The reactivity of acyl chlorides towards sodium phosphaethynolate, Na(OCP): a mechanistic case study
Heift, Dominikus; Benkő, Zoltán; Suter, Riccardo; Verel, René; Grützmacher, Hansjörg; Chem. Sci. 7 (2016) 6125–; doi:10.1039/C6SC01269H

data_1543489
_publ_section_title
;
 The reactivity of acyl chlorides towards sodium phosphaethynolate,
 Na(OCP): a mechanistic case study
;
_journal_issue                   9
_journal_name_full               'Chem. Sci.'
_journal_page_first              6125
_journal_paper_doi               10.1039/C6SC01269H
_journal_volume                  7
_journal_year                    2016
_chemical_formula_moiety         'C21 H22 O3 P2'
_chemical_formula_sum            'C21 H22 O3 P2'
_chemical_formula_weight         384.33
_chemical_properties_physical
'air-sensitive, moisture-sensitive, photo-sensitive'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_audit_update_record
;
2014-02-13 deposited with the CCDC.
2016-05-31 downloaded from the CCDC.
;
_cell_angle_alpha                102.227(6)
_cell_angle_beta                 90.177(6)
_cell_angle_gamma                90.407(6)
_cell_formula_units_Z            2
_cell_length_a                   7.1039(5)
_cell_length_b                   8.2133(6)
_cell_length_c                   17.3480(12)
_cell_measurement_temperature    120(2)
_cell_volume                     989.20(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.900
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_av_sigmaI/netI    0.0391
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19150
_diffrn_reflns_theta_full        26.36
_diffrn_reflns_theta_max         29.02
_diffrn_reflns_theta_min         3.03
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.237
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             404
_exptl_crystal_recrystallization_method THF
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         4744
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0476
_refine_ls_shift/su_max          0.079
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0883P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1280
_refine_ls_wR_factor_ref         0.1319
_reflns_number_gt                4256
_reflns_number_total             4744
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6sc01269h2.cif
_cod_data_source_block           dh2_056
_cod_depositor_comments
'Adding full bibliography for 1543489--1543491.cif.'
_cod_database_code               1543489