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_7707674
_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         'C34 H44 N4 O8 Ru2'
_chemical_formula_sum            'C34 H44 N4 O8 Ru2'
_chemical_formula_weight         838.36
_chemical_name_systematic        MK-AC-PZM
_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     dual
_audit_creation_date             2021-04-11
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2021-04-26 deposited with the CCDC.	2021-06-14 downloaded from the CCDC.
;
_cell_angle_alpha                88.880(6)
_cell_angle_beta                 78.068(6)
_cell_angle_gamma                84.835(6)
_cell_formula_units_Z            4
_cell_length_a                   12.6118(9)
_cell_length_b                   15.1919(12)
_cell_length_c                   22.0273(17)
_cell_measurement_reflns_used    5395
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.7350
_cell_measurement_theta_min      1.9200
_cell_volume                     4112.4(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(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  \f   -349.73   9.27   1.00    2.00   6.61  -9.84 -31.50    --   359
  2  \w    -68.10 -13.10   1.00    2.00    --   -9.90 114.93 127.10   55
  3  \w    -52.01  18.99   1.00    2.00    --   -9.90  87.17 -19.38   71
  4  \w   -100.81  15.19   1.00    2.00    --   -9.84 -59.25 164.08  116
  5  \w    -57.77  -2.77   1.00    2.00    --   -9.90  97.85-146.28   55
  6  \f    -10.27 348.73   1.00    2.00  81.02  -9.84  31.50    --   359
  7  \w    -52.01  17.99   1.00    2.00    --   -9.90  87.22 -92.14   70
  8  \w   -100.81  15.19   1.00    2.00    --   -9.84 -59.25 -51.92  116
  9  \f   -339.92  19.08   1.00    2.00  15.81  -9.84 -59.25    --   359
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0492456000
_diffrn_orient_matrix_UB_12      -0.0030762000
_diffrn_orient_matrix_UB_13      -0.0225711000
_diffrn_orient_matrix_UB_21      -0.0138092000
_diffrn_orient_matrix_UB_22      0.0427971000
_diffrn_orient_matrix_UB_23      -0.0110378000
_diffrn_orient_matrix_UB_31      0.0267247000
_diffrn_orient_matrix_UB_32      0.0188852000
_diffrn_orient_matrix_UB_33      0.0212584000
_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  0.3756
_diffrn_reflns_av_unetI/netI     0.1535
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            180369
_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         1.645
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.782
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40949
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic reddish brown'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_description       needle
_exptl_crystal_F_000             1710
_exptl_crystal_size_max          0.021
_exptl_crystal_size_mid          0.005
_exptl_crystal_size_min          0.004
_refine_diff_density_max         0.914
_refine_diff_density_min         -0.877
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.948
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     889
_refine_ls_number_reflns         14450
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.948
_refine_ls_R_factor_all          0.1320
_refine_ls_R_factor_gt           0.0668
_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^)+(0.0545P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1421
_refine_ls_wR_factor_ref         0.1715
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7796
_reflns_number_total             14450
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01488a2.cif
_cod_data_source_block           1b
_cod_depositor_comments
;
Adding full bibliography for 7707670--7707674.cif.

2024-09-23
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C68 H87 N8 O16 Ru4'
_cod_original_formula_weight         1676.73
_cod_original_formula_moiety         'C34 H45 N4 O8 Ru2, C34 H42 N4 O8 Ru2'
_cod_original_formula_units_Z            2
_cod_database_code               7707674
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.997
_shelx_estimated_absorpt_t_min   0.984
_reflns_odcompleteness_completeness 90.16
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     33.83
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C39(H39), C40(H40), C61(H61), C2(H2), C36(H36), C32(H32),
 C17(H17), C43(H43), C22(H22), C51(H51), C27(H27)
2.c Idealised Me refined as rotating group:
 C64(H64A,H64B,H64C), C11(H11A,H11B,H11C), C20(H20A,H20B,H20C), C34(H34A,H34B,
 H34C), C12(H12A,H12B,H12C), C59(H59A,H59B,H59C), C14(H14A,H14B,H14C), C68(H68A,
 H68B,H68C), C48(H48A,H48B,H48C), C46(H46A,H46B,H46C), C54(H54A,H54B,H54C),
 C47(H47A,H47B,H47C), C15(H15A,H15B,H15C), C19(H19A,H19B,H19C), C63(H63A,H63B,
 H63C), C49(H49A,H49B,H49C), C13(H13A,H13B,H13C), C45(H45A,H45B,H45C), C24(H24A,
 H24B,H24C), C53(H53A,H53B,H53C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C),
 C25(H25A,H25B,H25C), C58(H58A,H58B,H58C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              10489
_shelx_hkl_checksum              50281
_shelx_fab_checksum              89318
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 4.452
_oxdiff_exptl_absorpt_empirical_full_min 0.480