Using Pyridinyl-Substituted Diaminotriazines to Bind Pd(II) and Create Metallotectons for Engineering Hydrogen-Bonded Crystals
Adam Duong; Thierry Maris; James D. Wuest; Inorganic Chemistry 50 (2011) 5605–5618; doi:10.1021/ic2003047

data_4324185
_publ_section_title
;
 Using Pyridinyl-Substituted Diaminotriazines to Bind Pd(II) and Create
 Metallotectons for Engineering Hydrogen-Bonded Crystals
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5605
_journal_page_last               5618
_journal_paper_doi               10.1021/ic2003047
_journal_volume                  50
_journal_year                    2011
_chemical_compound_source        'Synthesized by the authors. See text'
_chemical_formula_moiety         'C32 H32 N24 Pd, 2(B F4), 9(H2 O)'
_chemical_formula_sum            'C32 H50 B2 F8 N24 O9 Pd'
_chemical_formula_weight         1194.98
_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                 98.680(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.2752(3)
_cell_length_b                   18.5707(4)
_cell_length_c                   17.5545(4)
_cell_measurement_reflns_used    15928
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      68.87
_cell_measurement_theta_min      3.49
_cell_volume                     4922.67(18)
_computing_cell_refinement       'SMART (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2003)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1997)'
_computing_publication_material  'UdMX (local program)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker Smart 6000'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'Montel 200 optics'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.052
_diffrn_reflns_av_sigmaI/netI    0.0461
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            67694
_diffrn_reflns_theta_full        68.94
_diffrn_reflns_theta_max         68.94
_diffrn_reflns_theta_min         3.49
_diffrn_standards_decay_%        4.44
_diffrn_standards_interval_time  1440
_diffrn_standards_number         278
_exptl_absorpt_coefficient_mu    3.987
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5700
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Sheldrick,1996)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2440
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.751
_refine_diff_density_min         -0.741
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     685
_refine_ls_number_reflns         8948
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0769
_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^)+(0.0883P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1869
_refine_ls_wR_factor_ref         0.1884
_reflns_number_gt                7082
_reflns_number_total             8948
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            COD_Inorg_Chem_50_2011_5605_5618.cif
_cod_data_source_block           jw1066
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4324185