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_7714816
_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 H42 N4 O8 Ru2, 2(Cl O4), 2(C H2 Cl2)'
_chemical_formula_sum            'C36 H46 Cl6 N4 O16 Ru2'
_chemical_formula_weight         1205.61
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-10-17
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2023-10-17 deposited with the CCDC.	2023-12-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.810(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.9403(5)
_cell_length_b                   12.6420(2)
_cell_length_c                   22.9581(7)
_cell_measurement_reflns_used    13879
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      31.2990
_cell_measurement_theta_min      1.9510
_cell_volume                     4726.3(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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.855
_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   -100.21 132.59   0.80    4.00  15.81  -9.84 -59.25    --   291
  2  \w   -100.81  15.19   0.80    4.00    --   -9.84 -59.25 -51.92  145
  3  \w   -100.81  15.19   0.80    4.00    --   -9.84 -59.25  92.08  145
  4  \w   -100.81  15.19   0.80    4.00    --   -9.84 -59.25  20.08  145
  5  \w   -100.81  15.19   0.80    4.00    --   -9.84 -59.25 164.08  145
;
_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      0.0038929000
_diffrn_orient_matrix_UB_12      -0.0550362000
_diffrn_orient_matrix_UB_13      0.0065794000
_diffrn_orient_matrix_UB_21      0.0245705500
_diffrn_orient_matrix_UB_22      0.0107353500
_diffrn_orient_matrix_UB_23      0.0328273000
_diffrn_orient_matrix_UB_31      -0.0357928500
_diffrn_orient_matrix_UB_32      0.0014569500
_diffrn_orient_matrix_UB_33      0.0059250000
_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  0.0564
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.855
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            67540
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.855
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.786
_diffrn_reflns_theta_min         1.954
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.049
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81347
_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 dark brown'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.694
_exptl_crystal_description       block
_exptl_crystal_F_000             2432
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.105
_refine_diff_density_min         -0.833
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         8096
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0413
_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^)+(0.0296P)^2^+15.4248P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0841
_refine_ls_wR_factor_ref         0.0933
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6301
_reflns_number_total             8096
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03730d2.cif
_cod_data_source_block           '[2](ClO4)2_autored'
_cod_depositor_comments
'Adding full bibliography for 7714816--7714822.cif.'
_cod_database_code               7714816
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 85.58
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     33.71
_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:
 C7(H7A,H7B), C18(H18A,H18B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C2(H2), C3(H3), C4(H4), C1(H1), C15(H15), C10(H10)
2.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C8(H8A,H8B,H8C), C17(H17A,H17B,H17C), C13(H13A,H13B,H13C)
;
_shelx_res_checksum              91760
_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 1.450
_oxdiff_exptl_absorpt_empirical_full_min 0.799