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#$Date: 2023-08-30 04:11:34 +0300 (Wed, 30 Aug 2023) $
#$Revision: 285903 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/72/7247259.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_7247259
loop_
_publ_author_name
'Mukherjee, Aparajita'
'Datta, Sayanti'
'Richmond, Michael G.'
'Bhattacharya, Samaresh'
_publ_section_title
;
 Ruthenium complexes of 1,4-diazabutadiene ligands with a cis-RuCl2 moiety
 for catalytic acceptorless dehydrogenation of alcohols: DFT evidence of
 chemically non-innocent ligand participation
;
_journal_issue                   36
_journal_name_full               'RSC Advances'
_journal_page_first              25660
_journal_page_last               25672
_journal_paper_doi               10.1039/D3RA04750D
_journal_volume                  13
_journal_year                    2023
_chemical_formula_sum            'C30 H30 Cl8 N4 Ru'
_chemical_formula_weight         831.25
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2023-06-01 deposited with the CCDC.	2023-08-07 downloaded from the CCDC.
;
_cell_angle_alpha                112.6980(10)
_cell_angle_beta                 94.0140(10)
_cell_angle_gamma                113.0940(10)
_cell_formula_units_Z            2
_cell_length_a                   10.8657(2)
_cell_length_b                   13.3710(2)
_cell_length_c                   14.4857(3)
_cell_measurement_reflns_used    345
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.572
_cell_measurement_theta_min      1.578
_cell_volume                     1724.14(6)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            30195
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.572
_diffrn_reflns_theta_min         1.578
_exptl_absorpt_coefficient_mu    1.103
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             836
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.716
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         7938
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0483P)²+0.3279P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1003
_refine_ls_wR_factor_ref         0.1102
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6057
_reflns_number_total             7938
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3ra04750d2.cif
_cod_data_source_block           AM-8
_cod_database_code               7247259
_shelx_shelxl_version_number     2016/6
_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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.44216(3) 0.22286(2) 0.48232(2) 0.03346(9) Uani 1 1 d . . . . .
Cl1 Cl 0.25724(8) 0.27571(7) 0.51645(7) 0.0430(2) Uani 1 1 d . . . . .
Cl2 Cl 0.28417(8) 0.01997(7) 0.35316(7) 0.0429(2) Uani 1 1 d . . . . .
Cl3 Cl 1.00484(17) 0.70880(18) 0.27138(18) 0.1395(7) Uani 1 1 d . . . . .
Cl4 Cl 0.7321(2) 0.5277(2) 0.14177(13) 0.1496(8) Uani 1 1 d . . . . .
Cl5 Cl 0.85773(14) 0.50127(13) 0.30551(12) 0.0978(4) Uani 1 1 d . . . . .
Cl6 Cl 0.2260(2) 0.71872(18) 0.09911(17) 0.1465(7) Uani 1 1 d . . . . .
Cl7 Cl 0.09737(19) 0.82392(17) 0.01361(15) 0.1370(7) Uani 1 1 d . . . . .
Cl8 Cl 0.38971(19) 0.90610(19) 0.05048(15) 0.1443(7) Uani 1 1 d . . . . .
N1 N 0.6058(3) 0.1829(2) 0.4763(2) 0.0384(6) Uani 1 1 d . . . . .
N2 N 0.4382(3) 0.1600(2) 0.5914(2) 0.0383(6) Uani 1 1 d . . . . .
N3 N 0.5879(3) 0.3968(2) 0.5737(2) 0.0398(6) Uani 1 1 d . . . . .
N4 N 0.4685(3) 0.2976(2) 0.3807(2) 0.0381(6) Uani 1 1 d . . . . .
C1 C 0.6339(4) 0.1515(3) 0.5461(3) 0.0457(8) Uani 1 1 d . . . . .
H1 H 0.711539 0.139247 0.554692 0.055 Uiso 1 1 calc R U . . .
C2 C 0.5400(4) 0.1369(3) 0.6090(3) 0.0479(9) Uani 1 1 d . . . . .
H2 H 0.551050 0.112239 0.659589 0.058 Uiso 1 1 calc R U . . .
C9 C 0.3358(4) 0.1378(3) 0.6495(3) 0.0470(8) Uani 1 1 d . . . . .
C14 C 0.3757(5) 0.1858(4) 0.7560(3) 0.0693(12) Uani 1 1 d . . . . .
H14 H 0.468831 0.234323 0.791750 0.083 Uiso 1 1 calc R U . . .
C13 C 0.2754(7) 0.1608(6) 0.8087(4) 0.0977(18) Uani 1 1 d . . . . .
H13 H 0.300877 0.193955 0.880621 0.117 Uiso 1 1 calc R U . . .
