Reactivity of the labile complex [MoCl(η3-allyl)(CO)2(NCMe)2] with diphosphanes
Pérez, Julio; Morales, Dolores; Riera, Víctor; Rodríguez, Amor; García-Granda, Santiago; Dalton Transactions  (2003) 1641–; doi:10.1039/b300350g

data_7012710
_publ_section_title
;
 Reactivity of the labile complex [MoCl(\h3-allyl)(CO)2(NCMe)2] with
 diphosphanes
;
_journal_issue                   8
_journal_name_full               'Dalton Transactions'
_journal_page_first              1641
_journal_paper_doi               10.1039/b300350g
_journal_year                    2003
_chemical_formula_moiety         'C34 H35 Cl Mo O3 P2'
_chemical_formula_sum            'C34 H35 Cl Mo O3 P2'
_chemical_formula_weight         684.95
_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                 123.229(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.119(5)
_cell_length_b                   10.830(5)
_cell_length_c                   23.494(5)
_cell_measurement_reflns_used    8452
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70
_cell_measurement_theta_min      3.49
_cell_volume                     3218(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collet (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2000)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF-96 (Beurskens, 1996)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.0339153
_diffrn_orient_matrix_UB_12      0.0192657
_diffrn_orient_matrix_UB_13      -0.0392624
_diffrn_orient_matrix_UB_21      -0.0383669
_diffrn_orient_matrix_UB_22      -0.0588777
_diffrn_orient_matrix_UB_23      -0.0291683
_diffrn_orient_matrix_UB_31      -0.0425366
_diffrn_orient_matrix_UB_32      0.0684670
_diffrn_orient_matrix_UB_33      -0.0140352
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_sigmaI/netI    0.0495
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            11578
_diffrn_reflns_theta_full        70.00
_diffrn_reflns_theta_max         70.00
_diffrn_reflns_theta_min         3.49
_exptl_absorpt_coefficient_mu    5.294
_exptl_absorpt_correction_T_max  0.651
_exptl_absorpt_correction_T_min  0.460
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'XABS (Parkin, Moezzi & Hope, 1995)'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.964
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         6058
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0365
_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^)+(0.0451P)^2^+1.5536P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0863
_refine_ls_wR_factor_ref         0.0923
_reflns_number_gt                4952
_reflns_number_total             6058
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b300350g.txt
_cod_data_source_block           6
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7012710