Triphenylphosphine oxide‒2-(4-hydroxybenzenyl)-4,4,5,5-tetramethylimidazolidine-1-oxyl 3-oxide (1/1)
Jing, Lin-Lin; Wang, Hai-Bo; Sun, Xiao-Li; Acta Crystallographica Section E 65 (2009) o2444–; doi:10.1107/S160053680903356X

data_2223514
_publ_section_title
;
 Triphenylphosphine
 oxide--2-(4-hydroxybenzenyl)-4,4,5,5-tetramethylimidazolidine-1-oxyl
 3-oxide (1/1)
;
_journal_coeditor_code           PB2003
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2444
_journal_paper_doi               10.1107/S160053680903356X
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C18 H15 O P, C13 H17 N2 O3'
_chemical_formula_moiety         'C18 H15 O P, C13 H17 N2 O3'
_chemical_formula_sum            'C31 H32 N2 O4 P'
_chemical_formula_weight         527.56
_chemical_name_systematic
;
Triphenylphosphine
oxide--2-(4-hydroxybenzenyl)-4,4,5,5-tetramethylimidazolidine-1-oxyl 3-oxide
(1/1)
;
_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                86.386(2)
_cell_angle_beta                 82.724(2)
_cell_angle_gamma                77.318(2)
_cell_formula_units_Z            2
_cell_length_a                   8.8431(11)
_cell_length_b                   12.0786(15)
_cell_length_c                   13.9649(16)
_cell_measurement_reflns_used    1409
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      20.64
_cell_measurement_theta_min      2.38
_cell_volume                     1442.6(3)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'APEX2 (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \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  0.0235
_diffrn_reflns_av_sigmaI/netI    0.0599
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7342
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         2.23
_exptl_absorpt_coefficient_mu    0.132
_exptl_absorpt_correction_T_max  0.9787
_exptl_absorpt_correction_T_min  0.9505
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             558
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.195
_refine_diff_density_min         -0.267
_refine_ls_extinction_coef       0.0101(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         5071
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0801
_refine_ls_R_factor_gt           0.0451
_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^)+(0.05P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1059
_refine_ls_wR_factor_ref         0.1238
_reflns_number_gt                2859
_reflns_number_total             5071
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            pb2003.cif
_cod_data_source_block           I
_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               2223514
_cod_database_fobs_code          2223514