Synthesis and characterisation of cycloruthenated benzhydrazone complexes: catalytic application to selective oxidative cleavage of olefins to aldehydes
Manikandan, Thimma Sambamoorthy; Ramesh, Rengan; Semeril, David; RSC Adv. 6 (2016) 97107–; doi:10.1039/C6RA19044H

data_7226787
_publ_section_title
;
 Synthesis and characterisation of cycloruthenated benzhydrazone
 complexes: catalytic application to selective oxidative cleavage of
 olefins to aldehydes
;
_journal_issue                   99
_journal_name_full               'RSC Adv.'
_journal_page_first              97107
_journal_paper_doi               10.1039/C6RA19044H
_journal_volume                  6
_journal_year                    2016
_chemical_formula_sum            'C54 H45 As2 Cl3 N2 O3 Ru'
_chemical_formula_weight         1127.18
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-02-15 deposited with the CCDC.
2016-09-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.754(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.5853(10)
_cell_length_b                   18.6290(12)
_cell_length_c                   17.3913(11)
_cell_measurement_reflns_used    8924
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.2
_cell_measurement_theta_min      2.5
_cell_volume                     5023.9(6)
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004)'
_computing_molecular_graphics
'ORTEP3 (Farrugia, 1997) and Mercury (Bruno et al., 2002)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SIR92 (Altornare et al., 1993)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker axs kappa apex2 CCD Diffractometer'
_diffrn_measurement_method       '\w and \f scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_av_unetI/netI     0.0506
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            37848
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.148
_diffrn_source                   'Sealed tube'
_exptl_absorpt_coefficient_mu    1.823
_exptl_absorpt_correction_T_max  0.79
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 1999)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_description       block
_exptl_crystal_F_000             2272
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.886
_refine_diff_density_min         -1.460
_refine_diff_density_rms         0.152
_refine_ls_extinction_coef       0.0021(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     736
_refine_ls_number_reflns         8809
_refine_ls_number_restraints     718
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0882
_refine_ls_R_factor_gt           0.0567
_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^)+(0.1216P)^2^+3.1079P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1569
_refine_ls_wR_factor_ref         0.1937
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6241
_reflns_number_total             8809
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra19044h2.cif
_cod_data_source_block           TS34
_cod_database_code               7226787
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.611
_shelx_estimated_absorpt_t_max   0.712
_shelx_res_checksum              45543