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_7714822
_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         'C89 H78 N4 O2 P4 Ru2, 2(Cl O4)'
_chemical_formula_sum            'C89 H78 Cl2 N4 O10 P4 Ru2'
_chemical_formula_weight         1760.47
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-10-18
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2023-10-23 deposited with the CCDC.	2023-12-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.558(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3963(3)
_cell_length_b                   21.3283(5)
_cell_length_c                   27.8750(6)
_cell_measurement_reflns_used    18476
_cell_measurement_temperature    273(30)
_cell_measurement_theta_max      25.9060
_cell_measurement_theta_min      1.7110
_cell_volume                     8555.8(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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      273.15
_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    -17.73 165.87   0.60    8.00   6.61  -9.84 -31.50    --   306
  2  \w   -100.81  15.59   0.60    8.00    --   -9.84 -59.25  20.08  194
  3  \w    -65.46  -0.06   0.60    8.00    --  -19.34  94.56 145.16  109
  4  \w   -100.81  15.59   0.60    8.00    --   -9.84 -59.25 -51.92  194
  5  \f   -150.07  65.33   0.60    8.00  81.02  -9.84  31.50    --   359
  6  \w    -60.89   0.31   0.60    8.00    --  -14.77  94.56 -34.84  102
  7  \w   -100.81  15.59   0.60    8.00    --   -9.84 -59.25  92.08  194
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0872
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            203800
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.707
_exptl_absorpt_coefficient_mu    0.549
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17466
_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            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_description       block
_exptl_crystal_F_000             3608
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.104
_refine_diff_density_min         -0.883
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1006
_refine_ls_number_reflns         15054
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0722
_refine_ls_R_factor_gt           0.0563
_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^)+(0.0730P)^2^+19.9573P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1501
_refine_ls_wR_factor_ref         0.1618
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11756
_reflns_number_total             15054
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03730d2.cif
_cod_data_source_block           '[7](clo4)2'
_cod_depositor_comments
'Adding full bibliography for 7714816--7714822.cif.'
_cod_database_code               7714822
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.978
_shelx_estimated_absorpt_t_min   0.952
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H) groups
2. Restrained distances
 H-Ru2
 1.51 with sigma of 0.02
 HA-Ru1
 1.51 with sigma of 0.02
 Ru2-H
 1.51 with sigma of 0.02
 Ru1-HA
 1.51 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O3) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O5) \\sim
Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(Cl1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(O6) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O5) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.002
4.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C7(H7A,H7B), C8(H8A,H8B)
4.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C29(H29), C28(H28), C77(H77), C55(H55), C79(H79), C53(H53), C21(H21),
 C2(H2), C43(H43), C10(H10), C74(H74), C3(H3), C71(H71), C37(H37), C4(H4),
 C25(H25), C1(H1), C73(H73), C23(H23), C85(H85), C22(H22), C15(H15), C49(H49),
 C46(H46), C89(H89), C50(H50), C56(H56), C19(H19), C80(H80), C83(H83), C75(H75),
  C38(H38), C67(H67), C12(H12), C76(H76), C45(H45), C65(H65), C47(H47),
 C51(H51), C61(H61), C14(H14), C41(H41), C13(H13), C63(H63), C20(H20), C27(H27),
  C70(H70), C64(H64), C52(H52), C81(H81), C34(H34), C59(H59), C68(H68),
 C35(H35), C33(H33), C82(H82), C31(H31), C26(H26), C57(H57), C58(H58), C86(H86),
  C69(H69), C44(H44), C39(H39), C87(H87), C88(H88), C32(H32), C62(H62), C40(H40)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              12365
_shelx_fab_checksum              86051
_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
;