Synthesis and Structural Characterization of a 4-Coordinate Molybdenum(VI) Dioxo Diaryloxide, MoO2(O-2,6-t-Bu2C6H3)2.HO-2,6-t-Bu2C6H3
Tracy A. Hanna; Christopher D. Incarvito; Arnold L. Rheingold; Inorganic Chemistry 39 (2000) 630–631; doi:10.1021/ic991271h

data_4300225
_publ_contact_author
; 
     Dr. T. Hanna 
     Department of Chemistry 
     Box 298860 
     Texas Christian University 
     USA 
;
_publ_contact_author_email       T.Hanna@tcu.edu
_publ_contact_author_fax         '+817 257 5851'
_publ_contact_author_phone       '+817 257 6197'
_publ_section_title
;
Synthesis and Structural Characterization of a 4-Coordinate Molybdenum(VI)
Dioxo Diaryloxide, MoO2(O-2,6-t-Bu2C6H3)2.HO-2,6-t-Bu2C6H3
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              630
_journal_page_last               631
_journal_paper_doi               10.1021/ic991271h
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C42 H64 Mo O5'
_chemical_formula_weight         744.87
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 99.1385(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.4344(2)
_cell_length_b                   19.4277(3)
_cell_length_c                   18.5445(3)
_cell_measurement_temperature    173(2)
_cell_volume                     4067.26(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.832
_diffrn_measured_fraction_theta_max 0.832
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0360
_diffrn_reflns_av_sigmaI/netI    0.0397
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            18681
_diffrn_reflns_theta_full        28.14
_diffrn_reflns_theta_max         28.14
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    0.362
_exptl_absorpt_correction_T_max  0.9647
_exptl_absorpt_correction_T_min  0.8990
_exptl_absorpt_correction_type   'empirical from SADABS'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.621
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.250
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         8275
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.250
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0486
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1505
_refine_ls_wR_factor_ref         0.1675
_reflns_number_gt                6879
_reflns_number_total             8275
_reflns_threshold_expression     >2sigma(I)
_cod_original_cell_volume        4067.27(12)
_cod_database_code               4300225