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_4316793
_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            'C62 H74 B2 Cl2 Mo2 N14 O8'
_chemical_formula_weight         1427.75
_chemical_name_common            Tp(iPr)MoO2(OC6H4CONH(C6H4Cl-4)-2)
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                96.058(5)
_cell_angle_beta                 95.106(5)
_cell_angle_gamma                98.953(5)
_cell_formula_units_Z            2
_cell_length_a                   12.287(5)
_cell_length_b                   15.054(5)
_cell_length_c                   18.663(5)
_cell_measurement_reflns_used    7753
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.21
_cell_volume                     3371(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0706
_diffrn_reflns_av_sigmaI/netI    0.0738
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            17933
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.10
_exptl_absorpt_coefficient_mu    0.514
_exptl_absorpt_correction_T_max  0.8611
_exptl_absorpt_correction_T_min  0.8017
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.736
_refine_diff_density_min         -0.641
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     811
_refine_ls_number_reflns         11685
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0430P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0954
_refine_ls_wR_factor_ref         0.0985
_reflns_number_gt                9550
_reflns_number_total             11685
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1011428_si_002_2.cif
_cod_data_source_block           jmwng10
_cod_database_code               4316793