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_4108006
_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            'C67 H91 O12 P3 S4 W'
_chemical_formula_weight         1493.40
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.3510(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.1372(6)
_cell_length_b                   24.2372(11)
_cell_length_c                   21.5715(10)
_cell_measurement_reflns_used    9988
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      26.56
_cell_measurement_theta_min      2.20
_cell_volume                     7055.1(5)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.1190
_diffrn_reflns_av_sigmaI/netI    0.1157
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            112399
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         1.30
_exptl_absorpt_coefficient_mu    1.881
_exptl_absorpt_correction_T_max  0.9286
_exptl_absorpt_correction_T_min  0.8058
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            ORANGE
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             3088
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_platon_squeeze_details
;
The unit cell contains 12 benzene molecules which have been treated as a 
diffuse cotribution to the overall scattering without specific atom positions
by SQUEEZE/PLATON
;
_refine_diff_density_max         1.157
_refine_diff_density_min         -0.797
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     619
_refine_ls_number_reflns         21530
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1038
_refine_ls_R_factor_gt           0.0499
_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^)+(0.0203P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0819
_refine_ls_wR_factor_ref         0.0883
_reflns_number_gt                12054
_reflns_number_total             21530
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja803215x-file011.cif
_cod_data_source_block           sows10p
_cod_original_cell_volume        7055.0(5)
_cod_database_code               4108006