Coordination of Lead(II) in the Supramolecular Environment Provided by a "Two-Story" Calix[6]arene-based N6 Ligand
Diana Over; Xianshun Zeng; Claudia Bornholdt; Jérôme Marrot; Olivia Reinaud; Inorganic Chemistry 52 (2013) 14089–14095; doi:10.1021/ic4018486

data_4336991
_publ_section_title
;
 Coordination of Lead(II) in the Supramolecular Environment Provided by a
 "Two-Story" Calix[6]arene-based N6 Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              14089
_journal_page_last               14095
_journal_paper_doi               10.1021/ic4018486
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C96 H122 Cl2 N6 O15 Pb'
_chemical_formula_weight         1878.09
_chemical_name_systematic
; 
 ? 
;
_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                 92.313(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.118(3)
_cell_length_b                   16.0159(18)
_cell_length_c                   25.074(2)
_cell_measurement_reflns_used    5487
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.17
_cell_measurement_theta_min      2.23
_cell_volume                     10480.0(19)
_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      100(2)
_diffrn_detector_area_resol_mean 512x512
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1072
_diffrn_reflns_av_sigmaI/netI    0.2205
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            18558
_diffrn_reflns_theta_full        25.28
_diffrn_reflns_theta_max         25.28
_diffrn_reflns_theta_min         1.49
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.719
_exptl_absorpt_correction_T_max  0.9664
_exptl_absorpt_correction_T_min  0.7036
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, V2.10)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.190
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             3904
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.131
_refine_diff_density_min         -1.212
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     966
_refine_ls_number_reflns         18558
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.2394
_refine_ls_R_factor_gt           0.1095
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0998P)^2^+12.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2590
_refine_ls_wR_factor_ref         0.2858
_reflns_number_gt                5501
_reflns_number_total             18558
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4018486_si_003.cif
_cod_data_source_block           xz048bsa
_cod_original_cell_volume        10480.3(18)
_cod_database_code               4336991