Metal-ligand synergy driven functionalisation of alkylene linked bis(aldimine) on a diruthenium(II) platform. Cyclisation <i>versus</i> oxygenation.
Biswas, Mitrali; Dey, Sanchaita; Dhara, Suman; Panda, Sanjib; Lahiri, Goutam Kumar; Dalton transactions (Cambridge, England : 2003) 53 (2024) 2167–2180; doi:10.1039/d3dt03730d

data_7714819
_publ_section_title
;
 Metal-ligand synergy driven functionalisation of alkylene linked
 bis(aldimine) on a diruthenium(II) platform. Cyclisation <i>versus</i>
 oxygenation.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2167
_journal_page_last               2180
_journal_paper_doi               10.1039/d3dt03730d
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C34 H40 N4 O10 Ru2'
_chemical_formula_sum            'C34 H40 N4 O10 Ru2'
_chemical_formula_weight         866.84
_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             2023-10-24
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2023-10-24 deposited with the CCDC.	2023-12-21 downloaded from the CCDC.
;
_cell_angle_alpha                72.100(8)
_cell_angle_beta                 69.913(8)
_cell_angle_gamma                81.135(7)
_cell_formula_units_Z            2
_cell_length_a                   12.5742(10)
_cell_length_b                   12.8511(11)
_cell_length_c                   13.6116(12)
_cell_measurement_reflns_used    10900
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      22.6700
_cell_measurement_theta_min      1.9760
_cell_volume                     1962.8(3)
_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 (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_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  10.27   0.80    4.00  11.09 -11.30 -31.50    --   450
  2  \w    -66.45  -0.05   0.80    4.00    --  -16.95  94.56 -34.84   83
  3  \w   -106.96  17.04   0.80    4.00    --  -11.30 -59.25 -51.92  155
  4  \w    -64.58   0.22   0.80    4.00    --  -15.09  94.56 145.16   81
  5  \f    -10.27 349.73   0.80    4.00  79.56 -11.30  31.50    --   450
  6  \w    -64.58   0.22   0.80    4.00    --  -15.09  94.56   1.16   81
  7  \w    -64.58   0.22   0.80    4.00    --  -15.09  94.56  73.16   81
  8  \w   -106.96  17.04   0.80    4.00    --  -11.30 -59.25 164.08  155
  9  \f   -339.92  20.08   0.80    4.00  17.79 -11.30 -59.25    --   450
;
_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      -0.0597788000
_diffrn_orient_matrix_UB_12      -0.0027688000
_diffrn_orient_matrix_UB_13      0.0220947000
_diffrn_orient_matrix_UB_21      -0.0002247000
_diffrn_orient_matrix_UB_22      0.0250572000
_diffrn_orient_matrix_UB_23      0.0398009000
_diffrn_orient_matrix_UB_31      -0.0066817000
_diffrn_orient_matrix_UB_32      0.0523317000
_diffrn_orient_matrix_UB_33      -0.0354481000
_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  0.1484
_diffrn_reflns_av_unetI/netI     0.0611
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            79306
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.656
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.825
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52090
_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 orangish orange'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_description       block
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.075
_refine_diff_density_min         -0.637
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     459
_refine_ls_number_reflns         6910
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0906
_refine_ls_R_factor_gt           0.0677
_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^)+(0.0815P)^2^+7.2215P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1683
_refine_ls_wR_factor_ref         0.1878
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5005
_reflns_number_total             6910
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03730d2.cif
_cod_data_source_block           2a
_cod_depositor_comments
'Adding full bibliography for 7714816--7714822.cif.'
_cod_database_code               7714819
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.886
_shelx_estimated_absorpt_t_min   0.846
_reflns_odcompleteness_completeness 82.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     34.71
_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:
 C8(H8A,H8B), C7(H7A,H7B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C14(H14), C11(H11), C4(H4), C27(H27), C17(H17), C13(H13), C2(H2),
 C12(H12), C22(H22), C32(H32), C3(H3)
2.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C25(H25A,H25B,H25C), C34(H34A,H34B,H34C), C30(H30A,H30B,
 H30C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C29(H29A,H29B,H29C), C24(H24A,
 H24B,H24C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              38403
_shelx_fab_checksum              62488
_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 1.664
_oxdiff_exptl_absorpt_empirical_full_min 0.660