C-N Bond-Forming Self-Condensation of Amide Promoted by MoCl5 at Room Temperature
Sara Dolci; Fabio Marchetti; Guido Pampaloni; Stefano Zacchini; Inorganic Chemistry 50 (2011) 3846–3848; doi:10.1021/ic2001199

data_4324989
_publ_section_title
;
 C-N Bond-Forming Self-Condensation of Amide Promoted by MoCl5 at Room
 Temperature
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3846
_journal_page_last               3848
_journal_paper_doi               10.1021/ic2001199
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C6 H14 Cl5 Mo N2 O2'
_chemical_formula_weight         419.38
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.499(3)
_cell_angle_beta                 102.981(2)
_cell_angle_gamma                119.087(2)
_cell_formula_units_Z            2
_cell_length_a                   8.7379(17)
_cell_length_b                   8.912(3)
_cell_length_c                   11.400(2)
_cell_measurement_temperature    100(2)
_cell_volume                     725.4(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0245
_diffrn_reflns_av_sigmaI/netI    0.0255
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7984
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    1.812
_exptl_absorpt_correction_T_max  0.7728
_exptl_absorpt_correction_T_min  0.6703
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            bright-green
_exptl_crystal_density_diffrn    1.920
_exptl_crystal_description       prism
_exptl_crystal_F_000             414
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.364
_refine_diff_density_min         -0.787
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         3144
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0421
_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^)+(0.0584P)^2^+2.6593P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1126
_refine_ls_wR_factor_ref         0.1134
_reflns_number_gt                3068
_reflns_number_total             3144
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2001199_si_002.cif
_cod_data_source_block           p-1
_cod_database_code               4324989