Synthesis of the sodium diphenylbis(cyanamido)phosphonium diylide by a new variation of the Staudinger reaction
Taillefer, Marc; Inguimbert, Nicolas; Cristau, Henri-Jean; Jäger, Lothar; Merzweiler, Kurt; Chemical Communications  (1999) 565–; doi:10.1039/a808641i

data_7110408
_publ_section_title
;
 Synthesis of the sodium diphenylbis(cyanamido)phosphonium diylide by a
 new variation of the Staudinger reaction
;
_journal_issue                   6
_journal_name_full               'Chemical Communications'
_journal_page_first              565
_journal_paper_doi               10.1039/a808641i
_journal_year                    1999
_chemical_compound_source        turqoise
_chemical_formula_sum            'C38 H30 Cu N10 P2'
_chemical_formula_weight         752.20
_chemical_melting_point          465.15
_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
_cell_angle_alpha                107.588(8)
_cell_angle_beta                 91.823(11)
_cell_angle_gamma                98.651(11)
_cell_formula_units_Z            2
_cell_length_a                   8.4325(14)
_cell_length_b                   13.5423(12)
_cell_length_c                   16.555(2)
_cell_measurement_temperature    293(2)
_cell_volume                     1775.6(4)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0513
_diffrn_reflns_av_sigmaI/netI    0.0548
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10554
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.45
_exptl_absorpt_coefficient_mu    0.749
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_F_000             774
_refine_diff_density_max         0.378
_refine_diff_density_min         -0.739
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.037
_refine_ls_goodness_of_fit_obs   1.106
_refine_ls_matrix_type           full
_refine_ls_number_parameters     580
_refine_ls_number_reflns         6478
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_restrained_S_obs      1.106
_refine_ls_R_factor_all          0.0739
_refine_ls_R_factor_obs          0.0479
_refine_ls_shift/esd_max         -0.009
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0787P)^2^+0.0554P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1330
_refine_ls_wR_factor_obs         0.1186
_reflns_number_observed          4688
_reflns_number_total             6478
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            808641isup1.cif
_cod_data_source_block           ipds3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '192 C' was changed to '465.15' - it
was converted from degrees Celsius(C) to Kelvins(K).

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0787P)^2^+0.0554P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0787P)^2^+0.0554P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1775.7(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7110408