Structural studies of (<i>N</i>-phenylthioureidoalkyl- and -aryl)phosphonates
Chęcińska, Lilianna; Fábián, László; Kudzin, Zbigniew H.; Acta Crystallographica Section B 60 (2004) 211–218; doi:10.1107/S0108768104002770

data_2102486
_publ_section_title
;
 Structural studies of (<i>N</i>-phenylthioureidoalkyl- and
 -aryl)phosphonates
;
_journal_date_accepted           2004-02-04
_journal_date_recd_electronic    2003-11-30
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              211
_journal_page_last               218
_journal_paper_category          FA
_journal_paper_doi               10.1107/S0108768104002770
_journal_volume                  60
_journal_year                    2004
_chemical_formula_moiety         'C26 H23 N2 O3 P S'
_chemical_formula_sum            'C26 H23 N2 O3 P S'
_chemical_formula_weight         474.49
_chemical_name_systematic
;
  diphenyl [1-(3-phenylthioureido)benzyl]phosphonate
;
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   direct
_audit_creation_method           SHELXL-97
_cell_angle_alpha                96.660(10)
_cell_angle_beta                 104.450(10)
_cell_angle_gamma                99.840(10)
_cell_formula_units_Z            2
_cell_length_a                   9.9530(10)
_cell_length_b                   10.0460(10)
_cell_length_c                   12.7010(10)
_cell_measurement_reflns_used    22
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.47
_cell_measurement_theta_min      22.59
_cell_volume                     1194.8(2)
_computing_cell_refinement
'MSC/AFC Diffractometer Control Software (1989a)'
_computing_data_collection
'MSC/AFC Diffractometer Control Software (1989a)'
_computing_data_reduction        'TEXSAN (1989b)'
_computing_molecular_graphics    'PLATON (Spek, 1998)'
_computing_publication_material  'PARST97 (Nardelli, 1996)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'AFC5S Rigaku'
_diffrn_measurement_method       '\w '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0187
_diffrn_reflns_av_sigmaI/netI    0.1114
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4431
_diffrn_reflns_theta_full        67.50
_diffrn_reflns_theta_max         67.50
_diffrn_reflns_theta_min         3.64
_diffrn_standards_decay_%        <2
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.086
_exptl_absorpt_correction_T_max  0.83610
_exptl_absorpt_correction_T_min  0.67483
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(De Meulenaer & Tompa, 1965)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       Plate
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.193
_refine_diff_density_min         -0.228
_refine_ls_extinction_coef       0.0060(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         4169
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0986
_refine_ls_R_factor_gt           0.0380
_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
 [1.00000exp(3.00(sin\q/\l)^2^)]/
 [\s^2^(Fo^2^)+0.0000*P+(0.0290P)^2^]
 where P = 0.33333Fo^2^ + 0.66667Fc^2^
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0819
_refine_ls_wR_factor_ref         0.0903
_reflns_number_gt                2147
_reflns_number_total             4169
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            de5004.cif
_cod_data_source_block           II
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2102486
_cod_database_fobs_code          2102486