C12 C 0.1372(6) 0.0866(6) 0.7552(5) 0.0970(18) Uani 1 1 d . . . . .
H12 H 0.069932 0.070395 0.790888 0.116 Uiso 1 1 calc R U . . .
C11 C 0.1004(5) 0.0377(5) 0.6501(4) 0.0750(13) Uani 1 1 d . . . . .
H11 H 0.007927 -0.014777 0.614053 0.090 Uiso 1 1 calc R U . . .
C10 C 0.1980(4) 0.0646(4) 0.5959(3) 0.0553(10) Uani 1 1 d . . . . .
H10 H 0.171251 0.033735 0.524263 0.066 Uiso 1 1 calc R U . . .
C3 C 0.6987(3) 0.1999(3) 0.4120(3) 0.0431(8) Uani 1 1 d . . . . .
C4 C 0.6454(4) 0.1501(4) 0.3074(3) 0.0576(10) Uani 1 1 d . . . . .
H4 H 0.549975 0.107545 0.278799 0.069 Uiso 1 1 calc R U . . .
C5 C 0.7352(5) 0.1636(5) 0.2443(4) 0.0786(13) Uani 1 1 d . . . . .
H5 H 0.700414 0.128465 0.172857 0.094 Uiso 1 1 calc R U . . .
C6 C 0.8751(5) 0.2290(5) 0.2880(5) 0.0827(15) Uani 1 1 d . . . . .
H6 H 0.935052 0.239693 0.245977 0.099 Uiso 1 1 calc R U . . .
C7 C 0.9275(5) 0.2782(5) 0.3912(5) 0.0872(16) Uani 1 1 d . . . . .
H7 H 1.022945 0.320994 0.419424 0.105 Uiso 1 1 calc R U . . .
C8 C 0.8406(4) 0.2655(4) 0.4551(4) 0.0666(11) Uani 1 1 d . . . . .
H8 H 0.876760 0.300503 0.526374 0.080 Uiso 1 1 calc R U . . .
C17 C 0.6529(4) 0.4460(3) 0.6812(3) 0.0433(8) Uani 1 1 d . . . . .
C22 C 0.7939(4) 0.4870(4) 0.7137(3) 0.0620(11) Uani 1 1 d . . . . .
H22 H 0.847151 0.482753 0.666156 0.074 Uiso 1 1 calc R U . . .
C21 C 0.8543(5) 0.5342(4) 0.8172(4) 0.0800(14) Uani 1 1 d . . . . .
H21 H 0.948821 0.560606 0.839497 0.096 Uiso 1 1 calc R U . . .
C20 C 0.7775(5) 0.5427(4) 0.8879(4) 0.0774(13) Uani 1 1 d . . . . .
H20 H 0.819228 0.575777 0.957984 0.093 Uiso 1 1 calc R U . . .
C19 C 0.6373(5) 0.5018(4) 0.8539(4) 0.0740(13) Uani 1 1 d . . . . .
H19 H 0.584580 0.508360 0.901779 0.089 Uiso 1 1 calc R U . . .
C18 C 0.5739(4) 0.4516(4) 0.7505(3) 0.0599(10) Uani 1 1 d . . . . .
H18 H 0.478639 0.421796 0.728015 0.072 Uiso 1 1 calc R U . . .
C15 C 0.6346(3) 0.4634(3) 0.5260(3) 0.0461(8) Uani 1 1 d . . . . .
H15 H 0.708124 0.541493 0.559679 0.055 Uiso 1 1 calc R U . . .
C16 C 0.5664(4) 0.4093(3) 0.4200(3) 0.0452(8) Uani 1 1 d . . . . .
H16 H 0.590080 0.451105 0.380320 0.054 Uiso 1 1 calc R U . . .
C23 C 0.3901(4) 0.2454(3) 0.2756(3) 0.0444(8) Uani 1 1 d . . . . .
C24 C 0.4564(4) 0.2538(4) 0.1983(3) 0.0607(10) Uani 1 1 d . . . . .
H24 H 0.552622 0.289761 0.213286 0.073 Uiso 1 1 calc R U . . .
C25 C 0.3786(5) 0.2084(5) 0.0993(3) 0.0761(13) Uani 1 1 d . . . . .
H25 H 0.422562 0.213883 0.047396 0.091 Uiso 1 1 calc R U . . .
C26 C 0.2359(5) 0.1550(5) 0.0767(4) 0.0782(13) Uani 1 1 d . . . . .
H26 H 0.184143 0.125073 0.009725 0.094 Uiso 1 1 calc R U . . .
C27 C 0.1703(5) 0.1460(4) 0.1525(3) 0.0660(11) Uani 1 1 d . . . . .
H27 H 0.073992 0.110261 0.136764 0.079 Uiso 1 1 calc R U . . .
