3-Chloromethyl-5-methoxy-4-methoxycarbonyl-3-oxo-2,3-dihydro-[1,3]oxaphosphole monohydrate
Ciptadi, Ciptadi; Cristau, Henri Jean; Bekro, Yves Alain; Tillard, Monique; Virieux, David; Acta Crystallographica Section E 60 (2004) o99–o101; doi:10.1107/S1600536803027351

data_2203113
_publ_section_title
;3-Chloromethyl-5-methoxy-4-methoxycarbonyl-3-oxo-2,3-dihydro-[1,3]oxaphosphole
 monohydrate
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o99
_journal_page_last               o101
_journal_paper_doi               10.1107/S1600536803027351
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          'C7 H10 Cl O5 P, H2 O'
_chemical_formula_moiety         'C7 H10 Cl O5 P, H2 O'
_chemical_formula_sum            'C7 H12 Cl O6 P'
_chemical_formula_weight         258.59
_chemical_melting_point          139.5(15)
_chemical_name_systematic
;3-Chloromethyl-5-methoxy-4-methoxycarbonyl-3-oxo-2,3-dihydro-[1,3]oxaphosphole
monohydrate
;
_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                71.019(9)
_cell_angle_beta                 81.102(8)
_cell_angle_gamma                72.999(8)
_cell_formula_units_Z            2
_cell_length_a                   7.6307(7)
_cell_length_b                   8.5404(8)
_cell_length_c                   9.1204(10)
_cell_measurement_reflns_used    9001
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.08
_cell_measurement_theta_min      3.5
_cell_volume                     536.32(10)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2001)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2001)'
_computing_data_reduction        'CrysAlis RED'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Xcalibur 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  0.0395
_diffrn_reflns_av_sigmaI/netI    0.0254
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            9001
_diffrn_reflns_theta_full        30.08
_diffrn_reflns_theta_max         30.08
_diffrn_reflns_theta_min         3.45
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.510
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             268
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.466
_refine_diff_density_min         -0.447
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     144
_refine_ls_number_reflns         3113
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0436
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0758P)^2^+0.1891P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1257
_refine_ls_wR_factor_ref         0.1315
_reflns_number_gt                2695
_reflns_number_total             3113
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            su6060.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '138-141' was changed to '139.5(15)'
- 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 '138-141' was changed to '139.5(15)'
- 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_database_code               2203113
_cod_database_fobs_code          2203113