Synthesis and Characterization of Diametrically Substituted Tetra-O-n-butylcalix[4]arene Ligands and Their Chelated Complexes of Titanium, Molybdenum, and Palladium
Daniel R. Evans; Mingsheng Huang; James C. Fettinger; Tracie L. Williams; Inorganic Chemistry 41 (2002) 5986–6000; doi:10.1021/ic020446b

data_4318838
_publ_contact_author_email       de44@umail.umd.edu
_publ_contact_author_fax         +1-301-314-9121
_publ_contact_author_name        'Prof Daniel R. Evans'
_publ_contact_author_phone       +1-301-405-8436
_publ_section_title
;
 Synthesis and Characterization of Diametrically Substituted
 Tetra-O-n-butylcalix[4]arene Ligands and Their Chelated Complexes of
 Titanium, Molybdenum, and Palladium
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5986
_journal_page_last               6000
_journal_paper_doi               10.1021/ic020446b
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C154 H133 O21'
_chemical_formula_weight         2319.60
_chemical_name_common            '(HOCH2)2-nBu4Clx, 7'
_chemical_name_systematic
;
  ?
;
_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                68.048(2)
_cell_angle_beta                 86.329(2)
_cell_angle_gamma                87.564(2)
_cell_formula_units_Z            2
_cell_length_a                   16.610(2)
_cell_length_b                   20.000(2)
_cell_length_c                   20.664(3)
_cell_measurement_temperature    113(2)
_cell_volume                     6352.5(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0418
_diffrn_reflns_av_sigmaI/netI    0.0606
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            31887
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.21
_exptl_absorpt_coefficient_mu    0.080
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2450
_refine_diff_density_max         1.811
_refine_diff_density_min         -2.281
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.322
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1521
_refine_ls_number_reflns         16502
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      1.334
_refine_ls_R_factor_all          0.1567
_refine_ls_R_factor_gt           0.1106
_refine_ls_shift/su_max          0.099
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3141
_refine_ls_wR_factor_ref         0.3504
_reflns_number_gt                10709
_reflns_number_total             16502
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020446b_03.cif
_cod_data_source_block           7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        6352.9(13)
_cod_database_code               4318838