 N 0.60526(9) 0.76267(11) 0.19363(11) 0.0129(2) Uani 1 1 d . . .
N2 N 0.58146(9) 0.76329(11) 0.40165(10) 0.0126(2) Uani 1 1 d . . .
N3 N 0.5000 1.12407(18) 0.2500 0.0171(4) Uani 1 2 d S T P
C1 C 0.64973(10) 0.86004(14) 0.20864(13) 0.0151(3) Uani 1 1 d . . .
C2 C 0.72303(11) 0.87074(16) 0.17685(14) 0.0196(3) Uani 1 1 d . . .
H2 H 0.7543 0.9374 0.1887 0.024 Uiso 1 1 calc R . .
C3 C 0.74894(12) 0.78544(17) 0.12916(15) 0.0220(4) Uani 1 1 d . . .
H3 H 0.7981 0.7929 0.1079 0.026 Uiso 1 1 calc R . .
C4 C 0.70301(12) 0.68723(17) 0.11162(14) 0.0205(3) Uani 1 1 d . . .
H4 H 0.7197 0.6270 0.0784 0.025 Uiso 1 1 calc R . .
C5 C 0.63285(10) 0.68186(14) 0.14458(12) 0.0150(3) Uani 1 1 d . . .
C6 C 0.58117(11) 0.86033(14) 0.45267(13) 0.0145(3) Uani 1 1 d . . .
C7 C 0.62861(12) 0.87029(15) 0.55661(13) 0.0186(3) Uani 1 1 d . . .
H7 H 0.6267 0.9365 0.5922 0.022 Uiso 1 1 calc R . .
C8 C 0.67718(12) 0.78465(16) 0.60580(13) 0.0204(3) Uani 1 1 d . . .
H8 H 0.7090 0.7915 0.6757 0.024 Uiso 1 1 calc R . .
C9 C 0.68044(11) 0.68659(15) 0.55382(13) 0.0182(3) Uani 1 1 d . . .
H9 H 0.7147 0.6266 0.5863 0.022 Uiso 1 1 calc R . .
C10 C 0.63162(10) 0.68199(14) 0.45375(13) 0.0141(3) Uani 1 1 d . . .
C11 C 0.52190(11) 1.17979(15) 0.33816(14) 0.0195(3) Uani 1 1 d . . .
H11 H 0.5380 1.1402 0.4005 0.023 Uiso 1 1 calc R . .
C12 C 0.52169(12) 1.29342(15) 0.34097(15) 0.0212(3) Uani 1 1 d . . .
H12 H 0.5362 1.3313 0.4042 0.025 Uiso 1 1 calc R . .
C13 C 0.5000 1.3507(2) 0.2500 0.0212(5) Uani 1 2 d S T P
H13 H 0.5000 1.4286 0.2500 0.025 Uiso 1 2 calc RS 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 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'
O O 0.0106 0.0060 '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
O1 Ru1 Ru2 89.95(3) . .
O1 Ru1 Ru2 89.96(3) 2_655 .
O1 Ru1 O1 179.91(7) 2_655 .
O1 Ru1 N3 90.04(3) 2_655 .
O1 Ru1 N3 90.05(3) . .
O2 Ru1 Ru2 90.29(3) . .
O2 Ru1 Ru2 90.29(3) 2_655 .
O2 Ru1 O1 90.80(5) 2_655 2_655
O2 Ru1 O1 89.20(5) 2_655 .
O2 Ru1 O1 90.80(5) . .
O2 Ru1 O1 89.20(5) . 2_655
O2 Ru1 O2 179.42(7) . 2_655
O2 Ru1 N3 89.71(3) . .
O2 Ru1 N3 89.71(3) 2_655 .
N3 Ru1 Ru2 180.0 . .
N1 Ru2 Ru1 87.50(4) 2_655 .
N1 Ru2 Ru1 87.51(4) . .
N1 Ru2 N1 175.01(8) . 2_655
N2 Ru2 Ru1 87.30(4) 2_655 .
N2 Ru2 Ru1 87.30(4) . .
N2 Ru2 N1 88.95(5) . 2_655
N2 Ru2 N1 88.95(5) 2_655 .
N2 Ru2 N1 90.82(5) . .
N2 Ru2 N1 90.82(5) 2_655 2_655
N2 Ru2 N2 174.60(8) 2_655 .
C1 O1 Ru1 117.70(11) . .
