Synthesis and structures of stable phosphorus zwitterions derived from mesoionic 4_trifluoroacetyl-1,3-oxazolium-5-olates
Ryosuke; Saijo; Hidemitsu; Uno; Shigeki; Mori; Masami; Kawase; Chem.Commun. 52 (2016) 8006–; doi:

data_7119440
_publ_section_title
;
 Synthesis and structures of stable phosphorus zwitterions derived from
 mesoionic 4_trifluoroacetyl-1,3-oxazolium-5-olates
;
_journal_name_full               Chem.Commun.
_journal_page_first              8006
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C29 H36 Br F3 N O3 P'
_chemical_formula_sum            'C29 H36 Br F3 N O3 P'
_chemical_formula_weight         614.48
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_update_record
;
2015-12-07 deposited with the CCDC.
2016-05-26 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 102.525(10)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   9.477(5)
_cell_length_b                   15.308(8)
_cell_length_c                   21.114(11)
_cell_measurement_reflns_used    9517
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.27
_cell_measurement_theta_min      1.98
_cell_volume                     2990(3)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla, et al., 2005)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0553
_diffrn_reflns_av_unetI/netI     0.0430
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            53271
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.996
_diffrn_reflns_theta_min         1.976
_exptl_absorpt_coefficient_mu    1.480
_exptl_absorpt_correction_T_max  0.801
_exptl_absorpt_correction_T_min  0.710
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1272.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         1.980
_refine_diff_density_min         -1.220
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.167
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     343
_refine_ls_number_reflns         8684
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.167
_refine_ls_R_factor_all          0.0874
_refine_ls_R_factor_gt           0.0717
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1041P)^2^+0.1945P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1832
_refine_ls_wR_factor_ref         0.1968
_reflns_number_gt                6943
_reflns_number_total             8685
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c6cc01627h2.cif
_cod_data_source_block           Saijo
_cod_database_code               7119440
_shelxl_version_number           2013-2
_shelx_res_checksum              98203