Mononuclear and Dinuclear Molybdenum and Tungsten Complexes of p-tert-Butyltetrathiacalix[4]arene and p-tert-Butyltetrasulfonylcalix[4]arene: Facile Cleavage of the Calixarene Ligand Framework by Nickel
Daniela Buccella; Gerard Parkin; Journal of the American Chemical Society 130 (2008) 8617–8619; doi:10.1021/ja803215x

data_4108008
_publ_section_title
;
 Mononuclear and Dinuclear Molybdenum and Tungsten Complexes of
 p-tert-Butyltetrathiacalix[4]arene and
 p-tert-Butyltetrasulfonylcalix[4]arene: Facile Cleavage of the Calixarene
 Ligand Framework by Nickel
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8617
_journal_page_last               8619
_journal_paper_doi               10.1021/ja803215x
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C61 H99 Ni O4 P5 S4 W'
_chemical_formula_weight         1422.05
_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                114.671(2)
_cell_angle_beta                 100.424(2)
_cell_angle_gamma                104.5620(10)
_cell_formula_units_Z            2
_cell_length_a                   14.5404(11)
_cell_length_b                   16.1285(13)
_cell_length_c                   17.951(2)
_cell_measurement_reflns_used    9785
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      31.854
_cell_measurement_theta_min      2.324
_cell_volume                     3501.6(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      125(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_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  0.0464
_diffrn_reflns_av_sigmaI/netI    0.0663
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            60282
_diffrn_reflns_theta_full        31.88
_diffrn_reflns_theta_max         31.88
_diffrn_reflns_theta_min         1.32
_exptl_absorpt_coefficient_mu    2.184
_exptl_absorpt_correction_T_max  0.8801
_exptl_absorpt_correction_T_min  0.7213
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_description       block
_exptl_crystal_F_000             1476
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.712
_refine_diff_density_min         -0.590
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     752
_refine_ls_number_reflns         23377
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0626
_refine_ls_R_factor_gt           0.0387
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0320P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0789
_reflns_number_gt                17884
_reflns_number_total             23377
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja803215x-file013.cif
_cod_data_source_block           wnis10
_cod_original_cell_volume        3501.7(6)
_cod_database_code               4108008