<i>N</i>-Allyl-4,6-bis(diphenylphosphino)phenoxazine-10-carboxamide
Ricken, Stefan; Schürmann, Markus; Preut, Hans; Eilbracht, Peter; Acta Crystallographica Section E 62 (2006) o2637–o2638; doi:10.1107/S1600536806020320

data_2209512
_publ_section_title
;
 <i>N</i>-Allyl-4,6-bis(diphenylphosphino)phenoxazine-10-carboxamide
;
_journal_coeditor_code           HB2073
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2637
_journal_page_last               o2638
_journal_paper_doi               10.1107/S1600536806020320
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C40 H32 N2 O2 P2'
_chemical_formula_moiety         'C40 H32 N2 O2 P2'
_chemical_formula_sum            'C40 H32 N2 O2 P2'
_chemical_formula_weight         634.62
_chemical_name_systematic
;
N-Allyl-4,6-bis(diphenylphosphino)phenoxazine-10-carboxamide
;
_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                115.644(4)
_cell_angle_beta                 97.432(5)
_cell_angle_gamma                92.527(4)
_cell_formula_units_Z            2
_cell_length_a                   11.3740(7)
_cell_length_b                   12.5567(8)
_cell_length_c                   13.1164(12)
_cell_measurement_reflns_used    26936
_cell_measurement_temperature    291.0(10)
_cell_measurement_theta_max      27.56
_cell_measurement_theta_min      3.02
_cell_volume                     1664.1(2)
_computing_cell_refinement
;
DENZO and SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction
;
DENZO and SCALEPACK
;
_computing_molecular_graphics    'SHELXTL-Plus (Sheldrick, 1991)'
_computing_publication_material
;
SHELXL97, PARST95 (Nardelli, 1995) and PLATON (Spek, 2003)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      291.0(10)
_diffrn_detector_area_resol_mean '19 vertical, 18 horizontal'
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method
;
517 frames via \w-rotation (\D\w=1\%) and two times 10 s per frame
(five sets at different \k-angles)
;
_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  0.032
_diffrn_reflns_av_sigmaI/netI    0.0849
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            26936
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         3.02
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.169
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.294
_refine_diff_density_min         -0.246
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         7593
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0987
_refine_ls_R_factor_gt           0.0443
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0298P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0882
_refine_ls_wR_factor_ref         0.0931
_reflns_number_gt                3761
_reflns_number_total             7593
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb2073.cif
_cod_data_source_block           I
_cod_database_code               2209512
_cod_database_fobs_code          2209512