Syntheses, spectroscopic study and X-ray crystallography of some new phosphoramidates and lanthanide(III) complexes of <i>N</i>-(4-nitrobenzoyl)-<i>N</i>',<i>N</i>''-bis(morpholino)phosphoric triamide
Gholivand, Khodayar; Mostaanzadeh, Hossein; Koval, Tomas; Dusek, Michal; Erben, Mauricio F.; Stoeckli-Evans, Helen; Della Védova, Carlos O.; Acta Crystallographica Section B 66 (2010) 441–450; doi:10.1107/S0108768110018550

data_2104799
_publ_section_title
;
 Syntheses, spectroscopic study and X-ray crystallography of some new
 phosphoramidates and lanthanide(III) complexes of
 <i>N</i>-(4-nitrobenzoyl)-<i>N</i>',<i>N</i>''-bis(morpholino)phosphoric
 triamide
;
_journal_coeditor_code           PS5006
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              441
_journal_page_last               450
_journal_paper_doi               10.1107/S0108768110018550
_journal_volume                  66
_journal_year                    2010
_chemical_formula_moiety         'C15 H21 N4 O4 P1'
_chemical_formula_sum            'C15 H21 N4 O4 P'
_chemical_formula_weight         352.3
_chemical_name_systematic        ' ?'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                109.909(2)
_cell_angle_beta                 110.445(2)
_cell_angle_gamma                96.024(2)
_cell_formula_units_Z            2
_cell_length_a                   9.1631(2)
_cell_length_b                   9.3224(2)
_cell_length_c                   11.4353(3)
_cell_measurement_reflns_used    10101
_cell_measurement_temperature    120
_cell_measurement_theta_max      39.2038
_cell_measurement_theta_min      2.9638
_cell_volume                     832.34(4)
_computing_cell_refinement       'Crysalis RED (Oxford diffraction, 2007)'
_computing_data_collection       'Crysalis CCD (Oxford diffraction, 2007)'
_computing_data_reduction        'Crysalis RED (Oxford diffraction, 2007)'
_computing_molecular_graphics    'Diamond (Brandenburg & Putz, 2005)'
_computing_publication_material
'Jana2006 (Petricek, Dusek & Palatinus, 2006)'
_computing_structure_refinement
'Jana2006 (Petricek, Dusek & Palatinus, 2006)'
_computing_structure_solution    'Superflip(Palatinus L., Chapuis G., 2007)'
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 8.3438
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device       'four-cycle diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction CCD'
_diffrn_measurement_method
'Rotation method data acquisition using \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0155
_diffrn_reflns_av_sigmaI/netI    0.0106
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10200
_diffrn_reflns_reduction_process
; Integration of the CCD images was done by program Crysalis RED
(Oxford diffraction, 2007). The same program was used for indexing of the
crystal shape and absorption correction.
;
_diffrn_reflns_theta_full        26.53
_diffrn_reflns_theta_max         26.53
_diffrn_reflns_theta_min         2.97
_exptl_absorpt_coefficient_mu    0.193
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94244
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.16 (release 23-01-2008 CrysAlis171 .NET)
(compiled Jan 23 2008,18:08:03)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.4054
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular shape'
_exptl_crystal_F_000             372
_exptl_crystal_size_max          0.9801
_exptl_crystal_size_mid          0.3608
_exptl_crystal_size_min          0.2244
_refine_diff_density_max         0.49
_refine_diff_density_min         -0.44
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   3.18
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_constraints    100
_refine_ls_number_parameters     225
_refine_ls_number_reflns         3460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.0389
_refine_ls_shift/su_mean         0.0019
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/(\s^2^(I)+0.0004I^2^)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0945
_refine_ls_wR_factor_ref         0.0955
_reflns_number_gt                2983
_reflns_number_total             3460
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            ps5006.cif
_cod_data_source_block           5
_cod_original_cell_volume        832.33(4)
_cod_original_formula_sum        'C15 H21 N4 O4 P1'
_cod_database_code               2104799