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#$Date: 2023-01-21 10:28:04 +0200 (Sat, 21 Jan 2023) $
#$Revision: 280490 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/65/8106517.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_8106517
loop_
_publ_author_name
'Gichumbi, Joel M.'
'Omondi, Bernard'
'Friedrich, Holger B.'
_publ_section_title
;
 Crystal structure of (η
 6-benzene)-(N-(2,6-dimethylphenyl)-1-(pyridin-2-yl)methanimine-κ2
 N,N′)ruthenium(II) perchlorate monohydrate, C20H20Cl2N2O5Ru
;
_journal_issue                   2
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              301
_journal_page_last               303
_journal_paper_doi               10.1515/ncrs-2016-0251
_journal_volume                  232
_journal_year                    2017
_chemical_formula_moiety         'C20 H20 Cl N2 Ru, Cl O4, H2 O'
_chemical_formula_sum            'C20 H22 Cl2 N2 O5 Ru'
_chemical_formula_weight         542.36
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                103.7520(10)
_cell_angle_beta                 107.2960(10)
_cell_angle_gamma                98.5620(10)
_cell_formula_units_Z            2
_cell_length_a                   8.7921(2)
_cell_length_b                   11.2515(3)
_cell_length_c                   11.7014(3)
_cell_measurement_reflns_used    20110
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.65
_cell_measurement_theta_min      1.91
_cell_measurement_wavelength     0.71073
_cell_volume                     1043.01(5)
_computing_cell_refinement       'SAINT-plus [11]'
_computing_data_collection       'APEX2 [11]'
_computing_data_reduction        'SAINT-Plus and XPREP [11]'
_computing_molecular_graphics    'ORTEP3 [13]'
_computing_publication_material  'WinGX [13]'
_computing_structure_refinement  'SHELXL-2014/7 [12]'
_computing_structure_solution    'SHELXL-2014 [12]'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_device_type  'Bruker Smart ApexII CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0179
_diffrn_reflns_av_unetI/netI     0.0121
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.929
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20110
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.646
_diffrn_reflns_theta_min         1.91
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.043
_exptl_absorpt_correction_T_max  0.779
_exptl_absorpt_correction_T_min  0.541
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS [11]'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.727
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.461
_refine_diff_density_min         -0.842
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     281
_refine_ls_number_reflns         4980
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.146
_refine_ls_R_factor_all          0.0203
_refine_ls_R_factor_gt           0.0198
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0307P)²+0.5686P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0545
_refine_ls_wR_factor_ref         0.0553
_reflns_Friedel_coverage         0
_reflns_number_gt                4879
_reflns_number_total             4980
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_ncrs-2016-0251_suppl.cif
_cod_data_source_block           exp_NCRS_2016_0251
_cod_database_code               8106517
_shelx_estimated_absorpt_t_min   0.583
_shelx_estimated_absorpt_t_max   0.788
loop_
_symmetry_equiv_pos_as_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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.79319(2) 0.63316(2) 0.21062(2) 0.01208(4) Uani 1 1 d . . . . .
Cl1 Cl 0.75521(4) 0.45859(3) 0.03217(3) 0.01658(7) Uani 1 1 d . . . . .
Cl2 Cl 0.82850(4) 0.12510(3) 0.24803(3) 0.02023(8) Uani 1 1 d . . . . .
O1 O 0.7398(2) 0.03512(14) 0.28872(17) 0.0464(4) Uani 1 1 d . . . . .
N1 N 0.77315(14) 0.73128(11) 0.07798(11) 0.0136(2) Uani 1 1 d . . . . .
O4 O 0.8445(2) 0.24870(13) 0.32510(14) 0.0393(3) Uani 1 1 d . . . . .
O3 O 0.98767(19) 0.10354(19) 0.25916(16) 0.0485(4) Uani 1 1 d . . . . .
O1W O 0.40261(17) 0.90548(13) 0.14686(14) 0.0305(3) Uani 1 1 d . . . . .
O2 O 0.73832(18) 0.11387(18) 0.11950(13) 0.0471(4) Uani 1 1 d . . . . .
N2 N 1.03560(14) 0.68976(11) 0.22141(11) 0.0132(2) Uani 1 1 d . . . . .
C15 C 0.56793(19) 0.54757(15) 0.23728(15) 0.0214(3) Uani 1 1 d . . . . .
H15 H 0.4768 0.4862 0.1639 0.026 Uiso 1 1 calc R U . . .
