Dibenzyl and diallyl 2,6-bisiminopyridinezinc(II) complexes: selective alkyl migration to the pyridine ring leads to remarkably stable dihydropyridinates
John J. Sandoval; Pilar Palma; Eleuterio Alvarez; Antonio Rodriguez-Delgado; Juan Campora; Chem.Commun. 49 (2013) 6791–; doi:10.1039/c3cc42798f

data_7109530
_publ_section_title
;
 Dibenzyl and diallyl 2,6-bisiminopyridinezinc(II) complexes: selective
 alkyl migration to the pyridine ring leads to remarkably stable
 dihydropyridinates
;
_journal_name_full               Chem.Commun.
_journal_page_first              6791
_journal_paper_doi               10.1039/c3cc42798f
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety         'C47 H57 N3 Zn, 0.5(C6 H14)'
_chemical_formula_sum            'C50 H64 N3 Zn'
_chemical_formula_weight         772.41
_chemical_name_systematic
;
?
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 100.793(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.0371(12)
_cell_length_b                   16.4360(15)
_cell_length_c                   23.031(2)
_cell_measurement_reflns_used    9898
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.62
_cell_measurement_theta_min      2.43
_cell_volume                     4475.9(7)
_computing_cell_refinement       'APEX2 Software Suite (Bruker, 2007)'
_computing_data_collection       'APEX2 Software Suite (Bruker, 2007)'
_computing_data_reduction        'APEX2 Software Suite (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL and publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2002 (Burla et al., 2003)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
;
Bruker-Nonius X8kappa APEX II CCD area detector
;
_diffrn_measurement_method       'phi and omega scans with narrow frames'
_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  0.0442
_diffrn_reflns_av_sigmaI/netI    0.0332
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            90841
_diffrn_reflns_theta_full        30.54
_diffrn_reflns_theta_max         30.54
_diffrn_reflns_theta_min         1.53
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.584
_exptl_absorpt_correction_T_max  0.9175
_exptl_absorpt_correction_T_min  0.8543
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
program SADABS, Bruker (2001).
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.146
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1660
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.905
_refine_diff_density_min         -0.535
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         13656
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0818
_refine_ls_R_factor_gt           0.0502
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0860P)^2^+2.5868P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1432
_refine_ls_wR_factor_ref         0.1662
_reflns_number_gt                9496
_reflns_number_total             13656
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc42798f.txt
_cod_data_source_block           c2b
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7109530