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_4318846
_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            'C69.6 H83 Mo0.8 N0 O7.2 P1.6'
_chemical_formula_weight         1161.06
_chemical_name_common
'fac-(CO)3Mo(NCCH2CH3)[(PPh2OCH2)2-nBu4Clx], 14b'
_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                90.000(13)
_cell_angle_beta                 90.000(16)
_cell_angle_gamma                102.273(14)
_cell_formula_units_Z            5
_cell_length_a                   17.704(17)
_cell_length_b                   19.137(18)
_cell_length_c                   23.17(2)
_cell_measurement_temperature    173(2)
_cell_volume                     7671(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.528
_diffrn_measured_fraction_theta_max 0.528
_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  0.0011
_diffrn_reflns_av_sigmaI/netI    0.0057
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            8703
_diffrn_reflns_theta_full        21.00
_diffrn_reflns_theta_max         21.00
_diffrn_reflns_theta_min         4.10
_exptl_absorpt_coefficient_mu    0.270
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3079
_refine_diff_density_max         4.883
_refine_diff_density_min         -3.449
_refine_diff_density_rms         0.269
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   4.717
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     719
_refine_ls_number_reflns         8697
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      4.717
_refine_ls_R_factor_all          0.2953
_refine_ls_R_factor_gt           0.2593
_refine_ls_shift/su_max          0.406
_refine_ls_shift/su_mean         0.080
_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          0.6642
_refine_ls_wR_factor_ref         0.7266
_reflns_number_gt                7171
_reflns_number_total             8697
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020446b_11.cif
_cod_data_source_block           14b
_cod_original_cell_volume        7670(12)
_cod_original_formula_sum        'C69.60 H83 Mo0.80 N0 O7.20 P1.60'
_cod_database_code               4318846