C7 C 1.17778(16) 0.69020(13) 0.32283(13) 0.0148(2) Uani 1 1 d . . . . .
C18 C 0.8553(2) 0.72331(19) 0.41112(14) 0.0285(4) Uani 1 1 d . . . . .
H18 H 0.9637 0.7843 0.4597 0.034 Uiso 1 1 calc R U . . .
C12 C 1.21479(17) 0.57616(14) 0.33606(13) 0.0166(3) Uani 1 1 d . . . . .
C19 C 0.8441(2) 0.5922(2) 0.39153(16) 0.0288(4) Uani 1 1 d . . . . .
H19 H 0.9452 0.5626 0.4257 0.035 Uiso 1 1 calc R U . . .
C1 C 0.63394(17) 0.74956(13) 0.00561(14) 0.0169(3) Uani 1 1 d . . . . .
H1 H 0.5339 0.7206 0.017 0.02 Uiso 1 1 calc R U . . .
C13 C 1.12083(19) 0.45164(14) 0.24141(15) 0.0219(3) Uani 1 1 d . . . . .
H13A H 1.1738 0.3853 0.263 0.033 Uiso 1 1 calc R U . . .
H13B H 1.1189 0.4544 0.1579 0.033 Uiso 1 1 calc R U . . .
H13C H 1.0083 0.4337 0.2414 0.033 Uiso 1 1 calc R U . . .
C5 C 0.91439(16) 0.76878(12) 0.05742(13) 0.0140(2) Uani 1 1 d . . . . .
C16 C 0.57873(19) 0.67633(16) 0.25842(14) 0.0208(3) Uani 1 1 d . . . . .
H16 H 0.4952 0.7052 0.1993 0.025 Uiso 1 1 calc R U . . .
C8 C 1.26938(17) 0.80731(14) 0.40904(13) 0.0182(3) Uani 1 1 d . . . . .
C2 C 0.63199(18) 0.80981(14) -0.08572(14) 0.0194(3) Uani 1 1 d . . . . .
H2 H 0.532 0.8228 -0.1349 0.023 Uiso 1 1 calc R U . . .
C20 C 0.7031(2) 0.50464(16) 0.30369(17) 0.0252(3) Uani 1 1 d . . . . .
H20 H 0.7046 0.4137 0.2768 0.03 Uiso 1 1 calc R U . . .
C4 C 0.92094(18) 0.82883(13) -0.03194(14) 0.0172(3) Uani 1 1 d . . . . .
H4 H 1.0217 0.8546 -0.0436 0.021 Uiso 1 1 calc R U . . .
C6 C 1.05802(16) 0.74499(13) 0.14126(13) 0.0143(2) Uani 1 1 d . . . . .
H6 H 1.1639 0.7692 0.137 0.017 Uiso 1 1 calc R U . . .
C14 C 1.2268(2) 0.92963(15) 0.39658(15) 0.0249(3) Uani 1 1 d . . . . .
H14A H 1.2845 0.9963 0.4761 0.037 Uiso 1 1 calc R U . . .
H14B H 1.1083 0.9202 0.3755 0.037 Uiso 1 1 calc R U . . .
H14C H 1.26 0.9519 0.33 0.037 Uiso 1 1 calc R U . . .
C17 C 0.7235(2) 0.76542(15) 0.34458(15) 0.0244(3) Uani 1 1 d . . . . .
H17 H 0.7389 0.8559 0.3466 0.029 Uiso 1 1 calc R U . . .
C3 C 0.77702(19) 0.85070(14) -0.10440(14) 0.0189(3) Uani 1 1 d . . . . .
H3 H 0.778 0.8929 -0.1656 0.023 Uiso 1 1 calc R U . . .
C11 C 1.34820(18) 0.58234(16) 0.44018(14) 0.0219(3) Uani 1 1 d . . . . .
H11 H 1.3757 0.5065 0.452 0.026 Uiso 1 1 calc R U . . .
C9 C 1.40247(18) 0.80774(16) 0.51109(14) 0.0239(3) Uani 1 1 d . . . . .
H9 H 1.4671 0.8856 0.5706 0.029 Uiso 1 1 calc R U . . .
C10 C 1.44134(18) 0.69647(18) 0.52658(14) 0.0254(3) Uani 1 1 d . . . . .
H10 H 1.5319 0.6984 0.5965 0.031 Uiso 1 1 calc R U . . .
H2W H 0.375(3) 0.902(3) 0.070(3) 0.050(8) Uiso 1 1 d . . . . .
