Facile high-yield synthesis of unsymmetric end-off compartmental double Schiff-base ligands: easy access to mononuclear precursor and unsymmetric dinuclear complexes
Schmidt, Markus; Görls, Helmar; Plass, Winfried; RSC Adv.  (2016) –; doi:10.1039/C6RA16870A

data_7226112
_publ_section_title
;
 Facile high-yield synthesis of unsymmetric end-off compartmental double
 Schiff-base ligands: easy access to mononuclear precursor and unsymmetric
 dinuclear complexes
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA16870A
_journal_year                    2016
_chemical_formula_moiety         'C28 H31 N7 O5 S Zn2, C2 H3 N, H2 O'
_chemical_formula_sum            'C30 H36 N8 O6 S Zn2'
_chemical_formula_weight         767.47
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-06-30 deposited with the CCDC.
2016-08-03 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 93.667(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.4746(8)
_cell_length_b                   15.0226(11)
_cell_length_c                   16.6745(12)
_cell_measurement_temperature    133(2)
_cell_volume                     3368.4(4)
_computing_cell_refinement       DENZO
_computing_data_collection       COLLECT
_computing_data_reduction        DENZO
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.913
_diffrn_measured_fraction_theta_max 0.874
_diffrn_measurement_device_type  Kappa_CCD
_diffrn_measurement_method       'phi- + omega-scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_sigmaI/netI    0.0471
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15345
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.42
_exptl_absorpt_coefficient_mu    1.540
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6133
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2002'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.046
_exptl_crystal_size_mid          0.046
_exptl_crystal_size_min          0.034
_refine_diff_density_max         0.538
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.177
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         6769
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.177
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0565
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0138P)^2^+11.0751P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1062
_refine_ls_wR_factor_ref         0.1176
_reflns_number_gt                5432
_reflns_number_total             6769
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ra16870a2.cif
_cod_data_source_block           FO4332
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_database_code               7226112