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_4111220
_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 O4 P3 W'
_chemical_formula_weight         1178.12
_chemical_name_systematic
; 
 ? 
;
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_atom_sites_solution_secondary   difmap
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_cell_angle_gamma                67.5780(10)
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_cell_length_b                   13.9630(6)
_cell_length_c                   18.9093(9)
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_cell_measurement_theta_max      25.918
_cell_measurement_theta_min      2.235
_cell_volume                     3059.9(2)
_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 0.988
_diffrn_measured_fraction_theta_max 0.988
_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
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_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -6
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_diffrn_reflns_limit_l_min       -23
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_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.12
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_exptl_absorpt_correction_T_max  0.6895
_exptl_absorpt_correction_T_min  0.5841
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            ORANGE
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_exptl_crystal_size_max          0.30
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_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
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_refine_ls_number_reflns         12365
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_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0382
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0269P)^2^+0.1764P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0686
_refine_ls_wR_factor_ref         0.0764
_reflns_number_gt                9551
_reflns_number_total             12365
_reflns_threshold_expression     >2sigma(I)
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_cod_database_code               4111220