Synthesis and Anion Sensing of Water-Soluble Metallomacrocycles
Liao-Yuan Yao; Lin Qin; Ting-Zheng Xie; Yi-Zhi Li; Shu-Yan Yu; Inorganic Chemistry 50 (2011) 6055–6062; doi:10.1021/ic200047t

data_4325477
_publ_section_title
;
 Synthesis and Anion Sensing of Water-Soluble Metallomacrocycles
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6055
_journal_page_last               6062
_journal_paper_doi               10.1021/ic200047t
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C56 H68 N12 Pd2, 4(N O3), 2(H2 O)'
_chemical_formula_sum            'C56 H72 N16 O14 Pd2'
_chemical_formula_weight         1406.10
_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                 98.295(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.8736(18)
_cell_length_b                   21.6334(15)
_cell_length_c                   27.5290(16)
_cell_measurement_reflns_used    4735
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      25.12
_cell_measurement_theta_min      2.12
_cell_volume                     6997.3(12)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Smart Aepex 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  0.0375
_diffrn_reflns_av_sigmaI/netI    0.0597
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            42533
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    0.582
_exptl_absorpt_correction_T_max  0.8925
_exptl_absorpt_correction_T_min  0.8541
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'sadabs; bRUKER, 2000'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2896
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.483
_refine_diff_density_min         -0.813
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     864
_refine_ls_number_reflns         13730
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0546
_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^)+(0.06P)^2^+1.99P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1192
_refine_ls_wR_factor_ref         0.1236
_reflns_number_gt                9603
_reflns_number_total             13730
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200047t_si_002_1.cif
_cod_data_source_block           1
_cod_database_code               4325477