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_4111221
_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            'C62 H92 Mo O4 P3'
_chemical_formula_weight         1090.21
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
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_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_cell_angle_beta                 74.798(2)
_cell_angle_gamma                65.808(2)
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_cell_length_b                   14.1131(10)
_cell_length_c                   19.0193(14)
_cell_measurement_reflns_used    5433
_cell_measurement_temperature    243(2)
_cell_measurement_theta_max      25.963
_cell_measurement_theta_min      2.322
_cell_volume                     3078.0(4)
_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      243(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0297
_diffrn_reflns_av_sigmaI/netI    0.0749
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18066
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.11
_exptl_absorpt_coefficient_mu    0.333
_exptl_absorpt_correction_T_max  0.9674
_exptl_absorpt_correction_T_min  0.9066
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            'DARK RED'
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1166
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.705
_refine_diff_density_min         -0.480
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       0.0004(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     654
_refine_ls_number_reflns         10829
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0879
_refine_ls_R_factor_gt           0.0486
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0538P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1051
_refine_ls_wR_factor_ref         0.1180
_reflns_number_gt                7288
_reflns_number_total             10829
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja066457bsi20060906_053101.cif
_cod_data_source_block           camos10
_cod_database_code               4111221