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_7714821
_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), 3(C H2 Cl2)'
_chemical_formula_sum            'C39 H52 Cl8 N4 O16 Ru2'
_chemical_formula_weight         1318.58
_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   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                 103.949(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.6627(3)
_cell_length_b                   36.9819(7)
_cell_length_c                   12.1433(3)
_cell_measurement_reflns_used    25127
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      22.6960
_cell_measurement_theta_min      1.6570
_cell_volume                     5518.9(2)
_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 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  \w   -100.81  15.39   0.70    2.00    --   -9.84 -59.25-123.92  166
  2  \f   -177.73   6.37   0.70    2.00   6.61  -9.84 -31.50    --   263
  3  \w   -100.81  15.39   0.70    2.00    --   -9.84 -59.25 -51.92  166
  4  \f   -138.46  93.94   0.70    2.00  81.02  -9.84  31.50    --   332
  5  \w   -100.81  15.39   0.70    2.00    --   -9.84 -59.25  20.08  166
;
_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      0.0529336000
_diffrn_orient_matrix_UB_12      0.0048649000
_diffrn_orient_matrix_UB_13      -0.0045792000
_diffrn_orient_matrix_UB_21      -0.0162929000
_diffrn_orient_matrix_UB_22      0.0183754000
_diffrn_orient_matrix_UB_23      -0.0071521000
_diffrn_orient_matrix_UB_31      0.0161792000
_diffrn_orient_matrix_UB_32      0.0025814000
_diffrn_orient_matrix_UB_33      0.0595971000
_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  0.0688
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            117314
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.657
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.999
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73297
_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    1.587
_exptl_crystal_description       block
_exptl_crystal_F_000             2664
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.961
_refine_diff_density_min         -0.569
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     630
_refine_ls_number_reflns         9712
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.0577
_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^)+(0.0863P)^2^+10.6439P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1558
_refine_ls_wR_factor_ref         0.1693
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7603
_reflns_number_total             9712
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03730d2.cif
_cod_data_source_block           '[4](ClO4)2'
_cod_depositor_comments
'Adding full bibliography for 7714816--7714822.cif.'
_cod_database_code               7714821
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.952
_shelx_estimated_absorpt_t_min   0.915
_reflns_odcompleteness_completeness 91.40
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     33.76
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H6(0.077) H24(0.088) H1(0.082) H7A(0.084) H7B(0.084) H19(0.089)
 H26A(0.137) H26B(0.137) H26C(0.137) H16(0.09) H3(0.115) H10A(0.099)
 H10B(0.099) H29(0.095) H11(0.086) H17A(0.133) H17B(0.133) H17C(0.133)
 H2(0.105) H4(0.1) H21A(0.139) H21B(0.139) H21C(0.139) H13(0.1) H34(0.106)
 H15(0.107) H31A(0.152) H31B(0.152) H31C(0.152) H38A(0.113) H38B(0.113)
 H27A(0.146) H27B(0.146) H27C(0.146) H14(0.108) H9A(0.116) H9B(0.116)
 H22A(0.153) H22B(0.153) H22C(0.153) H32A(0.181) H32B(0.181) H32C(0.181)
 H36A(0.177) H36B(0.177) H36C(0.177) H39A(0.186) H39B(0.186) H8A(0.144)
 H8B(0.144) H37A(0.226) H37B(0.226)
 Fixed X: H6(0.564485) H24(0.718867) H1(0.894992) H7A(0.409791) H7B(0.410192)
 H19(0.552089) H26A(0.919211) H26B(0.85429) H26C(0.826902) H16(0.260559)
 H3(0.940759) H10A(0.144621) H10B(0.260606) H29(-0.127906) H11(0.372245)
 H17A(0.356813) H17B(0.426404) H17C(0.446103) H2(1.010582) H4(0.754209)
 H21A(0.759087) H21B(0.640591) H21C(0.673015) H13(0.491543) H34(0.11323)
 H15(0.407089) H31A(-0.092187) H31B(-0.158054) H31C(-0.050658) H38A(0.318685)
 H38B(0.231766) H27A(-0.003737) H27B(-0.122412) H27C(-0.047142) H14(0.522512)
 H9A(0.233263) H9B(0.220601) H22A(0.50739) H22B(0.602388) H22C(0.615225)
 H32A(0.369913) H32B(0.279621) H32C(0.350465) H36A(-0.037243) H36B(-0.062601)
 H36C(-0.110979) H39A(0.227396) H39B(0.215173) H8A(0.393143) H8B(0.410708)
 H37A(0.823059) H37B(0.758338)
 Fixed Y: H6(0.70697) H24(0.539353) H1(0.621741) H7A(0.67884) H7B(0.636178)
 H19(0.544205) H26A(0.531645) H26B(0.508959) H26C(0.50362) H16(0.605695)
 H3(0.728526) H10A(0.684704) H10B(0.704202) H29(0.628933) H11(0.700967)
 H17A(0.536114) H17B(0.511746) H17C(0.508628) H2(0.670948) H4(0.737363)
 H21A(0.585609) H21B(0.576603) H21C(0.617475) H13(0.697004) H34(0.540473)
 H15(0.622146) H31A(0.708438) H31B(0.689535) H31C(0.712436) H38A(0.71252)
 H38B(0.681807) H27A(0.557719) H27B(0.569034) H27C(0.543634) H14(0.668313)
 H9A(0.663473) H9B(0.630856) H22A(0.591702) H22B(0.567914) H22C(0.610888)
 H32A(0.534507) H32B(0.511368) H32C(0.540672) H36A(0.598936) H36B(0.560229)
 H36C(0.596079) H39A(0.544486) H39B(0.529847) H8A(0.623658) H8B(0.665122)
 H37A(0.660706) H37B(0.698399)
 Fixed Z: H6(0.543108) H24(0.312195) H1(0.579375) H7A(0.552499) H7B(0.575676)
 H19(0.797661) H26A(0.544058) H26B(0.436756) H26C(0.557681) H16(-0.132623)
 H3(0.581594) H10A(0.262414) H10B(0.301314) H29(-0.164408) H11(0.184505)
 H17A(0.570549) H17B(0.671111) H17C(0.546139) H2(0.587887) H4(0.562288)
 H21A(0.933347) H21B(0.950833) H21C(0.930746) H13(0.035993) H34(0.265438) H15(-
 0.208169) H31A(-0.033443) H31B(-0.148032) H31C(-0.147316) H38A(0.715882)
 H38B(0.664501) H27A(-0.227677) H27B(-0.215607) H27C(-0.121976) H14(-0.121704)
 H9A(0.44189) H9B(0.352864) H22A(0.19131) H22B(0.161554) H22C(0.173205)
 H32A(0.209876) H32B(0.250836) H32C(0.333938) H36A(0.328523) H36B(0.269103)
 H36C(0.201711) H39A(0.957608) H39B(0.831154) H8A(0.387186) H8B(0.359814)
 H37A(0.305384) H37B(0.288814)
;
_shelx_res_checksum              9276
_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 1.347
_oxdiff_exptl_absorpt_empirical_full_min 0.653