Noninnocence of the deprotonated 1,2-bis((1<i>H</i>-pyrrol-2-yl)methylene)hydrazine bridge in diruthenium frameworks - a function of co-ligands.
Kumari, Maya; Bera, Sudip Kumar; Lahiri, Goutam Kumar; Dalton transactions (Cambridge, England : 2003) 50 (2021) 9891–9903; doi:10.1039/d1dt01488a

data_7707672
_publ_section_title
;
 Noninnocence of the deprotonated
 1,2-bis((1<i>H</i>-pyrrol-2-yl)methylene)hydrazine bridge in diruthenium
 frameworks - a function of co-ligands.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9891
_journal_page_last               9903
_journal_paper_doi               10.1039/d1dt01488a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C50 H40 N12 Ru2, 2(Cl O4), C H2 Cl2'
_chemical_formula_sum            'C51 H42 Cl4 N12 O8 Ru2'
_chemical_formula_weight         1294.90
_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_date             2019-11-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-04-26 deposited with the CCDC.	2021-06-14 downloaded from the CCDC.
;
_cell_angle_alpha                82.406(2)
_cell_angle_beta                 87.564(2)
_cell_angle_gamma                73.395(2)
_cell_formula_units_Z            2
_cell_length_a                   13.8250(3)
_cell_length_b                   14.1090(3)
_cell_length_c                   14.5097(3)
_cell_measurement_reflns_used    39045
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.2510
_cell_measurement_theta_min      2.0020
_cell_volume                     2688.37(10)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  25.00   1.00    8.00    --  -20.00   0.00 -36.00  135
  2  \w   -110.00  19.00   1.00    8.00    --  -20.00 -72.00 -36.00  129
  3  \w    -71.00  19.00   1.00    8.00    --  -20.00 -72.00 108.00   90
  4  \w    -39.00  19.00   1.00    8.00    --  -20.00 -72.00-180.00   58
  5  \w    -39.00  -9.00   1.00    8.00    --  -20.00 -72.00  36.00   30
  6  \w    -30.00   0.00   1.00    8.00    --  -20.00  72.00-108.00   30
  7  \w   -110.00  53.00   1.00    8.00    --  -20.00   0.00-180.00  163
  8  \w    -59.00  31.00   1.00    8.00    --  -20.00  72.00-180.00   90
  9  \w    -62.00  19.00   1.00    8.00    --  -20.00 -72.00-108.00   81
 10  \w    -44.00  -8.00   1.00    8.00    --  -20.00  72.00  36.00   36
 11  \w    -58.00  -4.00   1.00    8.00    --  -20.00  72.00 108.00   54
 12  \w    -79.00  44.00   1.00    8.00    --  -20.00   0.00-108.00  123
;
_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      -0.0470863000
_diffrn_orient_matrix_UB_12      0.0321902000
_diffrn_orient_matrix_UB_13      0.0120788000
_diffrn_orient_matrix_UB_21      0.0091052000
_diffrn_orient_matrix_UB_22      -0.0191081000
_diffrn_orient_matrix_UB_23      0.0475368000
_diffrn_orient_matrix_UB_31      0.0237995000
_diffrn_orient_matrix_UB_32      0.0373459000
_diffrn_orient_matrix_UB_33      0.0051582000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0567
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            52304
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.095
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.826
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87143
_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_colour            'metallic dark brown'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.600
_exptl_crystal_description       block
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.152
_exptl_crystal_size_mid          0.092
_exptl_crystal_size_min          0.056
_refine_diff_density_max         0.658
_refine_diff_density_min         -0.864
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     785
_refine_ls_number_reflns         9481
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0331
_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^)+(0.0349P)^2^+3.2672P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0757
_refine_ls_wR_factor_ref         0.0803
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8504
_reflns_number_total             9481
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01488a2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7707670--7707674.cif.'
_cod_database_code               7707672
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.955
_shelx_estimated_absorpt_t_min   0.885
_reflns_odcompleteness_completeness 91.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.07
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O8A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.002
Uanis(O3A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.002
Uanis(O2A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.002
Uanis(O9A) \\sim Ueq, Uanis(O9B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.002
3. Others
 Sof(Cl2)=Sof(Cl1B)=Sof(O2B)=Sof(O3B)=Sof(O4B)=Sof(O5B)=Sof(O6B)=Sof(O7B)=
 Sof(O8B)=Sof(O9B)=1-FVAR(1)
 Sof(O9A)=Sof(O7A)=Sof(O8A)=Sof(O2A)=Sof(Cl0A)=Sof(O4A)=Sof(O6A)=Sof(Cl1)=
 Sof(O3A)=Sof(O5A)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C51(H51A,H51B)
4.b Aromatic/amide H refined with riding coordinates:
 C41(H41), C42(H42), C31(H31), C12(H12), C14(H14), C50(H50), C32(H32), C6(H6),
 C40(H40), C9(H9), C43(H43), C8(H8), C11(H11), C5(H5), C13(H13), C49(H49),
 C10(H10), C34(H34), C17(H17), C33(H33), C20(H20), C19(H19), C44(H44), C18(H18),
  C21(H21), C3(H3), C39(H39), C47(H47), C1(H1), C48(H48), C30(H30), C37(H37),
 C38(H38), C2(H2), C22(H22), C23(H23), C29(H29), C24(H24), C28(H28), C27(H27)
;
_shelx_res_checksum              79899
_shelx_hkl_checksum              12387
_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 1.783
_oxdiff_exptl_absorpt_empirical_full_min 0.628