Alkylation of a Dimolybdenum SO Bridge, Subsequent Reactions, and Characterization of the Thioperoxide Bridge
Chi Minh Tuong; Whitney K. Hammons; Ashley L. Howarth; Kelly E. Lutz; Ackim D. Maduvu; Laura B. Haysley; Brian R. T. Allred; Lenore K. Hoyt; Mark S. Mashuta; Mark E. Noble; Inorganic Chemistry 48 (2009) 5027–5038; doi:10.1021/ic9002093

data_4302207
_publ_contact_author_address
;
Department of Chemistry
University of Louisville
2320 So. Brook St.
Louisville
KY 40292
USA
;
_publ_contact_author_email       menoble@louisville.edu
_publ_contact_author_fax         502-852-8149
_publ_contact_author_name        'Mark E. Noble'
_publ_contact_author_phone       502-852-7296
_publ_section_title
;
Alkylation of a Dimolybdenum SO Bridge, Subsequent Reactions, and
Characterization of the Thioperoxide Bridge
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5027
_journal_page_last               5038
_journal_paper_doi               10.1021/ic9002093
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C26 H42 Mo2 N2 O7 P2 S6'
_chemical_formula_sum            'C26 H42 Mo2 N2 O7 P2 S6'
_chemical_formula_weight         940.80
_chemical_name_common
; 
 proximal [Mo~2~(NTo)~2~(S~2~P(OEt)~2~)~2~(O~2~CMe)S(SOEt)]
;
_chemical_name_systematic
; 
 (\m-acetato)(\m-ethoxythiolato)(\m-sulfido)bis(O,O'-diethyl
 dithiophosphato)bis(p-tolylimido)dimolybdenum(V), E isomer 
;
_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
_audit_update_record
;
  May_17_2006 text and data added by Mark S. Mashuta
  Sept_23_2006 text and data added by Mark S. Mashuta
;
_cell_angle_alpha                90.00
_cell_angle_beta                 97.819(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.448(2)
_cell_length_b                   19.771(2)
_cell_length_c                   9.4698(10)
_cell_measurement_reflns_used    5628
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.75
_cell_measurement_theta_min      2.29
_cell_volume                     3792.8(7)
_computing_cell_refinement       'SAINT 6.36 (Bruker, 2002)'
_computing_data_collection       'SMART 5.628 (Bruker, 2002)'
_computing_data_reduction        'SAINT 6.36 (Bruker, 2002)'
_computing_molecular_graphics    'SHELXTL 6.12 (Bruker, 2001)'
_computing_publication_material  'SHELXTL 6.12 (Bruker, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-90 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device_type  'SMART APEX CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_sigmaI/netI    0.0546
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            32090
_diffrn_reflns_theta_full        28.09
_diffrn_reflns_theta_max         28.09
_diffrn_reflns_theta_min         2.01
_diffrn_standards_decay_%        <0.1
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.118
_exptl_absorpt_correction_T_max  0.895
_exptl_absorpt_correction_T_min  0.733
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS; Sheldrick, (1996).
;
_exptl_crystal_colour            red-orange
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       prism
_exptl_crystal_F_000             1912
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.018
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     423
_refine_ls_number_reflns         8687
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0510
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0250P)^2^+18.2069P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1085
_refine_ls_wR_factor_ref         0.1174
_reflns_number_gt                6193
_reflns_number_total             8687
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic9002093_si_002_2.cif
_cod_data_source_block           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 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4302207