Electronic Spectra and Structures of d2 Molybdenum-Oxo Complexes. Effects of Structural Distortions on Orbital Energies, Two-Electron Terms, and the Mixing of Singlet and Triplet States
Ryan E. Da Re; Michael D. Hopkins; Inorganic Chemistry 41 (2002) 6973–6985; doi:10.1021/ic020565r

data_4319071
_publ_contact_author
;
      Michael D. Hopkins
      Department of Chemistry
      5735 South Ellis Avenue
      Chicago, IL 60637
;
_publ_contact_author_email       mhopkins@uchicago.edu
_publ_contact_author_fax         '(773) 702-0850'
_publ_contact_author_phone       '(773) 702-6490'
_publ_section_title
;
 Electronic Spectra and Structures of d2 Molybdenum-Oxo Complexes. Effects
 of Structural Distortions on Orbital Energies, Two-Electron Terms, and
 the Mixing of Singlet and Triplet States
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6973
_journal_page_last               6985
_journal_paper_doi               10.1021/ic020565r
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         'C20 H36 Cl Mo N4 O, C24 H20 B'
_chemical_formula_sum            'C44 H56 B Cl Mo N4 O'
_chemical_formula_weight         799.13
_chemical_name_common            '[MoO(CNBut)4Cl][BPh4] at 300K'
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.5167(19)
_cell_length_b                   14.5167(19)
_cell_length_c                   22.230(4)
_cell_measurement_temperature    293(2)
_cell_volume                     4684.6(12)
_computing_cell_refinement       'SAINT 6.02'
_computing_data_collection       'SMART 5.622'
_computing_data_reduction        'SAINT 6.02'
_computing_molecular_graphics    'XP in SHELXTL 5.1 (Sheldrick, 1997) '
_computing_publication_material  ' SHELXTL 5.1 (Sheldrick, 1997) '
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       /w
_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  0.0307
_diffrn_reflns_av_sigmaI/netI    0.0166
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            22468
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         1.68
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.370
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  .908536
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1997) '
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.133
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          .35
_exptl_crystal_size_mid          .30
_exptl_crystal_size_min          .30
_refine_diff_density_max         0.528
_refine_diff_density_min         -0.201
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.211
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     135
_refine_ls_number_reflns         2088
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.211
_refine_ls_R_factor_all          0.0945
_refine_ls_R_factor_gt           0.0932
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0984P)^2^+9.2375P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2522
_refine_ls_wR_factor_ref         0.2532
_reflns_number_gt                2048
_reflns_number_total             2088
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020565r_1.cif
_cod_data_source_block           ryan07m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        4684.5(12)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               4319071