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_7708705
_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         'C24 H33 N2 O9 Ru2'
_chemical_formula_sum            'C24 H33 N2 O9 Ru2'
_chemical_formula_weight         695.66
_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             2021-07-08
_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                 105.161(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.0077(16)
_cell_length_b                   8.1608(3)
_cell_length_c                   23.5756(12)
_cell_measurement_reflns_used    6316
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      29.8250
_cell_measurement_theta_min      2.5700
_cell_volume                     5758.1(5)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f    -25.75 154.25   1.00    2.00 -25.75   0.00  73.76    --   180
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0082044000
_diffrn_orient_matrix_UB_12      -0.0068803000
_diffrn_orient_matrix_UB_13      -0.0309463000
_diffrn_orient_matrix_UB_21      0.0197481500
_diffrn_orient_matrix_UB_22      -0.0421156500
_diffrn_orient_matrix_UB_23      -0.0012522000
_diffrn_orient_matrix_UB_31      -0.0102287000
_diffrn_orient_matrix_UB_32      -0.0756989000
_diffrn_orient_matrix_UB_33      0.0035102000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            15861
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.201
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.099
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92864
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic pinkish pink'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   pinkish
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_description       block
_exptl_crystal_F_000             2808
_exptl_crystal_size_max          0.205
_exptl_crystal_size_mid          0.156
_exptl_crystal_size_min          0.089
_refine_diff_density_max         1.416
_refine_diff_density_min         -0.420
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         5024
_refine_ls_number_restraints     318
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0318
_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^)+(0.0401P)^2^+14.5084P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0808
_refine_ls_wR_factor_ref         0.0836
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4494
_reflns_number_total             5024
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03076k2.cif
_cod_data_source_block           1b
_cod_database_code               7708705
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.909
_shelx_estimated_absorpt_t_min   0.806
_reflns_odcompleteness_completeness 83.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.64
_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. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 1.7A
Uanis(C23) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C24) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C22) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C18(H18), C21(H21), C8(H8), C22(H22), C3(H3)
4.b Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C16(H16A,H16B,H16C), C5(H5A,H5B,H5C), C20(H20A,H20B,
 H20C), C15(H15A,H15B,H15C), C10(H10A,H10B,H10C), C1(H1A,H1B,H1C), C6(H6A,H6B,
 H6C), C24(H24A,H24B,H24C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              96463
_shelx_hkl_checksum              26226
_shelx_fab_checksum              40623
_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 1.116
_oxdiff_exptl_absorpt_empirical_full_min 0.896