cis-Dioxomolybdenum(VI) and Oxo(phosphine oxide)molybdenum(IV) Complexes: Steric and Electronic Fine-Tuning of cis-[MoOS]2+ Precursors
Christian J. Doonan; Andrew J. Millar; David J. Nielsen; Charles G. Young; Inorganic Chemistry 44 (2005) 4506–4514; doi:10.1021/ic050052v

data_4309077
_publ_section_title
;
cis-Dioxomolybdenum(VI) and Oxo(phosphine oxide)molybdenum(IV) Complexes:
Steric and Electronic Fine-Tuning of cis-[MoOS]2+ Precursors
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4506
_journal_page_last               4514
_journal_paper_doi               10.1021/ic050052v
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C28 H35 B Mo N6 O3'
_chemical_formula_weight         610.37
_chemical_name_systematic
;
cis-{hydrotris(3-isopropylpyrazol-1-yl)borato}-
(2-naphtholato)dioxomolybdenum(VI)
;
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 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                 99.593(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.6654(10)
_cell_length_b                   7.6780(6)
_cell_length_c                   15.3752(13)
_cell_measurement_temperature    293(2)
_cell_volume                     1474.3(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0415
_diffrn_reflns_av_sigmaI/netI    0.0565
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8985
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    0.484
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             632
_refine_diff_density_max         0.685
_refine_diff_density_min         -0.263
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.10(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.883
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         5077
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.882
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0398
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0356P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0779
_refine_ls_wR_factor_ref         0.0817
_reflns_number_gt                3880
_reflns_number_total             5077
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050052vsi20041222_062719_7.cif
_cod_data_source_block           Complex_9
_cod_database_code               4309077