Synthesis and Characterization of TpiPrMoO(S2PR2) (R = Pri, Ph, OEt, OPri, (-)-Mentholate) and {HB(OMe)(Pripz)2}MoO(S2PPri2), Including Isomers of Known 1,2-Borotropically-Shifted Complexes
Charles G. Young; Michael S. Malarek; David J. Evans; Christian J. Doonan; Victor Wee Lin Ng; Jonathan M. White; Inorganic Chemistry 48 (2009) 1960–1966; doi:10.1021/ic8015518

data_4301538
_publ_section_title
;
Synthesis and Characterization of TpiPrMoO(S2PR2) (R = Pri, Ph, OEt, OPri,
(-)-Mentholate) and {HB(OMe)(Pripz)2}MoO(S2PPri2), Including Isomers of
Known 1,2-Borotropically-Shifted Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1960
_journal_page_last               1966
_journal_paper_doi               10.1021/ic8015518
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C19 H36 B Mo N4 O2 P S2'
_chemical_formula_sum            'C19 H36 B Mo N4 O2 P S2'
_chemical_formula_weight         554.36
_chemical_name_systematic
; 
(diisopropyldithiophosphinato){hydrobis(isopropyl-
pyrazol-1-yl)(methoxy)borato}oxomolybdenum(IV) 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.6095(5)
_cell_length_b                   14.9183(8)
_cell_length_c                   34.4581(18)
_cell_measurement_reflns_used    9429
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      27.20
_cell_measurement_theta_min      2.25
_cell_volume                     5453.9(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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 0.999
_diffrn_measured_fraction_theta_max 0.996
_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  0.0493
_diffrn_reflns_av_sigmaI/netI    0.0348
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            32094
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.18
_exptl_absorpt_coefficient_mu    0.714
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2304
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.565
_refine_diff_density_min         -0.205
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.932
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         6253
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.932
_refine_ls_R_factor_all          0.0517
_refine_ls_R_factor_gt           0.0340
_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^)+(0.0468P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0766
_refine_ls_wR_factor_ref         0.0825
_reflns_number_gt                4533
_reflns_number_total             6253
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8015518_si_001_4.cif
_cod_data_source_block           {HB(3-iPrC3H2N2)2(OMe)}Mo(S2PiPr2)
_cod_database_code               4301538