Zinc(ii) ortho-hydroxyphenylhydrazo-β-diketonate complexes and their catalytic ability towards diastereoselective nitroaldol (Henry) reaction.
Kopylovich, Maximilian N.; Mac Leod, Tatiana C. O.; Mahmudov, Kamran T.; Guedes da Silva, M Fátima C; Pombeiro, Armando J. L.; Dalton transactions (Cambridge, England : 2003) 40 (2011) 5352–5361; doi:10.1039/c0dt01457e

data_7015296
_publ_section_title
;
 Zinc(ii) ortho-hydroxyphenylhydrazo-\b-diketonate complexes and their
 catalytic ability towards diastereoselective nitroaldol (Henry)
 reaction.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5352
_journal_page_last               5361
_journal_paper_doi               10.1039/c0dt01457e
_journal_volume                  40
_journal_year                    2011
_chemical_formula_moiety         'C14 H19 N3 O8 Zn'
_chemical_formula_sum            'C14 H19 N3 O8 Zn'
_chemical_formula_weight         422.69
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.006(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.5844(11)
_cell_length_b                   15.743(3)
_cell_length_c                   16.287(3)
_cell_measurement_reflns_used    275
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      17.92
_cell_measurement_theta_min      2.83
_cell_volume                     1679.0(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.1851
_diffrn_reflns_av_sigmaI/netI    0.2776
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8485
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.59
_exptl_absorpt_coefficient_mu    1.513
_exptl_absorpt_correction_T_max  0.735
_exptl_absorpt_correction_T_min  0.608
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.654
_refine_diff_density_min         -0.963
_refine_diff_density_rms         0.221
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         2936
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.2334
_refine_ls_R_factor_gt           0.1032
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1438P)^2^+4.5671P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2737
_refine_ls_wR_factor_ref         0.3351
_reflns_number_gt                1304
_reflns_number_total             2936
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt01457e.txt
_cod_data_source_block           Compound8
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7015296