2,2'-Methylenebis(5,5-dimethyl-1,3,2-dioxaphosphorinane 2-oxide)
Browning, C. S.; Burrow, T. E.; Farrar, D. H.; Lough, A. J.; Acta Crystallographica Section C 52 (1996) 652–654; doi:10.1107/S0108270195014685

data_2004608
_publ_section_title
;
 2,2'-Methylenebis(5,5-dimethyl-1,3,2-dioxaphosphorinane 2-oxide)
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              652
_journal_page_last               654
_journal_paper_doi               10.1107/S0108270195014685
_journal_volume                  52
_journal_year                    1996
_chemical_formula_moiety         'C11 H22 O6 P2'
_chemical_formula_sum            'C11 H22 O6 P2'
_chemical_formula_weight         312.23
_chemical_name_systematic
;
2,2'-Methylenebis[5,5-dimethyl-2,2'-dioxide]1,3,2-
dioxaphosphorinane
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 94.23(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.359(1)
_cell_length_b                   16.752(2)
_cell_length_c                   13.653(1)
_cell_measurement_reflns_used    49
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      35.0
_cell_measurement_theta_min      10.0
_cell_volume                     1450.4(3)
_computing_cell_refinement       'Siemens P4 software'
_computing_data_collection       'Siemens P4 software'
_computing_data_reduction        'Siemens P4 software'
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXTL/PC (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       \w-2\q
_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  0.0210
_diffrn_reflns_av_sigmaI/netI    0.0428
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            3651
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         3.21
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.319
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.405
_refine_diff_density_min         -0.282
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.015
_refine_ls_goodness_of_fit_obs   1.050
_refine_ls_hydrogen_treatment
;
H atoms riding, with SHELXL93 AFIX28 and AFIX138 constraints; C---H
0.94--0.99\%A
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         3375
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_restrained_S_obs      1.050
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_obs          0.0397
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;
calc w = 1/[\s^2^(F~o~^2^) + (0.0489P)^2^ + 0.5869P]
where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.1027
_refine_ls_wR_factor_obs         0.0930
_reflns_number_observed          2648
_reflns_number_total             3376
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            fg1133.cif
_cod_data_source_block           fg1133
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2004608