The Mo(CO)3 Fragment as an Organometallic Protection Group in the Synthesis of Functionalized Tripodal Phosphine Ligands
Philipp Stössel; Hermann A. Mayer; Cäcilia Maichle-Mössmer; Riad Fawzi; Manfred Steimann; Inorganic Chemistry 35 (1996) 5860–5867; doi:10.1021/ic9602512

data_4323908
_publ_section_title
;
 The Mo(CO)3 Fragment as an Organometallic Protection Group in the
 Synthesis of Functionalized Tripodal Phosphine Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5860
_journal_page_last               5867
_journal_paper_doi               10.1021/ic9602512
_journal_volume                  35
_journal_year                    1996
_chemical_formula_sum            'C51 H51 Mo O6 P3'
_chemical_formula_weight         948.77
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 96.51(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.705(5)
_cell_length_b                   16.941(9)
_cell_length_c                   22.526(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      15
_cell_volume                     4438(4)
_computing_cell_refinement       'Siemens P4'
_computing_data_collection       'Siemens P4'
_computing_data_reduction        'Siemens XDISK'
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  'Siemens XCIF'
_computing_structure_refinement  'SHELXTL-5.03 (Sheldrick, 1995)'
_computing_structure_solution    'SHELXTL-5.03 (Sheldrick, 1995)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       'Omega Scan'
_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  0.0912
_diffrn_reflns_av_sigmaI/netI    0.0715
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            31234
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.06
_diffrn_standards_interval_count 58
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.455
_exptl_crystal_colour            colerless
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_description       cube
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.386
_refine_diff_density_min         -1.808
_refine_diff_density_rms         0.156
_refine_ls_extinction_coef       0.0002(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.544
_refine_ls_goodness_of_fit_obs   1.612
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     551
_refine_ls_number_reflns         7826
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.544
_refine_ls_restrained_S_obs      1.612
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_obs          0.0540
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;  
 calc [0.00000+1.00000exp(5.00(sin\q/\l)^2^)]/ 
   [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.1059P)^2^+0.0000sin\q/\l] 
 where P = 0.33333Fo^2^ + 0.66667Fc^2^ 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1599
_refine_ls_wR_factor_obs         0.1375
_reflns_number_observed          5430
_reflns_number_total             7826
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9602512_2.cif
_cod_data_source_block           mayer15
_cod_original_cell_volume        4437.9(34)
_cod_database_code               4323908