cis-Dioxo- and cis-(Hydroxo)oxo-Mo(V) Complexes Stabilized by Intramolecular Hydrogen-Bonding
Victor W. L. Ng; Michelle K. Taylor; Jonathan M. White; Charles G. Young; Inorganic Chemistry 49 (2010) 9460–9469; doi:10.1021/ic1011428

data_4316792
_publ_section_title
;
 cis-Dioxo- and cis-(Hydroxo)oxo-Mo(V) Complexes Stabilized by
 Intramolecular Hydrogen-Bonding
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9460
_journal_page_last               9469
_journal_paper_doi               10.1021/ic1011428
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C31 H40 B Mo N7 O5'
_chemical_formula_weight         697.45
_chemical_name_common            Tp(iPr)MoO2(OC6H4CONHPh-2)
_chemical_name_systematic
;
 ?
;
_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                 90.2490(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.96030(10)
_cell_length_b                   10.55090(10)
_cell_length_c                   18.2873(2)
_cell_measurement_reflns_used    7936
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      72.9707
_cell_measurement_theta_min      3.5483
_cell_volume                     3272.42(5)
_computing_cell_refinement
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
;
_computing_data_reduction
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_sigmaI/netI    0.0543
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13544
_diffrn_reflns_theta_full        67.49
_diffrn_reflns_theta_max         67.49
_diffrn_reflns_theta_min         4.84
_exptl_absorpt_coefficient_mu    3.690
_exptl_absorpt_correction_T_max  0.7092
_exptl_absorpt_correction_T_min  0.2599
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.923
_refine_diff_density_min         -0.769
_refine_diff_density_rms         0.111
_refine_ls_extinction_coef       0.00009(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.170
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         5813
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.170
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0591
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+29.0697P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1500
_refine_ls_wR_factor_ref         0.1550
_reflns_number_gt                4824
_reflns_number_total             5813
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1011428_si_002_1.cif
_cod_data_source_block           jmwng7a
_cod_database_code               4316792