Nucleophilic behaviour of dioxo- and thiooxophosphorane complexes [MoCp(CO)2{E,P-EP(O)(2,4,6-C6H2(t)Bu3)}](-) (E = O, S).
Alonso, María; Alvarez, M. Angeles; García, M Esther; García-Vivó, Daniel; Ruiz, Miguel A.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 16074–16083; doi:10.1039/c4dt01942c

data_7032633
_publ_section_title
;
 Nucleophilic behaviour of dioxo- and thiooxophosphorane complexes
 [MoCp(CO)2{E,P-EP(O)(2,4,6-C6H2(t)Bu3)}](-) (E = O, S).
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16074
_journal_page_last               16083
_journal_paper_doi               10.1039/c4dt01942c
_journal_volume                  43
_journal_year                    2014
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C28 H43 Mo1 O3 P1 S1 Si1'
_chemical_formula_sum            'C28 H43 Mo O3 P S Si'
_chemical_formula_weight         614.69
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 106.4360(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.9470(3)
_cell_length_b                   10.0787(2)
_cell_length_c                   21.2080(4)
_cell_measurement_reflns_used    5419
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      68.251
_cell_measurement_theta_min      2.209
_cell_measurement_wavelength     1.54184
_cell_volume                     3064.35(11)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
;
 HKL Denzo and Scalepack (Otwinowski & Minor, 1997) 
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF (1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       '90 mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0476
_diffrn_reflns_av_unetI/netI     0.0449
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            19119
_diffrn_reflns_theta_full        68.21
_diffrn_reflns_theta_max         68.21
_diffrn_reflns_theta_min         3.08
_exptl_absorpt_coefficient_mu    5.205
_exptl_absorpt_correction_T_max  1.200
_exptl_absorpt_correction_T_min  0.843
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.398
_refine_diff_density_min         -0.787
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         5568
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0537
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+34.3529P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1473
_refine_ls_wR_factor_ref         0.1575
_reflns_number_gt                4899
_reflns_number_total             5568
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt01942c2.cif
_cod_data_source_block           compound9
_cod_depositor_comments
'Adding full bibliography for 7032632--7032633.cif.'
_cod_original_cell_volume        3064.35(10)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C28 H43 Mo1 O3 P1 S1 Si1'
_cod_database_code               7032633