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_7152313
_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         'C27 H37 O4 P'
_chemical_formula_sum            'C27 H37 O4 P'
_chemical_formula_weight         456.54
_chemical_melting_point          151.5(15)
_chemical_name_common
;
Propionyl-(5,5'6,6'-Tetramethyl-3,3'-di-tert-butyl-1,1-biphenyl)phosphite
;
_chemical_name_systematic
'4,8-di-tert-butyl-1,2,10,11-tetramethyldibenzo[d,f][1,3,2]dioxaphosphepin-6-yl propionate'
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.562(6)
_cell_length_b                   10.686(4)
_cell_length_c                   15.625(6)
_cell_measurement_reflns_used    6096
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      28.3203
_cell_measurement_theta_min      1.9058
_cell_volume                     2598.4(17)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.1675
_diffrn_reflns_av_sigmaI/netI    0.1350
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15727
_diffrn_reflns_theta_full        25.32
_diffrn_reflns_theta_max         25.32
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    0.134
_exptl_absorpt_correction_T_max  0.9920
_exptl_absorpt_correction_T_min  0.9633
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.167
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.957
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.1(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         4127
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.1454
_refine_ls_R_factor_gt           0.0919
_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^)+(0.1260P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2162
_refine_ls_wR_factor_ref         0.2483
_reflns_number_gt                2501
_reflns_number_total             4127
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ob07164a.txt
_cod_data_source_block           compound10
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '150-153' was changed to '151.5(15)'
- the average value was taken and precision was
estimated.

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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_cell_volume        2598.3(17)
_cod_original_sg_symbol_H-M      Pna21
_cod_database_code               7152313