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_7232894
_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         'C17 H17 N O4'
_chemical_formula_sum            'C17 H17 N O4'
_chemical_formula_weight         299.31
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2018-05-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 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                 94.508(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.6594(5)
_cell_length_b                   7.2685(7)
_cell_length_c                   17.267(2)
_cell_measurement_reflns_used    1083
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.3530
_cell_measurement_theta_min      3.0130
_cell_volume                     708.09(12)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9580
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -11.00  104.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -       27.3242   57.0000   60.0000 115

  2 omega  -32.00  110.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -       27.3242   38.0000 -150.0000 142

  3 omega   35.00  121.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -       27.3242  178.0000   60.0000 86

  4 omega  -49.00  -27.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -       27.3242  -57.0000   90.0000 22
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0405682000
_diffrn_orient_matrix_UB_12      -0.0730782000
_diffrn_orient_matrix_UB_13      0.0227248000
_diffrn_orient_matrix_UB_21      -0.1182253000
_diffrn_orient_matrix_UB_22      0.0312463000
_diffrn_orient_matrix_UB_23      -0.0075788000
_diffrn_orient_matrix_UB_31      -0.0130393000
_diffrn_orient_matrix_UB_32      -0.0565216000
_diffrn_orient_matrix_UB_33      -0.0335815000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0642
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            3178
_diffrn_reflns_point_group_measured_fraction_full 0.876
_diffrn_reflns_point_group_measured_fraction_max 0.876
_diffrn_reflns_theta_full        24.707
_diffrn_reflns_theta_max         24.707
_diffrn_reflns_theta_min         2.366
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.100
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53096
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_description       plate
_exptl_crystal_F_000             316
_exptl_crystal_size_max          0.2589
_exptl_crystal_size_mid          0.1589
_exptl_crystal_size_min          0.1111
_refine_diff_density_max         0.246
_refine_diff_density_min         -0.262
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details
;
 Flack x determined using 557 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.002(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         2117
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0518
_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^)+(0.0494P)^2^+0.1275P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1148
_refine_ls_wR_factor_ref         0.1213
_reflns_Friedel_coverage         0.612
_reflns_Friedel_fraction_full    0.729
_reflns_Friedel_fraction_max     0.729
_reflns_number_gt                1843
_reflns_number_total             2117
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce00695h2.cif
_cod_data_source_block           bi-ph-ser-ome
_cod_depositor_comments
'Adding full bibliography for 7232894--7232895.cif.'
_cod_original_cell_volume        708.09(13)
_cod_database_code               7232894
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H N O'
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.974
_reflns_odcompleteness_completeness 99.59
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.63
_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.a Ternary CH refined with riding coordinates:
 C14(H14)
2.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B)
2.c Aromatic/amide H refined with riding coordinates:
 N1(H1), C1(H1A), C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C11(H11),
 C12(H12)
2.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C)
2.e Idealised tetrahedral OH refined as rotating group:
 O4(H4)
;
_olex2_date_sample_data_collection 2018-04-07
_olex2_submission_special_instructions 'No special instructions were received'