Stacked Aryl Groups in P-Resolved Cyclic Phosphonamides as a new conformational constrain
Terraneo, Giancarlo; Cardellicchio, Cosimo; Pigliacelli, Claudia; Capozzi, Maria Annunziata M.; CrystEngComm  (2019) –; doi:10.1039/C9CE01382B

data_7234755
_publ_section_title
;
 Stacked Aryl Groups in P-Resolved Cyclic Phosphonamides as a new
 conformational constrain
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C9CE01382B
_journal_year                    2019
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C27 H25 Cl N O3 P'
_chemical_formula_sum            'C27 H25 Cl N O3 P'
_chemical_formula_weight         477.90
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2019-08-26 deposited with the CCDC.    2019-10-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.491(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.8897(3)
_cell_length_b                   14.6971(6)
_cell_length_c                   12.2755(5)
_cell_measurement_reflns_used    4155
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.22
_cell_measurement_theta_min      3.12
_cell_volume                     1208.70(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_unetI/netI     0.0476
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15596
_diffrn_reflns_point_group_measured_fraction_full 0.944
_diffrn_reflns_point_group_measured_fraction_max 0.898
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.014
_diffrn_reflns_theta_min         3.685
_exptl_absorpt_coefficient_mu    0.253
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.6623
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Bruker (2001). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_description       table
_exptl_crystal_F_000             500
_exptl_crystal_size_max          0.440
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.212
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details
;
 Flack x determined using 1895 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         7538
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0642P)^2^+0.0323P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1086
_refine_ls_wR_factor_ref         0.1254
_reflns_Friedel_coverage         0.757
_reflns_Friedel_fraction_full    0.889
_reflns_Friedel_fraction_max     0.801
_reflns_number_gt                5301
_reflns_number_total             7538
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce01382b1.cif
_cod_data_source_block           am20
_cod_original_formula_sum        'C27 H25 Cl N O3 P1'
_cod_database_code               7234755
_shelx_estimated_absorpt_t_min   0.897
_shelx_estimated_absorpt_t_max   0.956
_shelxl_version_number           2013-3
_shelx_res_checksum              50961