C6 O2 Ru1 118.03(11) . .
C1 N1 Ru2 116.36(11) . .
C5 N1 Ru2 126.49(11) . .
C5 N1 C1 117.16(14) . .
C6 N2 Ru2 116.41(11) . .
C10 N2 Ru2 126.40(11) . .
C10 N2 C6 117.17(14) . .
C11 N3 Ru1 120.41(11) . .
C11 N3 Ru1 120.41(11) 2_655 .
C11 N3 C11 119.2(2) 2_655 .
O1 C1 N1 119.56(15) . .
O1 C1 C2 120.36(16) . .
N1 C1 C2 120.07(16) . .
C1 C2 H2 119.9 . .
C3 C2 C1 120.21(17) . .
C3 C2 H2 119.9 . .
C2 C3 H3 120.0 . .
C2 C3 C4 120.02(16) . .
C4 C3 H3 120.0 . .
C3 C4 H4 121.5 . .
C5 C4 C3 116.97(17) . .
C5 C4 H4 121.5 . .
N1 C5 Cl1 115.99(12) . .
N1 C5 C4 125.52(17) . .
C4 C5 Cl1 118.48(14) . .
O2 C6 N2 119.45(15) . .
O2 C6 C7 120.25(15) . .
N2 C6 C7 120.29(15) . .
C6 C7 H7 120.1 . .
C8 C7 C6 119.87(16) . .
C8 C7 H7 120.1 . .
C7 C8 H8 119.8 . .
C7 C8 C9 120.45(16) . .
C9 C8 H8 119.8 . .
C8 C9 H9 121.7 . .
C10 C9 C8 116.51(16) . .
C10 C9 H9 121.7 . .
N2 C10 Cl2 115.52(12) . .
N2 C10 C9 125.64(16) . .
C9 C10 Cl2 118.83(13) . .
N3 C11 H11 119.0 . .
N3 C11 C12 121.94(18) . .
C12 C11 H11 119.0 . .
C11 C12 H12 120.6 . .
C13 C12 C11 118.76(18) . .
C13 C12 H12 120.6 . .
C12 C13 C12 119.4(2) . 2_655
C12 C13 H13 120.3 . .
C12 C13 H13 120.3 2_655 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru1 Ru2 2.2648(3) .
Ru1 O1 2.0497(13) 2_655
Ru1 O1 2.0498(13) .
Ru1 O2 2.0363(13) .
Ru1 O2 2.0363(13) 2_655
Ru1 N3 2.234(2) .
Ru2 N1 2.1159(14) .
Ru2 N1 2.1159(14) 2_655
Ru2 N2 2.1153(14) 2_655
Ru2 N2 2.1153(14) .
Cl1 C5 1.7318(18) .
Cl2 C10 1.7340(17) .
O1 C1 1.285(2) .
O2 C6 1.290(2) .
N1 C1 1.379(2) .
N1 C5 1.351(2) .
N2 C6 1.377(2) .
N2 C10 1.350(2) .
N3 C11 1.342(2) 2_655
N3 C11 1.342(2) .
C1 C2 1.416(2) .
C2 H2 0.9500 .
C2 C3 1.368(3) .
C3 H3 0.9500 .
C3 C4 1.399(3) .
C4 H4 0.9500 .
C4 C5 1.372(2) .
C6 C7 1.413(2) .
C7 H7 0.9500 .
C7 C8 1.365(3) .
C8 H8 0.9500 .
C8 C9 1.404(3) .
C9 H9 0.9500 .
C9 C10 1.370(2) .
C11 H11 0.9500 .
C11 C12 1.386(3) .
C12 H12 0.9500 .
C12 C13 1.383(2) .
C13 C12 1.384(2) 2_655
C13 H13 0.9500 .
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
Ru1 Ru2 N1 C1 19.88(11) . .
Ru1 Ru2 N1 C5 -160.05(13) . .
Ru1 Ru2 N2 C6 20.49(11) . .
Ru1 Ru2 N2 C10 -161.44(13) . .
Ru1 O1 C1 N1 -21.2(2) . .
Ru1 O1 C1 C2 158.90(13) . .
Ru1 O2 C6 N2 -19.2(2) . .
Ru1 O2 C6 C7 161.47(13) . .
Ru1 N3 C11 C12 -179.27(13) . .
Ru2 Ru1 O1 C1 30.21(12) . .