H1W H 0.505(4) 0.951(3) 0.178(3) 0.046(7) Uiso 1 1 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 0 '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 0.006 '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
N2 Ru1 N1 76.90(5) . .
N2 Ru1 C18 92.01(5) . .
N1 Ru1 C18 123.91(6) . .
N2 Ru1 C17 113.58(6) . .
N1 Ru1 C17 97.61(5) . .
C18 Ru1 C17 37.53(7) . .
N2 Ru1 C20 126.35(6) . .
N1 Ru1 C20 155.65(6) . .
C18 Ru1 C20 67.81(7) . .
C17 Ru1 C20 80.35(6) . .
N2 Ru1 C19 97.91(5) . .
N1 Ru1 C19 161.48(7) . .
C18 Ru1 C19 37.81(7) . .
C17 Ru1 C19 67.86(7) . .
C20 Ru1 C19 37.11(7) . .
N2 Ru1 C16 150.09(5) . .
N1 Ru1 C16 96.04(5) . .
C18 Ru1 C16 67.60(6) . .
C17 Ru1 C16 37.71(6) . .
C20 Ru1 C16 67.45(6) . .
C19 Ru1 C16 79.54(6) . .
N2 Ru1 C15 164.19(6) . .
N1 Ru1 C15 118.89(5) . .
C18 Ru1 C15 79.95(6) . .
C17 Ru1 C15 67.52(6) . .
C20 Ru1 C15 37.91(6) . .
C19 Ru1 C15 67.44(6) . .
C16 Ru1 C15 36.78(6) . .
N2 Ru1 Cl1 88.41(3) . .
N1 Ru1 Cl1 82.05(3) . .
C18 Ru1 Cl1 153.40(5) . .
C17 Ru1 Cl1 157.46(5) . .
C20 Ru1 Cl1 90.71(5) . .
C19 Ru1 Cl1 115.85(5) . .
C16 Ru1 Cl1 119.76(4) . .
C15 Ru1 Cl1 92.77(4) . .
O4 Cl2 O3 109.45(11) . .
O4 Cl2 O1 108.64(9) . .
O3 Cl2 O1 110.17(10) . .
O4 Cl2 O2 109.22(10) . .
O3 Cl2 O2 109.97(9) . .
O1 Cl2 O2 109.36(11) . .
C1 N1 C5 118.46(12) . .
C1 N1 Ru1 126.12(10) . .
C5 N1 Ru1 115.13(9) . .
C6 N2 C7 118.09(11) . .
C6 N2 Ru1 116.33(9) . .
C7 N2 Ru1 124.75(9) . .
C16 C15 C20 119.82(15) . .
C16 C15 Ru1 71.48(8) . .
C20 C15 Ru1 70.48(8) . .
C12 C7 C8 122.51(13) . .
C12 C7 N2 120.01(12) . .
C8 C7 N2 117.40(13) . .
C17 C18 C19 120.12(15) . .
C17 C18 Ru1 71.31(9) . .
C19 C18 Ru1 71.82(9) . .
C11 C12 C7 117.34(14) . .
C11 C12 C13 120.21(14) . .
C7 C12 C13 122.42(13) . .
C20 C19 C18 120.00(15) . .
C20 C19 Ru1 71.16(9) . .
C18 C19 Ru1 70.37(9) . .
N1 C1 C2 121.83(13) . .
N1 C5 C4 122.61(13) . .
N1 C5 C6 113.98(12) . .
C4 C5 C6 123.36(13) . .
C15 C16 C17 120.52(14) . .
C15 C16 Ru1 71.74(8) . .
C17 C16 Ru1 70.33(8) . .
C9 C8 C7 117.62(14) . .
C9 C8 C14 119.90(14) . .
C7 C8 C14 122.47(13) . .
C3 C2 C1 119.54(13) . .
C19 C20 C15 119.85(15) . .
C19 C20 Ru1 71.73(9) . .
C15 C20 Ru1 71.60(8) . .
C5 C4 C3 118.70(13) . .
N2 C6 C5 117.22(12) . .
C18 C17 C16 119.65(15) . .
C18 C17 Ru1 71.16(9) . .
C16 C17 Ru1 71.96(8) . .
C2 C3 C4 118.82(13) . .
C10 C11 C12 121.50(15) . .
C10 C9 C8 121.04(15) . .
C9 C10 C11 119.99(14) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru1 N2 2.0884(11) .
