A new dipeptide as selective gelator of Cu(II), Zn(II), Pb(II)
Kumar, Santosh; Nandi, Sujay; Suman, Saurav; Haldar, Debasish; CrystEngComm  (2020) –; doi:10.1039/D0CE01199A

data_7241416
_publ_section_title
;
 A new dipeptide as selective gelator of Cu(II), Zn(II), Pb(II)
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE01199A
_journal_year                    2020
_chemical_formula_moiety         'C12 H22 N2 O5'
_chemical_formula_sum            'C12 H22 N2 O5'
_chemical_formula_weight         274.32
_chemical_name_common            Boc-Gly-Aib-OMe
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-10-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-10-15 deposited with the CCDC.	2020-10-19 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 100.550(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.6077(4)
_cell_length_b                   5.8948(2)
_cell_length_c                   23.3133(10)
_cell_measurement_reflns_used    2881
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      65.7050
_cell_measurement_theta_min      3.8680
_cell_volume                     1568.25(10)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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_temperature      293.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9580
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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     57.00 123.00   1.00    2.00    --   25.52 178.00 150.00   66
  2  \w    -13.00 102.00   1.00    2.00    --   25.52  57.00   0.00  115
  3  \w    -13.00 102.00   1.00    2.00    --   25.52  57.00  90.00  115
  4  \w    100.00 153.00   1.00    2.00    --   66.76 111.00 -30.00   53
  5  \w    100.00 153.00   1.00    2.00    --   66.76 111.00 150.00   53
  6  \w    100.00 153.00   1.00    2.00    --   66.76 111.00  90.00   53
  7  \w    100.00 153.00   1.00    2.00    --   66.76 111.00  60.00   53
  8  \w    -11.00 106.00   1.00    2.00    --   66.76 -61.00  60.00  117
  9  \w    -22.00 155.00   1.00    2.00    --   66.76 -15.00 -60.00  177
 10  \w     57.00 150.00   1.00    2.00    --   66.76 178.00  60.00   93
 11  \w     70.00 178.00   1.00    4.00    --  108.00  65.00 -90.00  108
 12  \w     86.00 178.00   1.00    4.00    --  108.00 138.00  30.00   92
 13  \w    101.00 178.00   1.00    4.00    --  108.00 104.00 -60.00   77
 14  \w     20.00 113.00   1.00    4.00    --  108.00-104.00 120.00   93
 15  \w     33.00 178.00   1.00    4.00    --  108.00  32.00  30.00  145
 16  \w     30.00 148.00   1.00    4.00    --  108.00 -54.00  30.00  118
 17  \w     20.00 113.00   1.00    4.00    --  108.00-104.00  60.00   93
 18  \w     71.00 113.00   1.00    4.00    --  108.00  76.00   9.82   42
 19  \w    147.00 173.00   1.00    4.00    --  108.00  76.00   9.82   26
 20  \w    121.00 147.00   1.00    4.00    --  108.00 104.00-120.00   26
 21  \w     73.00 144.00   1.00    4.00    --  108.00  65.00 -60.00   71
 22  \w     96.00 132.00   1.00    4.00    --  108.00 138.00-180.00   36
 23  \w    104.00 178.00   1.00    4.00    --  108.00 104.00 -30.00   74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0054565000
_diffrn_orient_matrix_UB_12      0.1058362000
_diffrn_orient_matrix_UB_13      0.0598668000
_diffrn_orient_matrix_UB_21      -0.1313520000
_diffrn_orient_matrix_UB_22      -0.0582716000
_diffrn_orient_matrix_UB_23      -0.0082962000
_diffrn_orient_matrix_UB_31      0.0305993000
_diffrn_orient_matrix_UB_32      -0.2317208000
_diffrn_orient_matrix_UB_33      0.0294587000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            7274
_diffrn_reflns_theta_full        65.90
_diffrn_reflns_theta_max         65.90
_diffrn_reflns_theta_min         3.87
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.755
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_T_min  0.973
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
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    1.162
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.267
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.033
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         2685
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0565P)^2^+0.2467P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1188
_refine_ls_wR_factor_ref         0.1307
_reflns_number_gt                2132
_reflns_number_total             2685
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d0ce01199a2.cif
_cod_data_source_block           uk_1
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7241416
_chemical_oxdiff_formula         'C H N O'
_reflns_odcompleteness_completeness 96.61
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B)
2.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2)
2.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C11(H11A,H11B,H11C), C10(H10A,H10B,H10C), C3(H3A,H3B,
 H3C), C2(H2A,H2B,H2C), C1(H1A,H1B,H1C)
;
_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 1.335
_oxdiff_exptl_absorpt_empirical_full_min 0.457