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_7714820
_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         'C90 H80 N4 O2 P4 Ru2, 2(Cl O4), 2(C H2 Cl2)'
_chemical_formula_sum            'C92 H84 Cl6 N4 O10 P4 Ru2'
_chemical_formula_weight         1944.35
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-10-25
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2023-10-25 deposited with the CCDC.	2023-12-21 downloaded from the CCDC.
;
_cell_angle_alpha                64.066(2)
_cell_angle_beta                 72.589(2)
_cell_angle_gamma                82.031(2)
_cell_formula_units_Z            1
_cell_length_a                   13.0632(3)
_cell_length_b                   13.3460(2)
_cell_length_c                   14.6777(2)
_cell_measurement_reflns_used    20688
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      28.7050
_cell_measurement_theta_min      1.7060
_cell_volume                     2195.72(8)
_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   -349.73  10.27   0.80    4.00   6.61  -9.84 -31.50    --   450
  2  \w    -60.89  -0.09   0.80    4.00    --  -14.77  94.56 -34.84   76
  3  \w    -65.46   0.14   0.80    4.00    --  -19.34  94.56 145.16   82
  4  \w   -100.81  15.19   0.80    4.00    --   -9.84 -59.25  20.08  145
  5  \w    -65.46   0.14   0.80    4.00    --  -19.34  94.56   1.16   82
  6  \f    -10.27 349.73   0.80    4.00  81.02  -9.84  31.50    --   450
  7  \w    -65.46   0.14   0.80    4.00    --  -19.34  94.56  73.16   82
  8  \w   -100.81  15.19   0.80    4.00    --   -9.84 -59.25 -51.92  145
  9  \f   -339.92  20.08   0.80    4.00  15.81  -9.84 -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      -0.0452316000
_diffrn_orient_matrix_UB_12      0.0066288000
_diffrn_orient_matrix_UB_13      -0.0194734000
_diffrn_orient_matrix_UB_21      -0.0062420000
_diffrn_orient_matrix_UB_22      -0.0586582000
_diffrn_orient_matrix_UB_23      0.0236051000
_diffrn_orient_matrix_UB_31      -0.0339647000
_diffrn_orient_matrix_UB_32      0.0028501000
_diffrn_orient_matrix_UB_33      0.0466309000
_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  0.0706
_diffrn_reflns_av_unetI/netI     0.0318
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            95504
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.601
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.660
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94375
_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 light yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_description       block
_exptl_crystal_F_000             994
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.293
_refine_diff_density_min         -1.293
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     536
_refine_ls_number_reflns         7746
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0473
_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^)+(0.0699P)^2^+3.5788P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1264
_refine_ls_wR_factor_ref         0.1335
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6786
_reflns_number_total             7746
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03730d2.cif
_cod_data_source_block           '[8](ClO4)2'
_cod_depositor_comments
'Adding full bibliography for 7714816--7714822.cif.'
_cod_database_code               7714820
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.968
_shelx_estimated_absorpt_t_min   0.943
_reflns_odcompleteness_completeness 79.34
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 H-Ru1
 1.519 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C7(H7A,H7B), C01N(H01A,H01B)
3.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C45(H45), C23(H23), C41(H41), C35(H35), C33(H33), C1(H1), C4(H4),
 C11(H11), C31(H31), C24(H24), C29(H29), C27(H27), C39(H39), C36(H36), C21(H21),
  C32(H32), C2(H2), C3(H3), C44(H44), C30(H30), C37(H37), C38(H38), C12(H12),
 C14(H14), C42(H42), C15(H15), C26(H26), C43(H43), C17(H17), C20(H20), C25(H25),
  C13(H13), C19(H19), C18(H18)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              36958
_shelx_fab_checksum              27463
_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 1.167
_oxdiff_exptl_absorpt_empirical_full_min 0.873