Coordination Complexes of Molybdenum with 3,6-Di-tert-butylcatechol. Addition Products of DMSO, Pyridine N-oxide, and Triphenylarsine Oxide to the Putative [MoVIO(3,6-DBCat)2] Monomer and Self-Assembly of the Chiral [{MoVIO(3,6-DBCat)2}4] Square
Cai-Ming Liu; Ebbe Nordlander; Derek Schmeh; Richard Shoemaker; Cortlandt G. Pierpont; Inorganic Chemistry 43 (2004) 2114–2124; doi:10.1021/ic0354264

data_4310769
_publ_contact_author_address
;
Department of Chemistry and Biochemistry
University of Colorado
Boulder, CO  80309
;
_publ_contact_author_name        'Professor Cortlandt Pierpont'
_publ_section_title
;
 Coordination Complexes of Molybdenum with 3,6-Di-tert-butylcatechol.
 Addition Products of DMSO, Pyridine N-oxide, and Triphenylarsine Oxide to
 the Putative [MoVIO(3,6-DBCat)2] Monomer and Self-Assembly of the Chiral
 [{MoVIO(3,6-DBCat)2}4] Square
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2114
_journal_page_last               2124
_journal_paper_doi               10.1021/ic0354264
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C58 H70 As Mo O6'
_chemical_formula_weight         1034.00
_chemical_name_systematic
; 
 MoO(OAsPh3)(3,6-DBCat)2 1.5 C8H10 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 109.8060(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.6888(5)
_cell_length_b                   17.5638(5)
_cell_length_c                   19.6028(6)
_cell_measurement_reflns_used    1854
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      26.84
_cell_measurement_theta_min      8.42
_cell_volume                     5406.0(3)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    XP
_computing_publication_material  XTEXT
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      143(2)
_diffrn_measured_fraction_theta_full 0.932
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  Bruker
_diffrn_measurement_method       'SMART CCD'
_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  0.01200
_diffrn_reflns_av_sigmaI/netI    0.0468
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            16455
_diffrn_reflns_theta_full        31.27
_diffrn_reflns_theta_max         31.27
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    0.897
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.73
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            dark_brown
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2164
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.690
_refine_diff_density_min         -0.901
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       NA
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         16455
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0805
_refine_ls_R_factor_gt           0.0435
_refine_ls_shift/su_max          0.071
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0522P)^2^+2.3650P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.1096
_reflns_number_gt                11219
_reflns_number_total             16455
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0354264si20031211_050150_6.cif
_cod_data_source_block           MoO(OAsPh3)(3,6-DBCat)2
_cod_database_code               4310769