C28 C 0.2459(4) 0.1894(3) 0.2523(3) 0.0514(9) Uani 1 1 d . . . . .
H28 H 0.200915 0.181322 0.303198 0.062 Uiso 1 1 calc R U . . .
C29 C 0.8438(5) 0.6045(5) 0.2658(4) 0.0802(14) Uani 1 1 d . . . . .
H29 H 0.803484 0.649427 0.313658 0.096 Uiso 1 1 calc R U . . .
C30 C 0.2439(5) 0.8493(4) 0.0925(4) 0.0815(14) Uani 1 1 d . . . . .
H30 H 0.257422 0.910201 0.162532 0.098 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'
N N 0.0061 0.0033 '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'
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
_geom_angle_publ_flag
N3 Ru1 N1 84.98(10) . . ?
N3 Ru1 N2 97.34(11) . . ?
N1 Ru1 N2 77.43(10) . . ?
N3 Ru1 N4 77.57(11) . . ?
N1 Ru1 N4 98.50(10) . . ?
N2 Ru1 N4 173.84(11) . . ?
N3 Ru1 Cl1 91.92(7) . . ?
N1 Ru1 Cl1 171.27(8) . . ?
N2 Ru1 Cl1 94.93(8) . . ?
N4 Ru1 Cl1 88.76(7) . . ?
N3 Ru1 Cl2 171.36(8) . . ?
N1 Ru1 Cl2 91.89(8) . . ?
N2 Ru1 Cl2 89.80(8) . . ?
N4 Ru1 Cl2 94.99(8) . . ?
Cl1 Ru1 Cl2 92.29(3) . . ?
C1 N1 C3 118.4(3) . . ?
C1 N1 Ru1 114.7(2) . . ?
C3 N1 Ru1 126.5(2) . . ?
C2 N2 C9 116.9(3) . . ?
C2 N2 Ru1 115.0(2) . . ?
C9 N2 Ru1 128.1(2) . . ?
C15 N3 C17 118.5(3) . . ?
C15 N3 Ru1 115.6(2) . . ?
C17 N3 Ru1 125.4(2) . . ?
C16 N4 C23 116.9(3) . . ?
C16 N4 Ru1 114.3(2) . . ?
C23 N4 Ru1 128.7(2) . . ?
N1 C1 C2 116.6(3) . . ?
N1 C1 H1 121.7 . . ?
C2 C1 H1 121.7 . . ?
N2 C2 C1 115.7(3) . . ?
N2 C2 H2 122.1 . . ?
C1 C2 H2 122.1 . . ?
C14 C9 C10 120.7(4) . . ?
C14 C9 N2 120.6(3) . . ?
C10 C9 N2 118.7(3) . . ?
C9 C14 C13 119.0(4) . . ?
C9 C14 H14 120.5 . . ?
C13 C14 H14 120.5 . . ?
C12 C13 C14 120.4(5) . . ?
C12 C13 H13 119.8 . . ?
C14 C13 H13 119.8 . . ?
C11 C12 C13 119.7(5) . . ?
C11 C12 H12 120.2 . . ?
C13 C12 H12 120.2 . . ?
C12 C11 C10 121.1(5) . . ?
C12 C11 H11 119.5 . . ?
C10 C11 H11 119.5 . . ?
C9 C10 C11 119.1(4) . . ?
C9 C10 H10 120.5 . . ?
C11 C10 H10 120.5 . . ?
C4 C3 C8 120.5(4) . . ?
C4 C3 N1 119.1(3) . . ?
C8 C3 N1 120.4(3) . . ?
C3 C4 C5 119.3(4) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
C6 C5 C4 119.5(5) . . ?
C6 C5 H5 120.2 . . ?
C4 C5 H5 120.2 . . ?
C7 C6 C5 121.0(4) . . ?
C7 C6 H6 119.5 . . ?
C5 C6 H6 119.5 . . ?
C6 C7 C8 120.5(4) . . ?
C6 C7 H7 119.8 . . ?
C8 C7 H7 119.8 . . ?
C7 C8 C3 119.2(4) . . ?
C7 C8 H8 120.4 . . ?
C3 C8 H8 120.4 . . ?
C18 C17 C22 120.8(4) . . ?
C18 C17 N3 119.2(3) . . ?
C22 C17 N3 120.0(3) . . ?
C21 C22 C17 119.1(4) . . ?
C21 C22 H22 120.4 . . ?
C17 C22 H22 120.4 . . ?
C20 C21 C22 120.9(4) . . ?
C20 C21 H21 119.6 . . ?
C22 C21 H21 119.6 . . ?
C21 C20 C19 119.1(4) . . ?
C21 C20 H20 120.5 . . ?
C19 C20 H20 120.5 . . ?
