The synthesis and structural characterisation of some azo-containing phosphine chalcogenides and comparison to non-phosphorus-containing analogues
Alder, Mark J.; Bates, Vanessa M.; Cross, Wendy I.; Flower, Kevin R.; Pritchard, Robin G.; Journal of the Chemical Society, Perkin Transactions 1  (2001) 2669–; doi:10.1039/b104918f

data_7216896
_publ_section_title
;
 The synthesis and structural characterisation of some azo-containing
 phosphine chalcogenides and comparison to non-phosphorus-containing
 analogues
;
_journal_issue                   20
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 1'
_journal_page_first              2669
_journal_paper_doi               10.1039/b104918f
_journal_year                    2001
_chemical_formula_moiety         'C14 H14 N2 O1'
_chemical_formula_sum            'C14 H14 N2 O'
_chemical_formula_weight         226.27
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 96.99(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.809(4)
_cell_length_b                   18.173(7)
_cell_length_c                   11.540(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     1209.2(11)
_computing_cell_refinement       'CAD4 (Nonius, 1984)'
_computing_data_collection       'CAD4 (Nonius, 1984)'
_computing_data_reduction        'XCAD4/WingX (Farrugia, 1998)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_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  0.0706
_diffrn_reflns_av_sigmaI/netI    0.0469
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2194
_diffrn_reflns_theta_full        65.08
_diffrn_reflns_theta_max         65.08
_diffrn_reflns_theta_min         4.56
_exptl_absorpt_coefficient_mu    0.634
_exptl_absorpt_correction_T_max  0.8575
_exptl_absorpt_correction_T_min  0.8085
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.160
_refine_diff_density_min         -0.143
_refine_diff_density_rms         0.033
_refine_ls_extinction_coef       0.0041(10)
_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   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         1981
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0793P)^2^+0.1911P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1322
_refine_ls_wR_factor_ref         0.1550
_reflns_number_gt                1296
_reflns_number_total             1981
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b104918f.txt
_cod_data_source_block           comp5
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 
;
_cod_original_cell_volume        1209.1(11)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7216896