Ru2 Ru1 O2 C6 29.07(12) . .
Ru2 N1 C1 O1 -2.3(2) . .
Ru2 N1 C1 C2 177.55(12) . .
Ru2 N1 C5 Cl1 3.28(19) . .
Ru2 N1 C5 C4 -177.70(14) . .
Ru2 N2 C6 O2 -4.1(2) . .
Ru2 N2 C6 C7 175.15(13) . .
Ru2 N2 C10 Cl2 4.90(19) . .
Ru2 N2 C10 C9 -176.10(13) . .
O1 Ru1 Ru2 N1 -21.13(5) 2_655 2_655
O1 Ru1 Ru2 N1 158.87(5) 2_655 .
O1 Ru1 Ru2 N1 -21.14(5) . .
O1 Ru1 Ru2 N1 158.87(5) . 2_655
O1 Ru1 Ru2 N2 69.80(5) . .
O1 Ru1 Ru2 N2 69.80(5) 2_655 2_655
O1 Ru1 Ru2 N2 -110.20(5) . 2_655
O1 Ru1 Ru2 N2 -110.20(5) 2_655 .
O1 Ru1 O2 C6 -60.89(12) . .
O1 Ru1 O2 C6 119.02(12) 2_655 .
O1 Ru1 N3 C11 -89.86(10) 2_655 2_655
O1 Ru1 N3 C11 90.14(10) 2_655 .
O1 Ru1 N3 C11 90.14(10) . 2_655
O1 Ru1 N3 C11 -89.86(10) . .
O1 C1 C2 C3 -178.69(17) . .
O2 Ru1 Ru2 N1 68.07(5) . 2_655
O2 Ru1 Ru2 N1 68.07(5) 2_655 .
O2 Ru1 Ru2 N1 -111.93(5) 2_655 2_655
O2 Ru1 Ru2 N1 -111.93(5) . .
O2 Ru1 Ru2 N2 -20.99(5) 2_655 2_655
O2 Ru1 Ru2 N2 159.01(5) . 2_655
O2 Ru1 Ru2 N2 -20.99(5) . .
O2 Ru1 Ru2 N2 159.01(5) 2_655 .
O2 Ru1 O1 C1 120.50(12) . .
O2 Ru1 O1 C1 -60.08(12) 2_655 .
O2 Ru1 N3 C11 0.94(10) . .
O2 Ru1 N3 C11 0.94(10) 2_655 2_655
O2 Ru1 N3 C11 -179.06(10) 2_655 .
O2 Ru1 N3 C11 -179.06(10) . 2_655
O2 C6 C7 C8 -178.53(17) . .
N1 Ru2 N2 C6 -67.06(12) 2_655 .
N1 Ru2 N2 C6 107.96(12) . .
N1 Ru2 N2 C10 -73.97(14) . .
N1 Ru2 N2 C10 111.01(14) 2_655 .
N1 C1 C2 C3 1.4(3) . .
N2 Ru2 N1 C1 -67.38(12) . .
N2 Ru2 N1 C1 107.22(12) 2_655 .
N2 Ru2 N1 C5 112.69(14) . .
N2 Ru2 N1 C5 -72.70(14) 2_655 .
N2 C6 C7 C8 2.2(3) . .
N3 Ru1 O1 C1 -149.79(12) . .
N3 Ru1 O2 C6 -150.93(12) . .
N3 C11 C12 C13 -1.4(3) . .
C1 N1 C5 Cl1 -176.65(12) . .
C1 N1 C5 C4 2.4(2) . .
C1 C2 C3 C4 0.0(3) . .
C2 C3 C4 C5 -0.3(3) . .
C3 C4 C5 Cl1 178.03(14) . .
C3 C4 C5 N1 -1.0(3) . .
C5 N1 C1 O1 177.60(15) . .
C5 N1 C1 C2 -2.5(2) . .
C6 N2 C10 Cl2 -177.04(12) . .
C6 N2 C10 C9 2.0(2) . .
C6 C7 C8 C9 0.1(3) . .
C7 C8 C9 C10 -1.2(3) . .
C8 C9 C10 Cl2 179.18(13) . .
C8 C9 C10 N2 0.2(3) . .
C10 N2 C6 O2 177.62(15) . .
C10 N2 C6 C7 -3.1(2) . .
C11 N3 C11 C12 0.74(13) 2_655 .
C11 C12 C13 C12 0.69(12) . 2_655
