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_7714818
_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         'C36 H46 N4 O8 Ru2, 2(Cl O4), 4(C H Cl3)'
_chemical_formula_sum            'C40 H50 Cl14 N4 O16 Ru2'
_chemical_formula_weight         1541.28
_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     dual
_audit_creation_date             2023-08-23
_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                 97.806(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.5574(6)
_cell_length_b                   13.0011(3)
_cell_length_c                   21.5012(6)
_cell_measurement_reflns_used    9652
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      23.7240
_cell_measurement_theta_min      1.8100
_cell_volume                     6247.2(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_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   -106.56 101.94   0.50    2.00  81.02  -9.84  31.50    --   417
  2  \f   -161.73  22.77   0.50    2.00   6.61  -9.84 -31.50    --   369
  3  \w   -100.81  15.69   0.50    2.00    --   -9.84 -59.25-123.92  233
  4  \w   -100.81  15.69   0.50    2.00    --   -9.84 -59.25 -51.92  233
;
_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      0.0105584000
_diffrn_orient_matrix_UB_12      0.0041500000
_diffrn_orient_matrix_UB_13      -0.0294872000
_diffrn_orient_matrix_UB_21      0.0156719000
_diffrn_orient_matrix_UB_22      -0.0470633000
_diffrn_orient_matrix_UB_23      0.0057041000
_diffrn_orient_matrix_UB_31      -0.0255019000
_diffrn_orient_matrix_UB_32      -0.0272971000
_diffrn_orient_matrix_UB_33      -0.0143721000
_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  0.0676
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            52427
_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         1.812
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.144
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21928
_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 green'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.639
_exptl_crystal_description       block
_exptl_crystal_F_000             3088
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.544
_refine_diff_density_min         -0.939
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         5509
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0836
_refine_ls_R_factor_gt           0.0697
_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^)+(0.0865P)^2^+77.8670P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1819
_refine_ls_wR_factor_ref         0.1912
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4581
_reflns_number_total             5509
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03730d2.cif
_cod_data_source_block           '[5](ClO4)2'
_cod_depositor_comments
'Adding full bibliography for 7714816--7714822.cif.'
_cod_database_code               7714818
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.945
_shelx_estimated_absorpt_t_min   0.904
_reflns_odcompleteness_completeness 89.32
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     33.75
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H8A(0.04) H8B(0.04) H7A(0.042) H7B(0.042) H4(0.051) H1(0.046)
 H13A(0.074) H13B(0.074) H13C(0.074) H3(0.059) H6(0.041) H2(0.059) H14A(0.086)
 H14B(0.086) H14C(0.086) H11(0.069) H19(0.08) H20(0.088) H16(0.08) H9A(0.117)
 H9B(0.117) H9C(0.117) H18A(0.182) H18B(0.182) H18C(0.182)
 Fixed X: H8A(0.485421) H8B(0.491335) H7A(0.578408) H7B(0.589364) H4(0.728617)
 H1(0.671857) H13A(0.439424) H13B(0.399493) H13C(0.45313) H3(0.768133)
 H6(0.652694) H2(0.736903) H14A(0.695286) H14B(0.724618) H14C(0.749495)
 H11(0.414747) H19(0.693501) H20(0.627332) H16(0.661936) H9A(0.479435)
 H9B(0.416385) H9C(0.443951) H18A(0.635964) H18B(0.612069) H18C(0.566778)
 Fixed Y: H8A(0.56556) H8B(0.603877) H7A(0.645693) H7B(0.526228) H4(0.357175)
 H1(0.607212) H13A(0.548106) H13B(0.542684) H13C(0.462811) H3(0.353972)
 H6(0.444742) H2(0.477266) H14A(0.921721) H14B(0.964361) H14C(0.860925)
 H11(0.707759) H19(0.154101) H20(0.200123) H16(0.957237) H9A(0.903475)
 H9B(0.84632) H9C(0.908579) H18A(0.86328) H18B(0.963035) H18C(0.87214)
 Fixed Z: H8A(0.548908) H8B(0.479416) H7A(0.54947) H7B(0.565398) H4(0.443736)
 H1(0.293127) H13A(0.256699) H13B(0.312705) H13C(0.31039) H3(0.348309)
 H6(0.510898) H2(0.271583) H14A(0.516856) H14B(0.458222) H14C(0.492742)
 H11(0.345904) H19(0.219011) H20(0.347528) H16(0.370692) H9A(0.450052)
 H9B(0.433951) H9C(0.38042) H18A(0.232064) H18B(0.264502) H18C(0.240641)
;
_shelx_res_checksum              87976
_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 2.555
_oxdiff_exptl_absorpt_empirical_full_min 0.368