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_7012711
_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         'C35 H32 Cl2 Mo2 O4 P2, C H N'
_chemical_formula_sum            'C36 H33 Cl2 Mo2 N O4 P2'
_chemical_formula_weight         868.35
_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                 114.96(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.763(5)
_cell_length_b                   15.343(5)
_cell_length_c                   17.538(5)
_cell_measurement_reflns_used    6938
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      69.97
_cell_measurement_theta_min      3.30
_cell_volume                     3601(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 0.989
_diffrn_measured_fraction_theta_max 0.989
_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      0.0204518
_diffrn_orient_matrix_UB_12      0.0283964
_diffrn_orient_matrix_UB_13      -0.0416920
_diffrn_orient_matrix_UB_21      -0.0645093
_diffrn_orient_matrix_UB_22      0.0327636
_diffrn_orient_matrix_UB_23      -0.0240206
_diffrn_orient_matrix_UB_31      0.0314986
_diffrn_orient_matrix_UB_32      0.0486624
_diffrn_orient_matrix_UB_33      0.0405016
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0320
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6752
_diffrn_reflns_theta_full        69.97
_diffrn_reflns_theta_max         69.97
_diffrn_reflns_theta_min         3.30
_exptl_absorpt_coefficient_mu    8.229
_exptl_absorpt_correction_T_max  0.150
_exptl_absorpt_correction_T_min  0.085
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'XABS (Parkin, Moezzi & Hope, 1995)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.724
_refine_diff_density_min         -1.045
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         6752
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0375
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0127P)^2^+10.5670P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0836
_refine_ls_wR_factor_ref         0.0842
_reflns_number_gt                6548
_reflns_number_total             6752
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b300350g.txt
_cod_data_source_block           7
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7012711