Programmable Self-Assembly of Homo- or Hetero- Metallomacrocycles using 4-(1H-pyrazolyl-4-yl)pyridine
Jin Tong; Shu-Yan Yu; Hui Li; Chem.Commun. 48 (2012) 5343–; doi:10.1039/c2cc31234d

data_7107721
_publ_section_title
;
 Programmable Self-Assembly of Homo- or Hetero- Metallomacrocycles using
 4-(1H-pyrazolyl-4-yl)pyridine
;
_journal_name_full               Chem.Commun.
_journal_page_first              5343
_journal_paper_doi               10.1039/c2cc31234d
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety
'C92 H73.20 N24 O0.60 Pd6, 0.4(H4 O2), 8.6(H2 O)'
_chemical_formula_sum            'C92 H92 N24 O10 Pd6'
_chemical_formula_weight         2332.30
_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                75.0190(10)
_cell_angle_beta                 86.462(2)
_cell_angle_gamma                77.0910(10)
_cell_formula_units_Z            1
_cell_length_a                   12.6289(6)
_cell_length_b                   16.3546(8)
_cell_length_c                   17.1424(6)
_cell_measurement_reflns_used    3175
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      24.12
_cell_measurement_theta_min      2.33
_cell_volume                     3333.8(3)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart Apex CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_sigmaI/netI    0.0431
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20902
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.32
_exptl_absorpt_coefficient_mu    0.842
_exptl_absorpt_correction_T_max  0.837
_exptl_absorpt_correction_T_min  0.785
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.358
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     685
_refine_ls_number_reflns         13113
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0707
_refine_ls_R_factor_gt           0.0440
_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^)+(0.0519P)^2^+1.3779P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1026
_refine_ls_wR_factor_ref         0.1097
_reflns_number_gt                9144
_reflns_number_total             13113
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc31234d.txt
_cod_data_source_block           42
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7107721