Synthesis and Structural Characterization of Half-Sandwich Arene‒Ruthenium(II) Complexes with Bis(imidazol-1-yl)methane, Imidazole and Benzimidazole
Matveevskaya, Vladislava V.; Pavlov, Dmitry I.; Samsonenko, Denis G.; Ermakova, Ekaterina A.; Klyushova, Lyubov S.; Baykov, Sergey V.; Boyarskiy, Vadim P.; Potapov, Andrei S.; Inorganics 9 (2021) 34–; doi:10.3390/inorganics9050034

data_1563173
_publ_section_title
;
 Synthesis and Structural Characterization of Half-Sandwich
 Arene--Ruthenium(II) Complexes with Bis(imidazol-1-yl)methane, Imidazole
 and Benzimidazole
;
_journal_issue                   5
_journal_name_full               Inorganics
_journal_page_first              34
_journal_paper_doi               10.3390/inorganics9050034
_journal_volume                  9
_journal_year                    2021
_chemical_formula_moiety         'C16 H22 Cl N4 Ru, Cl'
_chemical_formula_sum            'C16 H22 Cl2 N4 Ru'
_chemical_formula_weight         442.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-11-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.019(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3972(2)
_cell_length_b                   17.3629(3)
_cell_length_c                   12.9511(3)
_cell_measurement_reflns_used    6284
_cell_measurement_temperature    300.48(10)
_cell_measurement_theta_max      32.1080
_cell_measurement_theta_min      3.0790
_cell_volume                     2097.30(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      300.48(10)
_diffrn_detector_area_resol_mean 16.2096
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.882
_diffrn_measurement_details
;
  1 omega  -93.00  -11.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.4311  -57.0000 -120.0000 82

  2 omega  -90.00   35.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.4311    0.0000   60.0000 125

  3 omega   62.00  102.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       26.3686  178.0000   90.0000 40
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0142908000
_diffrn_orient_matrix_UB_12      0.0152020000
_diffrn_orient_matrix_UB_13      -0.0511038000
_diffrn_orient_matrix_UB_21      -0.0744686000
_diffrn_orient_matrix_UB_22      -0.0003488000
_diffrn_orient_matrix_UB_23      0.0041847000
_diffrn_orient_matrix_UB_31      0.0051202000
_diffrn_orient_matrix_UB_32      0.0379229000
_diffrn_orient_matrix_UB_33      0.0205146000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_unetI/netI     0.0372
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.882
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12806
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.882
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.427
_diffrn_reflns_theta_min         2.831
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.006
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.99283
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.768
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         6659
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0274
_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/[\s^2^(Fo^2^)+(0.0234P)^2^+0.6145P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0600
_refine_ls_wR_factor_ref         0.0624
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5747
_reflns_number_total             6659
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Comp1.cif
_cod_data_source_block           1ver0-13960_acd-20
_cod_database_code               1563173
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C16 H20 Cl1 N4 Ru1'
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C00L(H00M)
2.b Aromatic/amide H refined with riding coordinates:
 N006(H006), N007(H007), C008(H008), C00B(H00B), C00C(H00C), C00D(H00D),
 C00E(H00E), C00F(H00F), C00G(H00G), C00H(H00H), C00I(H00I), C00J(H00J)
2.c Idealised Me refined as rotating group:
 C00K(H00A,H00K,H00L), C00M(H00N,H00O,H00P), C00N(H00Q,H00R,H00S)
;
_shelx_res_checksum              40366
_shelx_hkl_checksum              87498
_shelx_fab_checksum              27172
_olex2_submission_special_instructions 'No special instructions were received'