Investigation of crystal structures, energetics and isostructurality in halogen-substituted phosphoramidates
Hasija, Avantika; Som, Shubham; Chopra, Deepak; Acta Crystallographica Section B 78 (2022) –; doi:10.1107/S2052520622000889

data_2108940
_publ_section_title
;
 Investigation of crystal structures, energetics and isostructurality in
 halogen-substituted phosphoramidates
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052520622000889
_journal_volume                  78
_journal_year                    2022
_chemical_formula_moiety         'C18 H15 F N O3 P'
_chemical_formula_sum            'C18 H15 F N O3 P'
_chemical_formula_weight         343.28
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-01-21
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_cell_angle_alpha                86.225(3)
_cell_angle_beta                 90.171(3)
_cell_angle_gamma                91.354(3)
_cell_formula_units_Z            4
_cell_length_a                   10.1285(7)
_cell_length_b                   9.1480(7)
_cell_length_c                   17.8798(14)
_cell_measurement_reflns_used    9947
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.06
_cell_measurement_theta_min      2.44
_cell_volume                     1652.6(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0839
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9620
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.186
_diffrn_reflns_theta_min         2.232
_exptl_absorpt_coefficient_mu    0.192
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.5969
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2014/2
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_description       block
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.316
_exptl_crystal_size_mid          0.254
_exptl_crystal_size_min          0.068
_refine_diff_density_max         0.776
_refine_diff_density_min         -0.686
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         9620
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1305
_refine_ls_R_factor_gt           0.0761
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1157P)^2^+1.3293P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1902
_refine_ls_wR_factor_ref         0.2262
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6078
_reflns_number_total             9620
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            aw5064sup1.cif
_cod_data_source_block           4F
_cod_database_code               2108940
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.987
_shelx_estimated_absorpt_t_min   0.942
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.862(3)
 0.138(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C18(H18), C24(H24), C32(H32), C2(H2A), C17(H17), C36(H36), C23(H23), C33(H33),
  C14(H14), C6(H6), C35(H35), C26(H26), C15(H15), C8(H8), C20(H20), C30(H30),
 C29(H29), C3(H3), C12(H12), C5(H5), C9(H9), C28(H28), C27(H27), C22(H22),
 C4(H4), C10(H10), C11(H11), C21(H21)
;
_shelx_res_checksum              4865
_shelx_hkl_checksum              24539
_olex2_submission_special_instructions 'No special instructions were received'
_cod_database_fobs_code 2108940