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_7226786
_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            'C53 H42 As2 Br Cl3 N2 O2 Ru'
_chemical_formula_weight         1176.05
_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
;
2016-02-08 deposited with the CCDC.
2016-09-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.039(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.2764(10)
_cell_length_b                   18.6423(12)
_cell_length_c                   17.4632(12)
_cell_measurement_reflns_used    6548
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.6
_cell_measurement_theta_min      2.8
_cell_volume                     4954.1(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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0551
_diffrn_reflns_av_unetI/netI     0.0519
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            42584
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.999
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         3.207
_diffrn_source                   'Sealed tube'
_exptl_absorpt_coefficient_mu    2.653
_exptl_absorpt_correction_T_max  0.59
_exptl_absorpt_correction_T_min  0.45
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 1999)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_description       block
_exptl_crystal_F_000             2344
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.116
_refine_diff_density_min         -0.873
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     688
_refine_ls_number_reflns         9672
_refine_ls_number_restraints     441
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.0487
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0761P)^2^+8.2596P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1282
_refine_ls_wR_factor_ref         0.1489
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7079
_reflns_number_total             9672
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra19044h2.cif
_cod_data_source_block           ts35
_cod_database_code               7226786
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.503
_shelx_estimated_absorpt_t_max   0.619
_shelx_res_checksum              53178