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_7707673
_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
'C52.76 H42.76 N16 Ru2, Cl O3.91, Cl O4, C H4 O'
_chemical_formula_sum            'C53.75 H46.75 Cl2 N16 O8.92 Ru2'
_chemical_formula_weight         1332.58
_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
_atom_sites_solution_primary     iterative
_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                82.3750(18)
_cell_angle_beta                 80.6850(18)
_cell_angle_gamma                85.8215(18)
_cell_formula_units_Z            2
_cell_length_a                   11.3064(2)
_cell_length_b                   12.8799(3)
_cell_length_c                   20.0088(4)
_cell_measurement_reflns_used    35253
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.0330
_cell_measurement_theta_min      1.8910
_cell_volume                     2846.00(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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -38.00  15.00   1.00    8.00    --  -20.00 -72.00-180.00   53
  5  \w    -25.00   5.00   1.00    8.00    --  -20.00  72.00-108.00   30
  6  \w    -39.00  -9.00   1.00    8.00    --  -20.00 -72.00  36.00   30
  7  \w   -110.00  25.00   1.00    8.00    --  -20.00   0.00 108.00  135
  8  \w    -87.00  19.00   1.00    8.00    --  -20.00 -72.00-108.00  106
  9  \w    -59.00  36.00   1.00    8.00    --  -20.00  72.00 108.00   95
 10  \w    -58.00   4.00   1.00    8.00    --  -20.00  72.00-180.00   62
 11  \w    -44.00  -8.00   1.00    8.00    --  -20.00  72.00  36.00   36
 12  \w   -110.00 -46.00   1.00    8.00    --  -20.00   0.00  36.00   64
;
_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      0.0184147000
_diffrn_orient_matrix_UB_12      0.0246263000
_diffrn_orient_matrix_UB_13      -0.0335769000
_diffrn_orient_matrix_UB_21      -0.0312404000
_diffrn_orient_matrix_UB_22      -0.0364979000
_diffrn_orient_matrix_UB_23      -0.0132167000
_diffrn_orient_matrix_UB_31      -0.0523224000
_diffrn_orient_matrix_UB_32      0.0340157000
_diffrn_orient_matrix_UB_33      0.0028547000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0615
_diffrn_reflns_av_unetI/netI     0.0386
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            52111
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.382
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.695
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96613
_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    1.555
_exptl_crystal_description       block
_exptl_crystal_F_000             1349
_exptl_crystal_size_max          0.102
_exptl_crystal_size_mid          0.088
_exptl_crystal_size_min          0.064
_refine_diff_density_max         2.819
_refine_diff_density_min         -1.169
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     772
_refine_ls_number_reflns         10012
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0599
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0745P)^2^+18.1424P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1521
_refine_ls_wR_factor_ref         0.1593
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8886
_reflns_number_total             10012
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01488a2.cif
_cod_data_source_block           3b
_cod_depositor_comments
'Adding full bibliography for 7707670--7707674.cif.'
_cod_original_cell_volume        2846.00(11)
_cod_database_code               7707673
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.957
_shelx_estimated_absorpt_t_min   0.933
_reflns_odcompleteness_completeness 91.55
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.12
_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, All O(H) groups
2. Rigid bond restraints
 C24, C26, C27
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C24 \\sim C26 \\sim C27: within 1.7A with sigma of 0.05 and sigma for terminal
atoms of 0.05
Uanis(C24) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.001
Uanis(C23) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.002
Uanis(O8) \\sim Ueq, Uanis(O6) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.002
Uanis(O1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.002
Uanis(C25) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.002
Uanis(C26) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C23)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.001
Uanis(C19) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C21) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.002
Uanis(O6) \\sim Ueq, Uanis(O8) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.002
4. Others
 Sof(C23)=Sof(H23)=Sof(C25)=Sof(H25)=FVAR(1)
 Sof(C27)=Sof(H27)=Sof(C24)=Sof(H24)=Sof(C26)=Sof(H26)=FVAR(2)
 Sof(O2B)=1-FVAR(3)
 Sof(O2A)=FVAR(3)
5.a Aromatic/amide H refined with riding coordinates:
 C31(H31), C3(H3), C5(H5), C29(H29), C32(H32), C30(H30), C9(H9), C10(H10),
 C55(H55), C6(H6), C16(H16), C37(H37), C13(H13), C52(H52), C8(H8), C2(H2),
 C42(H42), C15(H15), C54(H54), C35(H35), C36(H36), C14(H14), C1(H1), C38(H38),
 C34(H34), C53(H53), C41(H41), C46(H46), C12(H12), C49(H49), C50(H50), C43(H43),
  C18(H18), C47(H47), C40(H40), C20(H20), C19(H19), C21(H21), C48(H48),
 C23(H23), C25(H25), C27(H27), C24(H24), C26(H26)
5.b Idealised Me refined as rotating group:
 C56(H56A,H56B,H56C)
5.c Idealised tetrahedral OH refined as rotating group:
 O9(H9A)
;
_shelx_res_checksum              73516
_shelx_hkl_checksum              78968
_shelx_fab_checksum              22297
_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 1.778
_oxdiff_exptl_absorpt_empirical_full_min 0.733