Phosphoramides bearing isoxazole derivative: spectroscopic and structural characterization, study of hydrogen-bonding interactions and two lanthanide complexes (LnIII = Ce and Eu).
Gholivand, Khodayar; Molaei, Foroogh; Hosseini, Mahdieh; Acta crystallographica Section B, Structural science, crystal engineering and materials 71 (2015) 176–185; doi:10.1107/S2052520615003297

data_2311666
_publ_section_title
;
 Phosphoramides bearing isoxazole derivative: spectroscopic and structural
 characterization, study of hydrogen-bonding interactions and two
 lanthanide complexes (LnIII = Ce and Eu).
;
_journal_issue                   'Pt 2'
_journal_name_full
'Acta crystallographica Section B, Structural science, crystal engineering and materials'
_journal_page_first              176
_journal_page_last               185
_journal_paper_doi               10.1107/S2052520615003297
_journal_volume                  71
_journal_year                    2015
_chemical_formula_moiety         'C14 H15 N4 O4 P'
_chemical_formula_sum            'C14 H15 N4 O4 P'
_chemical_formula_weight         334.27
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.96(4)
_cell_angle_beta                 84.78(3)
_cell_angle_gamma                80.54(2)
_cell_formula_units_Z            4
_cell_length_a                   9.2849(19)
_cell_length_b                   10.835(2)
_cell_length_c                   15.295(3)
_cell_measurement_reflns_used    1098
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      3
_cell_volume                     1511.3(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX II'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker APEX II CCD area detector'
_diffrn_measurement_method       'omega scans'
_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  0.0654
_diffrn_reflns_av_sigmaI/netI    0.0840
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7171
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.34
_exptl_absorpt_coefficient_mu    0.209
_exptl_absorpt_correction_T_max  0.986
_exptl_absorpt_correction_T_min  0.934
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   TWINABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.156
_refine_diff_density_min         -0.650
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     423
_refine_ls_number_reflns         7171
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.1532
_refine_ls_R_factor_gt           0.0976
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+11.7247P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1781
_refine_ls_wR_factor_ref         0.1951
_reflns_number_gt                4896
_reflns_number_total             7171
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            eb5037sup1.cif
_cod_data_source_block           m71
_cod_original_cell_volume        1511.4(5)
_cod_database_code               2311666