Influence of Terminal Acryloyl Arms on the Coordination Chemistry of a Ditopic Pyrimidine-Hydrazone Ligand: Comparison of Pb(II), Zn(II), Cu(II), and Ag(I) Complexes
Daniel J. Hutchinson; Lyall R. Hanton; Stephen C. Moratti; Inorganic Chemistry 52 (2013) 2716–2728; doi:10.1021/ic3027978

data_4334071
_publ_contact_author             'Hanton, Lyall R.'
_publ_contact_author_email       lhanton@Chemistry.otago.ac.nz
_publ_section_title
;
 Influence of Terminal Acryloyl Arms on the Coordination Chemistry of a
 Ditopic Pyrimidine-Hydrazone Ligand: Comparison of Pb(II), Zn(II),
 Cu(II), and Ag(I) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2716
_journal_page_last               2728
_journal_paper_doi               10.1021/ic3027978
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C29 H31 Cl4 N9 O20 Pb2'
_chemical_formula_sum            'C29 H31 Cl4 N9 O20 Pb2'
_chemical_formula_weight         1381.83
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                117.6600(10)
_cell_angle_beta                 92.1710(10)
_cell_angle_gamma                115.2450(10)
_cell_formula_units_Z            2
_cell_length_a                   13.3813(5)
_cell_length_b                   13.6338(5)
_cell_length_c                   14.6157(6)
_cell_measurement_reflns_used    9982
_cell_measurement_temperature    91(2)
_cell_measurement_theta_max      28.89
_cell_measurement_theta_min      2.74
_cell_volume                     2041.48(14)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      91(2)
_diffrn_measured_fraction_theta_full 0.909
_diffrn_measured_fraction_theta_max 0.909
_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  0.0292
_diffrn_reflns_av_sigmaI/netI    0.0280
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            26459
_diffrn_reflns_theta_full        25.49
_diffrn_reflns_theta_max         25.49
_diffrn_reflns_theta_min         2.11
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.591
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.3955
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2004)'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    2.248
_exptl_crystal_description       rod
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.350
_refine_diff_density_min         -1.368
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     581
_refine_ls_number_reflns         6916
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0242
_refine_ls_R_factor_gt           0.0202
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0101P)^2^+5.2836P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0416
_refine_ls_wR_factor_ref         0.0432
_reflns_number_gt                6259
_reflns_number_total             6916
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3027978_si_001_4.cif
_cod_data_source_block           Complex_3(djh740)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4334071