Reaction of sodium 2-(2-(2,4-dioxopentan-3-ylidene)hydrazinyl) benzenesulfonate with ethylenediamine on Cu(II) and Ni(II) centres: efficient Cu(II) homogeneous catalysts for cyanosilylation of aldehydes
Mahmoud, Abdallah G.; Mahmudov, Kamran T.; Guedes da Silva, M. Fátima C.; Pombeiro, Armando J. L.; RSC Adv.  (2016) –; doi:10.1039/C6RA12274D

data_7225404
_publ_section_title
;
 Reaction of sodium 2-(2-(2,4-dioxopentan-3-ylidene)hydrazinyl)
 benzenesulfonate with ethylenediamine on Cu(II) and Ni(II) centres:
 efficient Cu(II) homogeneous catalysts for cyanosilylation of aldehydes
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA12274D
_journal_year                    2016
_chemical_formula_moiety
'2(C11 H11 N2 O5 S), C6 H24 N6 Ni, C2 H6 O, 6(H2 O)'
_chemical_formula_sum            'C30 H64 N10 Ni O17 S2'
_chemical_formula_weight         959.74
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-05-30 deposited with the CCDC.
2016-05-31 downloaded from the CCDC.
;
_cell_angle_alpha                72.171(3)
_cell_angle_beta                 75.626(4)
_cell_angle_gamma                85.530(3)
_cell_formula_units_Z            2
_cell_length_a                   11.5824(7)
_cell_length_b                   13.5921(7)
_cell_length_c                   14.6115(9)
_cell_measurement_reflns_used    6908
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.64
_cell_measurement_theta_min      2.31
_cell_volume                     2121.2(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Mercury CSD 3.5.1'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SIR97 (Giacovazzo et al, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1097
_diffrn_reflns_av_unetI/netI     0.0797
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            39682
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.740
_diffrn_reflns_theta_min         2.308
_exptl_absorpt_coefficient_mu    0.638
_exptl_absorpt_correction_T_max  0.945
_exptl_absorpt_correction_T_min  0.901
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_description       prism
_exptl_crystal_F_000             1020
_exptl_crystal_size_max          0.430
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.418
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     521
_refine_ls_number_reflns         7996
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1335
_refine_ls_R_factor_gt           0.0604
_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^)+(0.0852P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1469
_refine_ls_wR_factor_ref         0.1705
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4331
_reflns_number_total             7996
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra12274d2.cif
_cod_data_source_block           Compound2rev
_cod_original_cell_volume        2121.3(2)
_cod_database_code               7225404
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.771
_shelx_estimated_absorpt_t_max   0.945
_shelx_res_checksum              49993
_shelx_fab_checksum              18653