Synthesis and Characterization of Monomeric Oxo Dichloro 1,3-Dialkyl p-tert-Butylcalix[4]arene Complexes of Molybdenum(VI,V) and Tungsten(VI,V)
Andrew J. Millar; Jonathan M. White; Christian J. Doonan; Charles G. Young; Inorganic Chemistry 39 (2000) 5151–5155; doi:10.1021/ic000431i

data_4321499
_publ_section_title
;
 Synthesis and Characterization of Monomeric Oxo Dichloro 1,3-Dialkyl
 p-tert-Butylcalix[4]arene Complexes of Molybdenum(VI,V) and
 Tungsten(VI,V)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5151
_journal_page_last               5155
_journal_paper_doi               10.1021/ic000431i
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C49 H63 Cl5 Mo O5'
_chemical_formula_weight         1005.18
_chemical_name_systematic
; 
(1,3-dimethyl tetra-p-tert-butylcalix[4]arene-O1,O2,O4)dichlorooxomolybdenum(VI)
;
_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                95.87(2)
_cell_angle_beta                 112.00(2)
_cell_angle_gamma                112.090(10)
_cell_formula_units_Z            2
_cell_length_a                   13.230(3)
_cell_length_b                   14.950(3)
_cell_length_c                   15.799(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      20
_cell_volume                     2574.9(12)
_computing_data_reduction        Process-Data
_computing_molecular_graphics    ZORTEP
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Enraf Nonius'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0151
_diffrn_reflns_av_sigmaI/netI    0.0379
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9132
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.05
_diffrn_standards_decay_%        2.5
_diffrn_standards_interval_time  9600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.556
_exptl_crystal_colour            dark_red
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.583
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       0.0010(4)
_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   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     592
_refine_ls_number_reflns         8703
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0478
_refine_ls_shift/su_max          0.255
_refine_ls_shift/su_mean         0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0725P)^2^+2.1545P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1214
_refine_ls_wR_factor_ref         0.1327
_reflns_number_gt                6943
_reflns_number_total             8703
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000431i_1.cif
_cod_data_source_block           jmwcd1
_cod_original_cell_volume        2574.9(10)
_cod_database_code               4321499