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_4325478
_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(F6 P), 4(H2 O)'
_chemical_formula_sum            'C56 H76 F24 N12 O4 P4 Pd2'
_chemical_formula_weight         1773.97
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 103.1050(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.1271(10)
_cell_length_b                   29.7501(15)
_cell_length_c                   14.7561(8)
_cell_measurement_reflns_used    7567
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      24.59
_cell_measurement_theta_min      2.28
_cell_volume                     9033.2(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart Apex CCD'
_diffrn_measurement_method       'phi and omega 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  0.0554
_diffrn_reflns_av_sigmaI/netI    0.0901
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            28029
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.20
_exptl_absorpt_coefficient_mu    0.560
_exptl_absorpt_correction_T_max  0.8867
_exptl_absorpt_correction_T_min  0.8589
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_description       platelet
_exptl_crystal_F_000             3584
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.746
_refine_diff_density_min         -0.791
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     502
_refine_ls_number_reflns         8892
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0889
_refine_ls_R_factor_gt           0.0574
_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^)+(0.0652P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1269
_refine_ls_wR_factor_ref         0.1366
_reflns_number_gt                5432
_reflns_number_total             8892
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200047t_si_002_2.cif
_cod_data_source_block           1a
_cod_database_code               4325478