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_4319072
_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 100K'
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_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                 90.925(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.227(3)
_cell_length_b                   21.291(4)
_cell_length_c                   14.626(3)
_cell_measurement_temperature    100(2)
_cell_volume                     4429.7(15)
_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      100(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0344
_diffrn_reflns_av_sigmaI/netI    0.0376
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11310
_diffrn_reflns_theta_full        25.09
_diffrn_reflns_theta_max         25.09
_diffrn_reflns_theta_min         1.69
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.392
_exptl_absorpt_correction_T_max  .8874
_exptl_absorpt_correction_T_min  .76908
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1997) '
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          .40
_exptl_crystal_size_mid          .40
_exptl_crystal_size_min          .30
_refine_diff_density_max         0.363
_refine_diff_density_min         -0.228
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.179
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     306
_refine_ls_number_reflns         3899
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.179
_refine_ls_R_factor_all          0.0669
_refine_ls_R_factor_gt           0.0630
_refine_ls_shift/su_max          0.146
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0542P)^2^+9.3451P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1611
_refine_ls_wR_factor_ref         0.1635
_reflns_number_gt                3635
_reflns_number_total             3899
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020565r_2.cif
_cod_data_source_block           ryan04m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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        4429.8(14)
_cod_database_code               4319072