A convenient synthetic route to substituted phosphavinyl Grignard reagents: synthesis and characterisation of [{RPC(But)MgX(OEt2)}2] (R = cyclohexyl, cyclopentyl, ethyl or mesityl; X = Cl or Br) †
Hibbs, David E.; Jones, Cameron; Richards, Anne F.; Journal of the Chemical Society, Dalton Transactions  (1999) 3531–; doi:10.1039/a906839b

data_7027786
_publ_section_title
;
 A convenient synthetic route to substituted phosphavinyl Grignard
 reagents: synthesis and characterisation of
 [{RP&#xE006;C(But)MgX(OEt2)}2] (R&#x2005;=&#x2005;cyclohexyl,
 cyclopentyl, ethyl or mesityl; X&#x2005;=&#x2005;Cl or
 Br)&#x200A;&#x2020;
;
_journal_issue                   20
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3531
_journal_paper_doi               10.1039/a906839b
_journal_year                    1999
_chemical_formula_sum            'C14 H28 Cl Mg O P'
_chemical_formula_weight         303.10
_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                70.69(2)
_cell_angle_beta                 75.440(18)
_cell_angle_gamma                78.995(16)
_cell_formula_units_Z            4
_cell_length_a                   8.162(9)
_cell_length_b                   9.682(7)
_cell_length_c                   12.341(10)
_cell_measurement_reflns_used    3583
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.29
_cell_measurement_theta_min      2.60
_cell_volume                     884.6(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0215
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3583
_diffrn_reflns_theta_full        26.29
_diffrn_reflns_theta_max         26.29
_diffrn_reflns_theta_min         2.60
_exptl_absorpt_coefficient_mu    0.331
_exptl_absorpt_correction_T_max  0.668
_exptl_absorpt_correction_T_min  0.954
_exptl_absorpt_correction_type   Diffabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.138
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.256
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         3583
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0346
_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^)+(0.0568P)^2^+0.2942P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0951
_refine_ls_wR_factor_ref         0.0972
_reflns_number_gt                3256
_reflns_number_total             3583
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            906839Bsup1.cif
_cod_data_source_block           compound2
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C14 H28 Cl1 Mg1 O1 P1'
_cod_database_code               7027786