Diethyl 5-Bis(diphenylphosphinoyl)methyl-2-hydroxy-3-<i>tert</i>-butylphenylphosphonate Hydrate at 173K
Ramm, M.; Costisella, B.; Acta Crystallographica Section C 52 (1996) 2305–2307; doi:10.1107/S0108270196003903

data_2005380
_publ_section_title
;Diethyl
 5-Bis(diphenylphosphinoyl)methyl-2-hydroxy-3-<i>tert</i>-butylphenylphosphonate
 Hydrate at 173K
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              2305
_journal_page_last               2307
_journal_paper_doi               10.1107/S0108270196003903
_journal_volume                  52
_journal_year                    1996
_chemical_formula_moiety         'C39 H43 O6 P3, H2 O'
_chemical_formula_sum            'C39 H45 O7 P3'
_chemical_formula_weight         718.70
_chemical_melting_point          448.6(5)
_chemical_name_systematic
;
(4-Hydroxy-3-diethylphosphono-5-tert-butyl-phenyl)-bis-(diphenylphosphinyl)-
methane
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_type_scat_source           IntTabIV
_audit_creation_method           'PLATON TABLE ACC option'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.233(2)
_cell_length_b                   17.313(2)
_cell_length_c                   13.300(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173
_cell_measurement_theta_max      46
_cell_measurement_theta_min      36
_cell_volume                     3737.9(7)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'MolEN PROCESS (Fair, 1990)'
_computing_publication_material  'PLATON  (Spek, 1990)'
_computing_structure_refinement  'MolEN LSFM'
_computing_structure_solution    'MULTAN11/82 (Main et al., 1982)'
_diffrn_ambient_temperature      173
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0
_diffrn_reflns_av_sigmaI/netI    0.0
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3774
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_max         70
_diffrn_reflns_theta_min         1.5
_diffrn_standards_decay_%        -4.0
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.85
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.270
_refine_diff_density_min         -0.092
_refine_ls_extinction_coef       5.47333E-7
_refine_ls_extinction_method     'Zachariasen (1963)'
_refine_ls_goodness_of_fit_obs   2.274
_refine_ls_hydrogen_treatment
;
All H atoms located in difference synthesis refined except for H1OW and H2OW
for which only U's refined
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     617
_refine_ls_number_reflns         3443
_refine_ls_R_factor_obs          0.044
_refine_ls_shift/esd_max         0.15
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/\s^2^(F)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.059
_reflns_number_observed          3443
_reflns_number_total             3774
_reflns_observed_criterion       F>3.0\s(F)
_cod_data_source_file            ka1188.cif
_cod_data_source_block           ramm
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '175-176 C' was changed to '448.6(5)'
- it was converted from degrees Celsius(C) to Kelvins(K), the average
value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w = 1/\s^2^(F)' was changed
to 'calc'. New tag '_refine_ls_weighting_details' was created. The
value of the new tag was set to 'w = 1/\s^2^(F)'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3737.7(7)
_cod_database_code               2005380