Highly selective metallogel from 4-biphenylcarboxy capped diphenylalanine and FeCl3
Sasmal, Supriya; Maji, Krishnendu; Díaz Díaz, David; Haldar, Debasish; CrystEngComm 21 (2019) 4289–; doi:10.1039/C9CE00695H

data_7232895
_publ_section_title
;
 Highly selective metallogel from 4-biphenylcarboxy capped diphenylalanine
 and FeCl3
;
_journal_issue                   29
_journal_name_full               CrystEngComm
_journal_page_first              4289
_journal_paper_doi               10.1039/C9CE00695H
_journal_volume                  21
_journal_year                    2019
_chemical_absolute_configuration s
_chemical_formula_moiety         'C23 H21 N O4'
_chemical_formula_sum            'C23 H21 N O4'
_chemical_formula_weight         375.41
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-05-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.18 svn.r3508 for OlexSys, GUI svn.r5497)
;
_audit_update_record
;
2018-10-15 deposited with the CCDC.    2019-05-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.0318(3)
_cell_length_b                   8.6573(5)
_cell_length_c                   43.325(2)
_cell_measurement_reflns_used    4305
_cell_measurement_temperature    123(30)
_cell_measurement_theta_max      65.7720
_cell_measurement_theta_min      4.0770
_cell_volume                     1887.32(18)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123(30)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9580
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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    -13.00 102.00   1.00    2.50    --   25.65  57.00 -60.00  115
  2  \w     57.00 123.00   1.00    2.50    --   25.65 178.00   0.00   66
  3  \w    -13.00 102.00   1.00    2.50    --   25.65  57.00-180.00  115
  4  \w    100.00 153.00   1.00   10.00    --   66.82 111.00-180.00   53
  5  \w    101.00 153.00   1.00   10.00    --   66.82 108.00 -13.00   52
  6  \w     57.00 150.00   1.00   10.00    --   66.82 178.00-180.00   93
  7  \w    102.00 155.00   1.00   10.00    --   66.82  99.00  86.00   53
  8  \w    -14.00 116.00   1.00   10.00    --   66.82 -45.00  90.00  130
  9  \w     70.00 178.00   1.00   15.00    --  108.00  65.00 -30.00  108
 10  \w     20.00 113.00   1.00   15.00    --  108.00-104.00  30.00   93
 11  \w    101.00 178.00   1.00   15.00    --  108.00 104.00 -30.00   77
 12  \w     86.00 178.00   1.00   15.00    --  108.00 138.00-120.00   92
 13  \w     70.00 178.00   1.00   15.00    --  108.00  65.00 120.00  108
 14  \w     30.00 148.00   1.00   15.00    --  108.00 -54.00 -90.00  118
 15  \w     64.00 178.00   1.00   15.00    --  108.00  77.00 -60.00  114
 16  \w     64.00 178.00   1.00   15.00    --  108.00  77.00-120.00  114
 17  \w    -13.00 102.00   1.00    2.50    --   25.65  57.00  60.00  115
 18  \w    -51.00  64.00   1.00    2.50    --   25.65 -57.00 -60.00  115
 19  \w    -51.00  64.00   1.00    2.50    --   25.65 -57.00  60.00  115
 20  \w     17.00 148.00   1.00   10.00    --   66.82  45.00  60.00  131
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.2415097000
_diffrn_orient_matrix_UB_12      -0.0690966000
_diffrn_orient_matrix_UB_13      -0.0169510000
_diffrn_orient_matrix_UB_21      0.1621229000
_diffrn_orient_matrix_UB_22      0.0059598000
_diffrn_orient_matrix_UB_23      0.0301448000
_diffrn_orient_matrix_UB_31      -0.0956883000
_diffrn_orient_matrix_UB_32      -0.1638574000
_diffrn_orient_matrix_UB_33      0.0082946000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            8645
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        65.762
_diffrn_reflns_theta_max         65.762
_diffrn_reflns_theta_min         4.082
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.736
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73969
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_description       irregular
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.3258
_exptl_crystal_size_mid          0.2187
_exptl_crystal_size_min          0.1111
_refine_diff_density_max         0.273
_refine_diff_density_min         -0.573
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
;
 Flack x determined using 1027 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.0(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         3140
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0732
_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^)+(0.0635P)^2^+6.2594P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1790
_refine_ls_wR_factor_ref         0.1869
_reflns_Friedel_coverage         0.612
_reflns_Friedel_fraction_full    0.920
_reflns_Friedel_fraction_max     0.920
_reflns_number_gt                2962
_reflns_number_total             3140
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce00695h2.cif
_cod_data_source_block           biptyrome
_cod_depositor_comments
'Adding full bibliography for 7232894--7232895.cif.'
_cod_original_cell_volume        1887.29(18)
_cod_database_code               7232895
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H N O'
_shelx_estimated_absorpt_t_max   0.923
_shelx_estimated_absorpt_t_min   0.796
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C12) = Uanis(C7) = Uanis(C8) = Uanis(C9) = Uanis(C10) = Uanis(C11)
3.a Ternary CH refined with riding coordinates:
 C14(H14)
3.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B)
3.c Aromatic/amide H refined with riding coordinates:
 N1(H1), C17(H17), C18(H18), C21(H21), C20(H20), C5(H5), C3(H3), C1(H1A),
 C4(H4A), C2(H2), C9(H9), C11(H11), C12(H12), C8(H8)
3.d Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C)
3.e Idealised tetrahedral OH refined as rotating group:
 O4(H4)
;
_olex2_date_sample_data_collection 2018-05-28
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.725
_oxdiff_exptl_absorpt_empirical_full_min 0.754