Crystal structure of 2-(3-(2-(4-phenylpiperazin-1-yl)ethyl)benzyl)isoindoline-1,3-dione, C27H27N3O2
Feng, Aiqing; Lv, Bin; Zeitschrift für Kristallographie - New Crystal Structures 235 (2019) 49–51; doi:10.1515/ncrs-2019-0463

data_8105012
_publ_section_title
;
 Crystal structure of
 2-(3-(2-(4-phenylpiperazin-1-yl)ethyl)benzyl)isoindoline-1,3-dione,
 C27H27N3O2
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              49
_journal_page_last               51
_journal_paper_doi               10.1515/ncrs-2019-0463
_journal_volume                  235
_journal_year                    2019
_chemical_formula_moiety         'C27 H27 N3 O2'
_chemical_formula_sum            'C27 H27 N3 O2'
_chemical_formula_weight         425.53
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_atom_sites_solution_primary     dual
_cell_angle_alpha                75.708(5)
_cell_angle_beta                 87.142(5)
_cell_angle_gamma                74.935(6)
_cell_formula_units_Z            2
_cell_length_a                   6.9263(4)
_cell_length_b                   10.0832(7)
_cell_length_c                   17.3531(10)
_cell_measurement_reflns_used    2853
_cell_measurement_temperature    289.36(10)
_cell_measurement_theta_max      26.0210
_cell_measurement_theta_min      3.7550
_cell_volume                     1133.92(13)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      289.36(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.9917
_diffrn_measured_fraction_theta_max 0.9917
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -39.00  55.00   1.00    4.17    --  -12.53  77.00  30.00   94
  2  \w     51.00  77.00   1.00    4.17    --   13.55  77.00 -30.00   26
  3  \w     35.00  78.00   1.00    4.17    --   13.55  77.00-180.00   43
  4  \w    -13.00  75.00   1.00    4.17    --   13.55  77.00 -60.00   88
  5  \w    -12.00  57.00   1.00    4.17    --   13.55  77.00 150.00   69
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0376062000
_diffrn_orient_matrix_UB_12      -0.0609165000
_diffrn_orient_matrix_UB_13      0.0069700000
_diffrn_orient_matrix_UB_21      -0.0249131000
_diffrn_orient_matrix_UB_22      0.0063376000
_diffrn_orient_matrix_UB_23      0.0393044000
_diffrn_orient_matrix_UB_31      -0.0959931000
_diffrn_orient_matrix_UB_32      0.0434463000
_diffrn_orient_matrix_UB_33      -0.0136434000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_av_unetI/netI     0.0414
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7776
_diffrn_reflns_theta_full        24.9973
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.30
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.080
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65221
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.2462
_exptl_crystal_description       block
_exptl_crystal_F_000             452.1922
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.2246
_refine_diff_density_min         -0.3563
_refine_diff_density_rms         0.0691
_refine_ls_d_res_high            0.8410
_refine_ls_d_res_low             6.1753
_refine_ls_goodness_of_fit_ref   1.0262
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    47
_refine_ls_number_parameters     289
_refine_ls_number_reflns         3957
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0262
_refine_ls_R_factor_all          0.0800
_refine_ls_R_factor_gt           0.0605
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0742P)^2^+0.3825P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1488
_refine_ls_wR_factor_ref         0.1661
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              8
_reflns_limit_h_min              -8
_reflns_limit_k_max              11
_reflns_limit_k_min              -11
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                2968
_reflns_number_total             3957
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            suppl_ncrs-2019-0463_suppl.cif
_cod_data_source_block           161206zj-50
_cod_database_code               8105012
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.66
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C9(H9a,H9b), C17(H17a,H17b), C16(H16a,H16b), C21(H21a,H21b), C20(H20a,H20b),
 C19(H19a,H19b), C18(H18a,H18b)
2.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C3(H3), C6(H6), C11(H11), C1(H1), C27(H27), C2(H2), C13(H13),
 C12(H12), C26(H26), C25(H25), C23(H23), C24(H24)
;