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_4310768
_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            'C33 H45 Mo N O6'
_chemical_formula_weight         647.64
_chemical_name_systematic
; 
 MoO(OPy)(3,6-DBCat)2 
;
_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                82.2430(10)
_cell_angle_beta                 76.3460(10)
_cell_angle_gamma                60.8420(10)
_cell_formula_units_Z            2
_cell_length_a                   10.34000(10)
_cell_length_b                   10.6052(3)
_cell_length_c                   17.1703(3)
_cell_measurement_temperature    154(2)
_cell_volume                     1597.35(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      154(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Siemens SMART'
_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  0.0557
_diffrn_reflns_av_sigmaI/netI    0.0904
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14786
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    0.454
_exptl_absorpt_correction_T_max  0.9910
_exptl_absorpt_correction_T_min  0.8501
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            dark_blue
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.566
_refine_diff_density_min         -1.363
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         7768
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0716
_refine_ls_R_factor_gt           0.0507
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0571P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1193
_refine_ls_wR_factor_ref         0.1321
_reflns_number_gt                6005
_reflns_number_total             7768
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0354264si20031211_050150_5.cif
_cod_data_source_block           MoO(OPy)(3,6-DBCat)2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Multiscan' changed to 'multi-scan'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4310768