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_4310764
_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            'C39.5 H52.5 Cl Co Mo N0.5 O5'
_chemical_formula_weight         809.11
_chemical_name_systematic
; 
 (CoCp2)[MoO(3,6-DBCat)2] 1/2CH2Cl2 1/2CH3CN 
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 105.8010(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.0347(2)
_cell_length_b                   15.1104(2)
_cell_length_c                   20.13870(10)
_cell_measurement_reflns_used    564
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.4
_cell_measurement_theta_min      13.2
_cell_volume                     3816.63(8)
_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      138(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  0.0319
_diffrn_reflns_av_sigmaI/netI    0.0413
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            34467
_diffrn_reflns_theta_max         31.34
_diffrn_reflns_theta_min         1.62
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.877
_exptl_absorpt_correction_T_max  0.663
_exptl_absorpt_correction_T_min  0.879
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_description       needle
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.59
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.730
_refine_diff_density_min         -1.120
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.031
_refine_ls_goodness_of_fit_obs   1.058
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         11673
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_restrained_S_obs      1.058
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_obs          0.0417
_refine_ls_shift/esd_max         0.020
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0563P)^2^+3.8500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1150
_refine_ls_wR_factor_obs         0.1063
_reflns_number_observed          9537
_reflns_number_total             11673
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0354264si20031211_050150_1.cif
_cod_data_source_block           (CoCp2)[MoO(3,6-DBCat)2]
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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^)+(0.0563P)^2^+3.8500P] 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^)+(0.0563P)^2^+3.8500P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'C39.5 H52.5 Cl Co Mo N0.50 O5'
_cod_database_code               4310764