Activation of cyanamide by a molybdenum(0) diphosphinic centre. Formation of cyanoimide and its reactivity with electrophiles
Cunha, Sónia M. P. R. M.; Guedes da Silva, M. Fátima C.; Pombeiro, Armando J. L.; Journal of the Chemical Society, Dalton Transactions  (2002) 1791–; doi:10.1039/b108165a

data_7011154
_publ_section_title
;
 Activation of cyanamide by a molybdenum(0) diphosphinic centre.
 Formation of cyanoimide and its reactivity with electrophiles
;
_journal_issue                   8
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1791
_journal_paper_doi               10.1039/b108165a
_journal_year                    2002
_chemical_formula_sum            'C56 H53 B F4 Mo N4 O P4'
_chemical_formula_weight         1104.65
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.85(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.778(2)
_cell_length_b                   21.290(4)
_cell_length_c                   22.115(4)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.8
_cell_measurement_theta_min      12.2
_cell_volume                     5544.8(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.278
_diffrn_measured_fraction_theta_max 0.278
_diffrn_measurement_device_type  CAD4
_diffrn_measurement_method       theta/2theta
_diffrn_radiation_monochromator  filter
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0155
_diffrn_reflns_av_sigmaI/netI    0.0313
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            7930
_diffrn_reflns_theta_full        22.46
_diffrn_reflns_theta_max         22.46
_diffrn_reflns_theta_min         1.84
_diffrn_standards_decay_%        2
_diffrn_standards_interval_time  100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.407
_exptl_absorpt_correction_T_max  0.9304
_exptl_absorpt_correction_T_min  0.8673
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            dark_brown
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2272
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.543
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     621
_refine_ls_number_reflns         2003
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0468
_refine_ls_shift/su_max          0.773
_refine_ls_shift/su_mean         0.086
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1112P)^2^+7.0505P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1210
_refine_ls_wR_factor_ref         0.1210
_reflns_number_gt                2003
_reflns_number_total             2003
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b108165a.txt
_cod_data_source_block           pmb03
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7011154