p-tert-Butylcalix[4]arene Complexes of Molybdenum and Tungsten: Reactivity of the Calixarene Methylene CH Bond and the Facile Migration of the Metal around the Phenolic Rim of the Calixarene
Daniela Buccella; Gerard Parkin; Journal of the American Chemical Society 128 (2006) 16358–16364; doi:10.1021/ja066457b

data_4111219
_publ_section_title
;
 p-tert-Butylcalix[4]arene Complexes of Molybdenum and Tungsten:
 Reactivity of the Calixarene Methylene CH Bond and the Facile Migration
 of the Metal around the Phenolic Rim of the Calixarene
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16358
_journal_page_last               16364
_journal_paper_doi               10.1021/ja066457b
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C77 H86 O4 W'
_chemical_formula_weight         1259.31
_chemical_name_systematic
; 
 ? 
;
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_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_hydrogens   constr
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                99.540(2)
_cell_angle_beta                 91.222(4)
_cell_angle_gamma                110.178(2)
_cell_formula_units_Z            2
_cell_length_a                   11.2558(11)
_cell_length_b                   14.5191(17)
_cell_length_c                   21.579(2)
_cell_measurement_reflns_used    2444
_cell_measurement_temperature    243(2)
_cell_measurement_theta_max      19.70
_cell_measurement_theta_min      2.66
_cell_volume                     3252.6(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_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      243(2)
_diffrn_measured_fraction_theta_full 0.920
_diffrn_measured_fraction_theta_max 0.920
_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  0.0556
_diffrn_reflns_av_sigmaI/netI    0.1958
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15992
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         0.96
_exptl_absorpt_coefficient_mu    1.824
_exptl_absorpt_correction_T_max  0.9143
_exptl_absorpt_correction_T_min  0.8386
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            ORANGE
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1308
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_platon_squeeze_details
; 
The unit cell contains 2 pentane molecules which have been treated as a 
diffuse cotribution to the overall scattering without specific atom positions
by SQUEEZE/PLATON
;
_refine_diff_density_max         1.429
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     695
_refine_ls_number_reflns         12227
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1585
_refine_ls_R_factor_gt           0.0768
_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^)+(0.0610P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1555
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_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja066457bsi20060906_052940.cif
_cod_data_source_block           walks10p
_cod_original_cell_volume        3252.5(6)
_cod_database_code               4111219