1,3-Bis(5,5-dimethyl-2-oxo-1,3,2-dioxaphosphinan-2-yloxy)benzene
Li, Xiao-Jun; Sun, Shu-Juan; Wang, Jing; Wang, Yan-Fei; Acta Crystallographica Section E 63 (2007) o619–o620; doi:10.1107/S1600536806055425

data_2212182
_publ_section_title
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 1,3-Bis(5,5-dimethyl-2-oxo-1,3,2-dioxaphosphinan-2-yloxy)benzene
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_journal_coeditor_code           HB2242
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o619
_journal_page_last               o620
_journal_paper_doi               10.1107/S1600536806055425
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C16 H24 O8 P2'
_chemical_formula_moiety         'C16 H24 O8 P2'
_chemical_formula_sum            'C16 H24 O8 P2'
_chemical_formula_weight         406.29
_chemical_melting_point          440.5(5)
_chemical_name_systematic
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1,3-Bis(5,5-dimethyl-2-oxo-1,3,2-dioxaphosphinan-2-yloxy)benzene
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 97.960(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.646(7)
_cell_length_b                   6.3642(19)
_cell_length_c                   13.795(4)
_cell_measurement_reflns_used    1849
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      23.36
_cell_measurement_theta_min      2.50
_cell_volume                     1969.0(10)
_computing_cell_refinement       'SAINT (Bruker, 1997)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Bruker, 1997)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       \w
_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  0.0312
_diffrn_reflns_av_sigmaI/netI    0.0541
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5559
_diffrn_reflns_theta_full        26.43
_diffrn_reflns_theta_max         26.43
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    0.260
_exptl_absorpt_correction_T_max  0.955
_exptl_absorpt_correction_T_min  0.926
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.219
_refine_diff_density_min         -0.253
_refine_ls_abs_structure_details 'Flack (1983), 1154 Friedel pairs?'
_refine_ls_abs_structure_Flack   0.05(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         3370
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0406
_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^)+(0.0405P)^2^+0.0335P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0783
_refine_ls_wR_factor_ref         0.0895
_reflns_number_gt                2440
_reflns_number_total             3370
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb2242.cif
_cod_data_source_block           I
_cod_depositor_comments
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The following automatic conversions were performed:

'_chemical_melting_point' value '440-441' was changed to '440.5(5)' -
the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '440-441' was changed to '440.5(5)' -
the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               2212182
_cod_database_fobs_code          2212182