Intra- and intermolecular interactions and water pincer in the crystal structure of a 3-P(O)Ph2 substituted 1,2,3,6-tetrahydrophosphinine oxide hydrate
Mátyás Czugler; Tamás Körtvélyesi; László Fábián; Melinda Sipos; György Keglevich; CrystEngComm 9 (2007) 561–; doi:10.1039/b702137b

data_7202814
_publ_section_title
;
 Intra- and intermolecular interactions and water pincer in the crystal
 structure of a 3-P(O)Ph2 substituted 1,2,3,6-tetrahydrophosphinine
 oxide hydrate
;
_journal_issue                   7
_journal_name_full               CrystEngComm
_journal_page_first              561
_journal_paper_doi               10.1039/b702137b
_journal_volume                  9
_journal_year                    2007
_chemical_formula_moiety         'C24 H23 Cl O2 P2, H2 O'
_chemical_formula_sum            'C24 H25 Cl O3 P2'
_chemical_formula_weight         458.83
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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            8
_cell_length_a                   12.277(2)
_cell_length_b                   16.356(2)
_cell_length_c                   23.341(4)
_cell_measurement_reflns_used    55211
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.56
_cell_measurement_theta_min      3.04
_cell_volume                     4686.9(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku R-Axis Rapid'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_sigmaI/netI    0.0149
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            69157
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.04
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.322
_exptl_absorpt_correction_T_max  0.9331
_exptl_absorpt_correction_T_min  0.8692
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.59
_exptl_crystal_size_mid          0.54
_exptl_crystal_size_min          0.49
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.223
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         5363
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0368
_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^)+(0.0543P)^2^+1.3426P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0979
_refine_ls_wR_factor_ref         0.1021
_reflns_number_gt                4339
_reflns_number_total             5363
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b702137b.txt
_cod_data_source_block           sm01
_cod_original_cell_volume        4686.9(13)
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7202814