A second monoclinic polymorph of <i>N</i>-[bis(morpholin-4-yl)phosphinoyl]-4-fluorobenzamide with the <i>P</i>2~1~/<i>n</i> space group
Tarahhomi, Atekeh; Pourayoubi, Mehrdad; Keikha, Mojtaba; Rheingold, Arnold L.; Golen, James A.; Acta Crystallographica Section E 68 (2012) o2444–; doi:10.1107/S1600536812031418

data_2235890
_publ_section_title
;
 A second monoclinic polymorph of
 <i>N</i>-[bis(morpholin-4-yl)phosphinoyl]-4-fluorobenzamide with the
 <i>P</i>2~1~/<i>n</i> space group
;
_journal_coeditor_code           JJ2145
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2444
_journal_paper_doi               10.1107/S1600536812031418
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C15 H21 F N3 O4 P'
_chemical_formula_moiety         'C15 H21 F N3 O4 P'
_chemical_formula_sum            'C15 H21 F N3 O4 P'
_chemical_formula_weight         357.32
_chemical_name_systematic
;
<i>N</i>-[Bis(morpholin-4-yl)phosphinoyl]-4-fluorobenzamide
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.896(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.6093(6)
_cell_length_b                   10.7114(4)
_cell_length_c                   21.0045(9)
_cell_measurement_reflns_used    7455
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.41
_cell_measurement_theta_min      2.34
_cell_volume                     3360.3(2)
_computing_cell_refinement       '<i>SAINT</i> (Bruker, 2005)'
_computing_data_collection       '<i>APEX2</i> (Bruker, 2005)'
_computing_data_reduction        '<i>SAINT</i> (Bruker, 2005)'
_computing_molecular_graphics
'SHELXTL (Sheldrick, 2008) and Mercury (Macrae <i>et al.</i>, 2008)'
_computing_publication_material
'SHELXTL (Sheldrick, 2008) and enCIFer (Allen <i>et al.</i>, 2004)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w 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  0.0371
_diffrn_reflns_av_sigmaI/netI    0.0383
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25230
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.43
_diffrn_reflns_theta_min         1.44
_exptl_absorpt_coefficient_mu    0.199
_exptl_absorpt_correction_T_max  0.9804
_exptl_absorpt_correction_T_min  0.9651
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Sheldrick, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.454
_refine_diff_density_min         -0.730
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         6912
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.0558
_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^)+(0.0816P)^2^+4.9555P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1457
_refine_ls_wR_factor_ref         0.1595
_reflns_number_gt                5355
_reflns_number_total             6912
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jj2145.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2235890
_cod_database_fobs_code          2235890