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_4301536
_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         '2(C30 H38 B Mo N6 O P S2), 0.5(C H2 Cl2)'
_chemical_formula_sum            'C60.5 H77 B2 Cl Mo2 N12 O2 P2 S4'
_chemical_formula_weight         1443.47
_chemical_name_systematic
;
 (diphenyldithiophosphinato){hydrotris(3-
isopropylpyrazol-1-yl)borato}oxomolybdenum(IV)
dichloromethane solvate
 
;
_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                 90.3550(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.2135(15)
_cell_length_b                   15.1996(11)
_cell_length_c                   21.5221(15)
_cell_measurement_reflns_used    7152
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.42
_cell_measurement_theta_min      2.34
_cell_volume                     6939.4(9)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1242
_diffrn_reflns_av_sigmaI/netI    0.0887
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            43202
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    0.616
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2980
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.051
_refine_diff_density_min         -0.662
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    geom
_refine_ls_matrix_type           full
_refine_ls_number_parameters     779
_refine_ls_number_reflns         15735
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0456
_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^)+(0.0603P)^2^+0.2779P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1198
_refine_ls_wR_factor_ref         0.1266
_reflns_number_gt                12948
_reflns_number_total             15735
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8015518_si_001_2.cif
_cod_data_source_block           '[TpiPrMoO(S2PPh2)'
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C60.50 H77 B2 Cl Mo2 N12 O2 P2 S4'
_cod_database_code               4301536