C18 C19 C20 121.1(4) . . ?
C18 C19 H19 119.4 . . ?
C20 C19 H19 119.4 . . ?
C17 C18 C19 118.9(4) . . ?
C17 C18 H18 120.5 . . ?
C19 C18 H18 120.5 . . ?
N3 C15 C16 115.7(3) . . ?
N3 C15 H15 122.2 . . ?
C16 C15 H15 122.2 . . ?
N4 C16 C15 116.4(3) . . ?
N4 C16 H16 121.8 . . ?
C15 C16 H16 121.8 . . ?
C24 C23 C28 120.0(4) . . ?
C24 C23 N4 120.8(3) . . ?
C28 C23 N4 119.2(3) . . ?
C25 C24 C23 119.5(4) . . ?
C25 C24 H24 120.2 . . ?
C23 C24 H24 120.2 . . ?
C24 C25 C26 120.5(4) . . ?
C24 C25 H25 119.8 . . ?
C26 C25 H25 119.8 . . ?
C27 C26 C25 120.2(4) . . ?
C27 C26 H26 119.9 . . ?
C25 C26 H26 119.9 . . ?
C26 C27 C28 120.6(4) . . ?
C26 C27 H27 119.7 . . ?
C28 C27 H27 119.7 . . ?
C27 C28 C23 119.3(4) . . ?
C27 C28 H28 120.4 . . ?
C23 C28 H28 120.4 . . ?
Cl3 C29 Cl5 111.2(3) . . ?
Cl3 C29 Cl4 111.5(3) . . ?
Cl5 C29 Cl4 110.3(3) . . ?
Cl3 C29 H29 107.9 . . ?
Cl5 C29 H29 107.9 . . ?
Cl4 C29 H29 107.9 . . ?
Cl6 C30 Cl7 111.4(3) . . ?
Cl6 C30 Cl8 109.7(3) . . ?
Cl7 C30 Cl8 111.3(3) . . ?
Cl6 C30 H30 108.1 . . ?
Cl7 C30 H30 108.1 . . ?
Cl8 C30 H30 108.1 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ru1 N3 2.028(3) . ?
Ru1 N1 2.046(2) . ?
Ru1 N2 2.053(2) . ?
Ru1 N4 2.053(3) . ?
Ru1 Cl1 2.4010(8) . ?
Ru1 Cl2 2.4055(8) . ?
Cl3 C29 1.729(5) . ?
Cl4 C29 1.747(5) . ?
Cl5 C29 1.739(5) . ?
Cl6 C30 1.721(5) . ?
Cl7 C30 1.726(5) . ?
Cl8 C30 1.734(5) . ?
N1 C1 1.293(4) . ?
N1 C3 1.434(4) . ?
N2 C2 1.293(4) . ?
N2 C9 1.449(4) . ?
N3 C15 1.301(4) . ?
N3 C17 1.431(4) . ?
N4 C16 1.304(4) . ?
N4 C23 1.436(4) . ?
C1 C2 1.421(5) . ?
C1 H1 0.9300 . ?
C2 H2 0.9300 . ?
C9 C14 1.379(5) . ?
C9 C10 1.380(5) . ?
C14 C13 1.383(6) . ?
C14 H14 0.9300 . ?
C13 C12 1.383(7) . ?
C13 H13 0.9300 . ?
C12 C11 1.359(7) . ?
C12 H12 0.9300 . ?
C11 C10 1.380(5) . ?
C11 H11 0.9300 . ?
C10 H10 0.9300 . ?
C3 C4 1.367(5) . ?
C3 C8 1.385(5) . ?
C4 C5 1.392(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.368(6) . ?
C5 H5 0.9300 . ?
C6 C7 1.349(7) . ?
C6 H6 0.9300 . ?
C7 C8 1.376(6) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C17 C18 1.365(5) . ?
C17 C22 1.382(5) . ?
C22 C21 1.373(6) . ?
C22 H22 0.9300 . ?
C21 C20 1.364(6) . ?
C21 H21 0.9300 . ?
C20 C19 1.377(6) . ?
C20 H20 0.9300 . ?
C19 C18 1.373(6) . ?
C19 H19 0.9300 . ?
C18 H18 0.9300 . ?
C15 C16 1.413(5) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C23 C24 1.391(5) . ?
C23 C28 1.393(5) . ?
C24 C25 1.376(6) . ?
C24 H24 0.9300 . ?
C25 C26 1.378(6) . ?
C25 H25 0.9300 . ?
C26 C27 1.369(6) . ?
C26 H26 0.9300 . ?
C27 C28 1.383(5) . ?
C27 H27 0.9300 . ?
C28 H28 0.9300 . ?
C29 H29 0.9800 . ?
C30 H30 0.9800 . ?