Ru1 N1 2.0902(12) .
Ru1 C18 2.1847(16) .
Ru1 C17 2.1867(15) .
Ru1 C20 2.1964(15) .
Ru1 C19 2.2037(15) .
Ru1 C16 2.2079(14) .
Ru1 C15 2.2112(14) .
Ru1 Cl1 2.4021(3) .
Cl2 O4 1.4273(14) .
Cl2 O3 1.4289(14) .
Cl2 O1 1.4402(14) .
Cl2 O2 1.4413(14) .
N1 C1 1.3412(18) .
N1 C5 1.3594(17) .
N2 C6 1.2866(18) .
N2 C7 1.4437(17) .
C15 C16 1.394(2) .
C15 C20 1.432(2) .
C7 C12 1.402(2) .
C7 C8 1.4040(19) .
C18 C17 1.406(3) .
C18 C19 1.422(3) .
C12 C11 1.3966(19) .
C12 C13 1.499(2) .
C19 C20 1.400(3) .
C1 C2 1.392(2) .
C5 C4 1.3832(19) .
C5 C6 1.4552(19) .
C16 C17 1.420(2) .
C8 C9 1.400(2) .
C8 C14 1.507(2) .
C2 C3 1.387(2) .
C4 C3 1.391(2) .
C11 C10 1.385(2) .
C9 C10 1.384(3) .
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
C6 N2 C7 C12 -119.27(15) . . . .
Ru1 N2 C7 C12 71.60(15) . . . .
C6 N2 C7 C8 64.02(17) . . . .
Ru1 N2 C7 C8 -105.11(13) . . . .
C8 C7 C12 C11 0.2(2) . . . .
N2 C7 C12 C11 -176.30(12) . . . .
C8 C7 C12 C13 -177.63(13) . . . .
N2 C7 C12 C13 5.8(2) . . . .
C17 C18 C19 C20 1.5(2) . . . .
Ru1 C18 C19 C20 -53.01(14) . . . .
C17 C18 C19 Ru1 54.52(13) . . . .
C5 N1 C1 C2 -2.5(2) . . . .
Ru1 N1 C1 C2 -175.98(11) . . . .
C1 N1 C5 C4 2.3(2) . . . .
Ru1 N1 C5 C4 176.50(10) . . . .
C1 N1 C5 C6 179.80(12) . . . .
Ru1 N1 C5 C6 -6.04(14) . . . .
C20 C15 C16 C17 0.6(2) . . . .
Ru1 C15 C16 C17 -52.70(13) . . . .
C20 C15 C16 Ru1 53.27(13) . . . .
C12 C7 C8 C9 0.2(2) . . . .
N2 C7 C8 C9 176.84(12) . . . .
C12 C7 C8 C14 -178.35(14) . . . .
N2 C7 C8 C14 -1.7(2) . . . .
N1 C1 C2 C3 1.0(2) . . . .
C18 C19 C20 C15 -2.4(2) . . . .
Ru1 C19 C20 C15 -55.06(13) . . . .
C18 C19 C20 Ru1 52.64(13) . . . .
C16 C15 C20 C19 1.4(2) . . . .
Ru1 C15 C20 C19 55.12(13) . . . .
C16 C15 C20 Ru1 -53.73(13) . . . .
N1 C5 C4 C3 -0.6(2) . . . .
C6 C5 C4 C3 -177.81(13) . . . .
C7 N2 C6 C5 -166.42(12) . . . .
Ru1 N2 C6 C5 3.63(16) . . . .
N1 C5 C6 N2 1.64(18) . . . .
C4 C5 C6 N2 179.08(13) . . . .
C19 C18 C17 C16 0.4(2) . . . .
Ru1 C18 C17 C16 55.19(13) . . . .
C19 C18 C17 Ru1 -54.76(13) . . . .
C15 C16 C17 C18 -1.5(2) . . . .
Ru1 C16 C17 C18 -54.82(13) . . . .
C15 C16 C17 Ru1 53.34(13) . . . .
C1 C2 C3 C4 0.8(2) . . . .
C5 C4 C3 C2 -1.0(2) . . . .
C7 C12 C11 C10 -0.5(2) . . . .
C13 C12 C11 C10 177.41(14) . . . .
C7 C8 C9 C10 -0.4(2) . . . .
C14 C8 C9 C10 178.18(14) . . . .
C8 C9 C10 C11 0.2(2) . . . .
C12 C11 C10 C9 0.3(2) . . . .
