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_7708706
_publ_section_title
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 Structural and electronic forms of doubly oxido/Pz and triply oxido/(Pz)2
 bridged mixed valent and isovalent diruthenium complexes (Pz=Pyrazolate)
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_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03076K
_journal_year                    2021
_chemical_formula_moiety         'C24 H30 N16 O Ru2'
_chemical_formula_sum            'C24 H30 N16 O Ru2'
_chemical_formula_weight         760.78
_space_group_crystal_system      tetragonal
_space_group_IT_number           110
_space_group_name_Hall           'I 4bw -2c'
_space_group_name_H-M_alt        'I 41 c d'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   29.6769(4)
_cell_length_b                   29.6769(4)
_cell_length_c                   15.2915(4)
_cell_measurement_reflns_used    13797
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.7740
_cell_measurement_theta_min      2.7430
_cell_volume                     13467.5(4)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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   -110.00  19.00   0.50    8.00    --  -20.00 -72.00-108.00  258
  2  \w    -47.00  70.00   0.50    8.00    --  -20.00  72.00-108.00  234
  3  \w    -30.00   0.00   0.50    8.00    --  -20.00   0.00-180.00   60
  4  \w    -30.00 -18.00   0.50    8.00    --  -20.00   0.00-180.00   24
;
_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      0.0099305000
_diffrn_orient_matrix_UB_12      0.0040042000
_diffrn_orient_matrix_UB_13      0.0414780000
_diffrn_orient_matrix_UB_21      -0.0072544000
_diffrn_orient_matrix_UB_22      -0.0215307000
_diffrn_orient_matrix_UB_23      0.0143863000
_diffrn_orient_matrix_UB_31      0.0205016000
_diffrn_orient_matrix_UB_32      -0.0095449000
_diffrn_orient_matrix_UB_33      -0.0150022000
_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  0.0786
_diffrn_reflns_av_unetI/netI     0.0522
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            35667
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.170
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.941
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72643
_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    1.497
_exptl_crystal_description       block
_exptl_crystal_F_000             6080
_exptl_crystal_size_max          0.102
_exptl_crystal_size_mid          0.088
_exptl_crystal_size_min          0.054
_refine_diff_density_max         3.259
_refine_diff_density_min         -1.391
_refine_diff_density_rms         0.217
_refine_ls_abs_structure_details
;
 Flack x determined using 1859 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.04(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         5912
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.0637
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0991P)^2^+25.0135P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1603
_refine_ls_wR_factor_ref         0.1745
_reflns_Friedel_coverage         0.920
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                4800
_reflns_number_total             5912
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03076k2.cif
_cod_data_source_block           3a
_cod_original_cell_volume        13467.5(5)
_cod_database_code               7708706
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.951
_shelx_estimated_absorpt_t_min   0.910
_reflns_odcompleteness_completeness 95.19
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.11
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N4) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(O1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(C23) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C2) \\sim
Ueq, Uanis(N7) \\sim Ueq, Uanis(N1) \\sim Ueq: with sigma of 0.001 and sigma
for terminal atoms of 0.001
Uanis(C10) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
3.a Aromatic/amide H refined with riding coordinates:
 N10(H10), N2(H2), N6(H6), C3(H3), C8(H8), C2(H2A), C5(H5), C12(H12), C18(H18),
  C14(H14), C6(H6A), C1(H1), C9(H9), C23(H23), N8(H8A), C20(H20), C13(H13),
 C7(H7), C17(H17), C4(H4), C15(H15), C11(H11), C22(H22), C21(H21), C24(H24),
 C16(H16), C10(H10A), C19(H19)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              19295
_shelx_hkl_checksum              72492
_shelx_fab_checksum              91568
_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 1.289
_oxdiff_exptl_absorpt_empirical_full_min 0.794