Methyl 3-[4,6-bis(diphenylphosphino)phenoxazin-10-yl]propionate
Ricken, Stefan; Osinski, Piotr W.; Schürmann, Markus; Preut, Hans; Eilbracht, Peter; Acta Crystallographica Section E 62 (2006) o1807–o1808; doi:10.1107/S1600536806012438

data_2208981
_publ_section_title
;
 Methyl 3-[4,6-bis(diphenylphosphino)phenoxazin-10-yl]propionate
;
_journal_coeditor_code           RZ2019
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1807
_journal_page_last               o1808
_journal_paper_doi               10.1107/S1600536806012438
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C40 H33 N O3 P2'
_chemical_formula_moiety         'C40 H33 N O3 P2'
_chemical_formula_sum            'C40 H33 N O3 P2'
_chemical_formula_weight         637.61
_chemical_name_systematic
;
Methyl 3-[4,6-bis(diphenylphosphino)phenoxazin-10-yl]propionate
;
_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                68.961(6)
_cell_angle_beta                 84.619(10)
_cell_angle_gamma                80.182(9)
_cell_formula_units_Z            2
_cell_length_a                   10.431(2)
_cell_length_b                   11.354(2)
_cell_length_c                   15.337(3)
_cell_measurement_reflns_used    21372
_cell_measurement_temperature    291.0(10)
_cell_measurement_theta_max      25.38
_cell_measurement_theta_min      2.97
_cell_volume                     1669.5(5)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        DENZO/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, 1990)'
_diffrn_ambient_temperature      291.0(10)
_diffrn_detector_area_resol_mean '19 vertical, 18 horizontal'
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method
;
235 frames via \w-rotation (\D\w=2\%) and two times 75 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  0.033
_diffrn_reflns_av_sigmaI/netI    0.1542
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21372
_diffrn_reflns_theta_full        25.38
_diffrn_reflns_theta_max         25.38
_diffrn_reflns_theta_min         2.97
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.170
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             668
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.16
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_refine_diff_density_min         -0.154
_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
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_refine_ls_number_reflns         6052
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1565
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = [exp{4.20(sin\q/\l}^2^)]/[\s^2^(Fo^2^)]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0697
_refine_ls_wR_factor_ref         0.0882
_reflns_number_gt                2007
_reflns_number_total             6052
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            rz2019.cif
_cod_data_source_block           I
_cod_database_code               2208981
_cod_database_fobs_code          2208981