Solid-state and gas-phase structures of two conformers of <i>N</i>-(4-methylphenyl)-<i>N</i>',<i>N</i>''-bis(morpholinyl) phosphoric triamide; insights from X-ray crystallography and DFT calculations
Gholivand, Khodayar; Mahzouni, Hamid Reza; Acta Crystallographica Section B 67 (2011) 238–243; doi:10.1107/S0108768111010470

data_2104967
_publ_section_title
;
 Solid-state and gas-phase structures of two conformers of
 <i>N</i>-(4-methylphenyl)-<i>N</i>',<i>N</i>''-bis(morpholinyl)
 phosphoric triamide; insights from X-ray crystallography and DFT
 calculations
;
_journal_coeditor_code           SO5046
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              238
_journal_page_last               243
_journal_paper_doi               10.1107/S0108768111010470
_journal_volume                  67
_journal_year                    2011
_chemical_formula_moiety         'C15 H24 N3 O3 P'
_chemical_formula_sum            'C15 H24 N3 O3 P'
_chemical_formula_weight         325.34
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.029(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.517(3)
_cell_length_b                   10.723(3)
_cell_length_c                   32.993(8)
_cell_measurement_reflns_used    2756
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.0
_cell_measurement_theta_min      2.3
_cell_volume                     3348.3(16)
_computing_cell_refinement       'SAINTPlus (Bruker, 1998a)'
_computing_data_collection       'SMART (Bruker, 1998b)'
_computing_data_reduction        'SAINTPlus (Bruker, 1998a)'
_computing_molecular_graphics    'SHELXTL ver. 5.1 (Sheldrick, 1998a)'
_computing_publication_material  'SHELXTL ver. 5.1 (Sheldrick, 1998a)'
_computing_structure_refinement  'SHELXTL ver. 5.1 (Sheldrick, 1998a)'
_computing_structure_solution    'SHELXTL ver. 5.1 (Sheldrick, 1998a)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0681
_diffrn_reflns_av_sigmaI/netI    0.1056
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            16054
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    0.180
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.421
_refine_diff_density_min         -0.362
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.868
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         6459
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.868
_refine_ls_R_factor_all          0.1087
_refine_ls_R_factor_gt           0.0514
_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^)+(0.0456P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1013
_refine_ls_wR_factor_ref         0.1191
_reflns_number_gt                3369
_reflns_number_total             6459
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            so5046.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1698 2011-06-07 10:41:20Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2104967
_cod_database_fobs_code          2104967