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_7011153
_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            'C55 H48 B Cl2 F4 Mo N4 P4'
_chemical_formula_weight         1142.50
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 98.93(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.450(4)
_cell_length_b                   12.196(2)
_cell_length_c                   39.540(8)
_cell_measurement_reflns_used    15
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      35.7
_cell_measurement_theta_min      24.2
_cell_volume                     10695(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.727
_diffrn_measured_fraction_theta_max 0.727
_diffrn_measurement_device_type  Nicolet_P3
_diffrn_measurement_method       theta/2theta
_diffrn_radiation_monochromator  filter
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0228
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            4006
_diffrn_reflns_theta_full        50.06
_diffrn_reflns_theta_max         50.06
_diffrn_reflns_theta_min         4.14
_diffrn_standards_decay_%        10
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.511
_exptl_absorpt_correction_T_max  0.4811
_exptl_absorpt_correction_T_min  0.3447
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4664
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.969
_refine_diff_density_min         -0.726
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       0.000013(18)
_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_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     641
_refine_ls_number_reflns         4004
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0742
_refine_ls_R_factor_gt           0.0729
_refine_ls_shift/su_max          0.234
_refine_ls_shift/su_mean         0.034
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1336P)^2^+104.6649P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1938
_refine_ls_wR_factor_ref         0.1964
_reflns_number_gt                3931
_reflns_number_total             4004
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b108165a.txt
_cod_data_source_block           pmb01
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7011153