Shaping the Cavity of the Macrocyclic Ligand in Metallocalix[4]arenes: The Role of the Ligand Sphere
Udo Radius; Inorganic Chemistry 40 (2001) 6637–6642; doi:10.1021/ic010482v

data_4320692
_publ_author_name                'Udo Radius'
_publ_contact_author
;
  Udo Radius
  Institut f\"ur Anorganische Chemie der Universit\"at
  Engesserstrasse, Geb\"aude 30.45
  D-76128 Karlsruhe
  Deutschland
;
_publ_contact_author_email       uradius@achibm6.chemie.uni_karlsruhe.de
_publ_contact_author_fax         'Int + 721 661921'
_publ_contact_author_phone       'Int + 721 608 2855'
_publ_section_title
;
 Shaping the Cavity of the Macrocyclic Ligand in Metallocalix[4]arenes:
 The Role of the Ligand Sphere
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6637
_journal_page_last               6642
_journal_paper_doi               10.1021/ic010482v
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C60 H71 Cl2 O4 Ti'
_chemical_formula_weight         974.97
_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                 95.68(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.639(4)
_cell_length_b                   20.152(4)
_cell_length_c                   12.750(3)
_cell_measurement_temperature    190(2)
_cell_volume                     5533(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      190(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0420
_diffrn_reflns_av_sigmaI/netI    0.0326
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            46404
_diffrn_reflns_theta_full        24.92
_diffrn_reflns_theta_max         24.92
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    0.295
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2076
_refine_diff_density_max         0.959
_refine_diff_density_min         -0.661
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         9554
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0540
_refine_ls_shift/su_max          1.353
_refine_ls_shift/su_mean         0.023
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1117P)^2^+1.5960P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1604
_refine_ls_wR_factor_ref         0.1675
_reflns_number_gt                7655
_reflns_number_total             9554
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010482v_2.cif
_cod_data_source_block           1
_cod_original_cell_volume        5532.6(19)
_cod_database_code               4320692