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_4318844
_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            'C44 H54 Br2 O4'
_chemical_formula_weight         806.69
_chemical_name_common            '5,17-Br2-nBu4Clx, 5'
_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                 120.205(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   31.528(6)
_cell_length_b                   18.821(4)
_cell_length_c                   16.165(3)
_cell_measurement_temperature    178(2)
_cell_measurement_theta_max      55.06
_cell_volume                     8290(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      178(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_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  0.1279
_diffrn_reflns_av_sigmaI/netI    0.0995
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            49040
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         1.31
_exptl_absorpt_coefficient_mu    1.995
_exptl_absorpt_correction_T_max  0.7676
_exptl_absorpt_correction_T_min  0.6150
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             3360
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.059
_refine_diff_density_min         -0.922
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         9480
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.1290
_refine_ls_R_factor_gt           0.0646
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1782
_refine_ls_wR_factor_ref         0.1976
_reflns_number_gt                4620
_reflns_number_total             9480
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020446b_09.cif
_cod_data_source_block           5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_database_code               4318844