3,9-Bis(2-hydroxy-2-propyl)-2,4,8,10-tetraoxa-3,9-diphosphaspiro[5.5]undecane 3,9-dioxide hemihydrate
Yu-Hua Zhang; Xiao-Hui Wang; Shan Liu; Cheng Yao; Acta Crystallographica Section E 62 (2006) o2620–o2621; doi:10.1107/S1600536806020605

data_2209544
_publ_section_title
;3,9-Bis(2-hydroxy-2-propyl)-2,4,8,10-tetraoxa-3,9-diphosphaspiro[5.5]undecane
 3,9-dioxide hemihydrate
;
_journal_coeditor_code           HK2053
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2620
_journal_page_last               o2621
_journal_paper_doi               10.1107/S1600536806020605
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C11 H22 O8 P2, 0.5H2 O'
_chemical_formula_moiety         'C11 H22 O8 P2, 0.5H2 O'
_chemical_formula_sum            'C11 H23 O8.5 P2'
_chemical_formula_weight         353.24
_chemical_melting_point          460.15(2)
_chemical_name_systematic
;
3,9-Bis(2-hydroxy-2-propyl)-2,4,8,10-tetraoxa-3,9-diphosphaspiro[5.5]undecane
3,9-dioxide hemihydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_cell_angle_alpha                86.28(3)
_cell_angle_beta                 82.40(3)
_cell_angle_gamma                77.11(3)
_cell_formula_units_Z            4
_cell_length_a                   7.5500(15)
_cell_length_b                   10.539(2)
_cell_length_c                   21.068(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      12
_cell_measurement_theta_min      9
_cell_volume                     1618.7(6)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf--Nonius, 1985)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2000)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Enraf--Nonius CAD-4'
_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  0.0397
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_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
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_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            6846
_diffrn_reflns_theta_full        25.97
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         1.95
_diffrn_standards_decay_%        1
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.306
_exptl_absorpt_correction_T_max  0.9414
_exptl_absorpt_correction_T_min  0.9290
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North <i>et al.</i>,  1968)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             748.0
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.436
_refine_diff_density_min         -0.421
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         6337
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1443
_refine_ls_R_factor_gt           0.0689
_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^)+(0.07P)^2^+2P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1467
_refine_ls_wR_factor_ref         0.1907
_reflns_number_gt                3535
_reflns_number_total             6337
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hk2053.cif
_cod_data_source_block           I
_cod_database_code               2209544
_cod_database_fobs_code          2209544