Structural and electronic forms of doubly oxido/Pz and triply oxido/(Pz)2 bridged mixed valent and isovalent diruthenium complexes (Pz=Pyrazolate)
Lahiri, Goutam Kumar; Bera, Sudip Kumar; Dalton Transactions  (2021) –; doi:10.1039/D1DT03076K

data_7708699
_publ_section_title
;
 Structural and electronic forms of doubly oxido/Pz and triply oxido/(Pz)2
 bridged mixed valent and isovalent diruthenium complexes (Pz=Pyrazolate)
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03076K
_journal_year                    2021
_chemical_formula_moiety         'C23 H31 N2 O9 Ru2'
_chemical_formula_sum            'C23 H31 N2 O9 Ru2'
_chemical_formula_weight         681.64
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-07-03
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-07-25 deposited with the CCDC.	2021-11-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.249(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   30.4609(5)
_cell_length_b                   8.14030(10)
_cell_length_c                   23.6002(4)
_cell_measurement_reflns_used    8446
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.5830
_cell_measurement_theta_min      3.0520
_cell_volume                     5524.77(16)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -191.00 -11.00   1.00    1.00    -- -101.00   0.00 108.00  180
  2  \w   -122.00  -8.00   1.00    1.00    --  -32.00 -72.00 -36.00  114
  3  \w   -135.00 -13.00   1.00    1.00    -- -101.00  72.00 108.00  122
  4  \w   -135.00 -15.00   1.00    1.00    -- -101.00  72.00-180.00  120
  5  \w    -53.00  35.00   1.00    1.00    --  -32.00   0.00 108.00   88
  6  \w    -96.00 -17.00   1.00    1.00    -- -101.00  72.00-108.00   79
  7  \w    -44.00 -14.00   1.00    1.00    -- -101.00  72.00 -36.00   30
  8  \w   -191.00-161.00   1.00    1.00    -- -101.00 -72.00-108.00   30
  9  \w   -191.00-125.00   1.00    1.00    -- -101.00 -72.00  36.00   66
 10  \w    -97.00 -67.00   1.00    1.00    -- -101.00 -72.00 -36.00   30
 11  \w   -135.00-105.00   1.00    1.00    -- -101.00  72.00  36.00   30
 12  \w   -191.00 -58.00   1.00    1.00    -- -101.00   0.00-180.00  133
 13  \w   -191.00 -69.00   1.00    1.00    -- -101.00 -72.00-180.00  122
 14  \w    -96.00 -48.00   1.00    1.00    --  -32.00   0.00  36.00   48
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0440007000
_diffrn_orient_matrix_UB_12      -0.0853562000
_diffrn_orient_matrix_UB_13      0.0415569000
_diffrn_orient_matrix_UB_21      -0.0191558000
_diffrn_orient_matrix_UB_22      0.0134989000
_diffrn_orient_matrix_UB_23      0.0526511000
_diffrn_orient_matrix_UB_31      -0.0237923000
_diffrn_orient_matrix_UB_32      -0.1683433000
_diffrn_orient_matrix_UB_33      -0.0168243000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1051
_diffrn_reflns_av_unetI/netI     0.0750
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            20899
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        64.997
_diffrn_reflns_theta_max         64.997
_diffrn_reflns_theta_min         3.073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.292
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21744
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.639
_exptl_crystal_description       block
_exptl_crystal_F_000             2744
_exptl_crystal_size_max          0.365
_exptl_crystal_size_mid          0.325
_exptl_crystal_size_min          0.102
_refine_diff_density_max         1.859
_refine_diff_density_min         -0.965
_refine_diff_density_rms         0.226
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         4693
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0572
_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/[\s^2^(Fo^2^)+(0.0972P)^2^+9.3906P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1478
_refine_ls_wR_factor_ref         0.1622
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3976
_reflns_number_total             4693
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03076k2.cif
_cod_data_source_block           1a
_cod_database_code               7708699
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 97.55
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     72.66
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C3(H3), C8(H8), C22(H22), C23(H23), C18(H18), C21(H21)
2.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C1(H1A,H1B,H1C), C20(H20A,H20B,H20C), C11(H11A,H11B,
 H11C), C15(H15A,H15B,H15C), C6(H6A,H6B,H6C), C5(H5A,H5B,H5C), C16(H16A,H16B,
 H16C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              20731
_shelx_hkl_checksum              46244
_shelx_fab_checksum              95790
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.676
_oxdiff_exptl_absorpt_empirical_full_min 0.389