4-Nitrobenzyl 3-oxo-2-(triphenylphosphoranylidene)butanoate
Shi-Jun Li; Jian-Hua Zhong; Acta Crystallographica Section E 62 (2006) o642–o643; doi:10.1107/S1600536806001280

data_2208161
_publ_section_title
;
 4-Nitrobenzyl 3-oxo-2-(triphenylphosphoranylidene)butanoate
;
_journal_coeditor_code           SG6053
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o642
_journal_page_last               o643
_journal_paper_doi               10.1107/S1600536806001280
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C29 H24 N O5 P'
_chemical_formula_moiety         'C29 H24 N O5 P'
_chemical_formula_sum            'C29 H24 N O5 P'
_chemical_formula_weight         497.46
_chemical_name_systematic
;
4-Nitrobenzyl 3-oxo-2-(triphenylphosphoranylidene)butanoate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 93.928(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   39.826(3)
_cell_length_b                   8.1857(6)
_cell_length_c                   15.1786(10)
_cell_measurement_reflns_used    15308
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      55.06
_cell_measurement_theta_min      6.15
_cell_volume                     4936.7(6)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2004)'
_computing_molecular_graphics    SHELXL97
_computing_publication_material  'CrystalStructure and PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0667
_diffrn_reflns_av_sigmaI/netI    0.0571
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -51
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_diffrn_reflns_limit_k_min       -10
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_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22380
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.08
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.152
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_T_min  0.955
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.240
_refine_diff_density_min         -0.325
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         5612
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.1009
_refine_ls_R_factor_gt           0.0535
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0028P)^2^+8.1979P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0857
_refine_ls_wR_factor_ref         0.1065
_reflns_number_gt                3278
_reflns_number_total             5612
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sg6053.cif
_cod_data_source_block           I
_cod_original_cell_volume        4936.6(6)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2208161
_cod_database_fobs_code          2208161