Phosphorus containing mixed anhydrides-their preparation, labile behaviour and potential routes to their stabilisation.
Coetzee, Jacorien; Eastham, Graham R.; Slawin, Alexandra M. Z.; Cole-Hamilton, David J; Organic & biomolecular chemistry 10 (2012) 3677–3688; doi:10.1039/c2ob07164a

data_7152314
_publ_section_title
;
 Phosphorus containing mixed anhydrides-their preparation, labile
 behaviour and potential routes to their stabilisation.
;
_journal_issue                   18
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              3677
_journal_page_last               3688
_journal_paper_doi               10.1039/c2ob07164a
_journal_volume                  10
_journal_year                    2012
_chemical_formula_moiety         'C32 H39 O4 P'
_chemical_formula_sum            'C32 H39 O4 P'
_chemical_formula_weight         518.60
_chemical_melting_point          438.1(10)
_chemical_name_common
phenylacetyl-(5,5',6,6'-tetramethyl-3,3'-di-tert-butyl-1,1'-biphenyl-2,2'-diyl)phosphite
_chemical_name_systematic
'4,8-di-tert-butyl-1,2,10,11-tetramethyldibenzo[d,f][1,3,2]dioxaphosphepin-6-yl 2-phenylacetate'
_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                 98.366(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.820(7)
_cell_length_b                   16.178(10)
_cell_length_c                   15.982(10)
_cell_measurement_reflns_used    9258
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      28.9
_cell_measurement_theta_min      2.3
_cell_volume                     2768(3)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2004)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2004)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2004)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.2879
_diffrn_reflns_av_sigmaI/netI    0.3208
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18083
_diffrn_reflns_theta_full        25.46
_diffrn_reflns_theta_max         25.46
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    0.135
_exptl_absorpt_correction_T_max  0.9960
_exptl_absorpt_correction_T_min  0.9801
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.189
_refine_diff_density_min         -1.314
_refine_diff_density_rms         0.184
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         5075
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.2445
_refine_ls_R_factor_gt           0.1477
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1809P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3207
_refine_ls_wR_factor_ref         0.3668
_reflns_number_gt                2310
_reflns_number_total             5075
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ob07164a.txt
_cod_data_source_block           compound11
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '164-166 deg C' was changed to
'438.1(10)' - it was converted from degrees Celsius(C) to Kelvins(K),
the average value was taken and precision was
estimated.

'_symmetry_cell_setting' value 'Monoclinic' changed to
'monoclinic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_Hall     -P2yn
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7152314