Synthesis, crystal structure and spectroscopic properties of a novel carbacylamidophosphate: <i>N</i>-(3-nitrobenzoyl)-<i>N</i>',<i>N</i>''-bis(<i>tert</i>-butyl)phosphoric triamide
Gholivand, Khodayar; Mostaanzadeh, Hossein; Koval, Tomas; Dusek, Michal; Erben, Mauricio F.; Della Védova, Carlos O.; Acta Crystallographica Section B 65 (2009) 502–508; doi:10.1107/S0108768109020023

data_2104390
_publ_section_title
;Synthesis, crystal structure and spectroscopic properties of a novel
 carbacylamidophosphate:
 <i>N</i>-(3-nitrobenzoyl)-<i>N</i>',<i>N</i>''-bis(<i>tert</i>-butyl)phosphoric
 triamide
;
_journal_coeditor_code           BP5021
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              502
_journal_page_last               508
_journal_paper_doi               10.1107/S0108768109020023
_journal_volume                  65
_journal_year                    2009
_chemical_formula_sum            'C90 H150 N24 O24 P6'
_chemical_formula_weight         2138.16
_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                87.8019(12)
_cell_angle_beta                 70.8182(13)
_cell_angle_gamma                83.8446(14)
_cell_formula_units_Z            1
_cell_length_a                   13.1528(2)
_cell_length_b                   13.7179(2)
_cell_length_c                   16.5876(2)
_cell_measurement_reflns_used    14590
_cell_measurement_temperature    120
_cell_measurement_theta_max      39.3259
_cell_measurement_theta_min      2.5979
_cell_volume                     2810.41(7)
_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 0.98
_diffrn_measured_fraction_theta_max 0.98
_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  0.0277
_diffrn_reflns_av_sigmaI/netI    0.0387
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            34749
_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        26.54
_diffrn_reflns_theta_max         26.54
_diffrn_reflns_theta_min         2.75
_exptl_absorpt_coefficient_mu    0.172
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_correction_T_min  0.945
_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            'pale yellow'
_exptl_crystal_density_diffrn    1.2629
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular shape'
_exptl_crystal_F_000             1140
_exptl_crystal_size_max          0.6658
_exptl_crystal_size_mid          0.2607
_exptl_crystal_size_min          0.2202
_refine_diff_density_max         0.37
_refine_diff_density_min         -0.35
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.79
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_constraints    300
_refine_ls_number_parameters     679
_refine_ls_number_reflns         11679
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0416
_refine_ls_shift/su_max          0.0460
_refine_ls_shift/su_mean         0.0018
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     w=1/(\s^2^(F)+0.0001F^2^)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0432
_refine_ls_wR_factor_ref         0.0443
_reflns_number_gt                7286
_reflns_number_total             11679
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            bp5021.cif
_cod_data_source_block           I
_cod_database_code               2104390