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_4310767
_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            'C32 H52 Mo O7 S2'
_chemical_formula_weight         708.80
_chemical_name_systematic
; 
 MoO(dmso)(3,6-DBCat)2_DMSO 
;
_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
_cell_angle_alpha                99.5230(10)
_cell_angle_beta                 93.2470(10)
_cell_angle_gamma                114.6640(10)
_cell_formula_units_Z            2
_cell_length_a                   10.69460(10)
_cell_length_b                   11.23830(10)
_cell_length_c                   16.68450(10)
_cell_measurement_reflns_used    134
_cell_measurement_temperature    145(2)
_cell_measurement_theta_max      15.4
_cell_measurement_theta_min      10.1
_cell_volume                     1779.48(3)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      145(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w 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  0.0576
_diffrn_reflns_av_sigmaI/netI    0.0931
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19712
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.25
_diffrn_standards_decay_%        2.11
_diffrn_standards_interval_count 95
_diffrn_standards_number         5
_exptl_absorpt_coefficient_mu    0.527
_exptl_absorpt_correction_T_max  0.955
_exptl_absorpt_correction_T_min  0.671
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            dark_blue
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_description       plate
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.625
_refine_diff_density_min         -1.465
_refine_diff_density_rms         0.112
_refine_ls_extinction_coef       0.0006(5)
_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_all   1.000
_refine_ls_goodness_of_fit_obs   1.041
_refine_ls_hydrogen_treatment    'fixed, riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         8707
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_restrained_S_obs      1.041
_refine_ls_R_factor_all          0.0856
_refine_ls_R_factor_obs          0.0513
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0578P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1288
_refine_ls_wR_factor_obs         0.1090
_reflns_number_observed          6304
_reflns_number_total             8712
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0354264si20031211_050150_4.cif
_cod_data_source_block           MoO(dmso)(3,6-DBCat)2_DMSO
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0578P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0578P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1779.48(2)
_cod_database_code               4310767