Pentapeptide Nanoreactor as a Platform for Halogenations, Diels-Alder Reaction, and Morita-Baylis-Hillman Reaction.
Debnath, Mintu; Sasmal, Supriya; Podder, Debasish; Haldar, Debasish; ACS omega 4 (2019) 13872–13878; doi:10.1021/acsomega.9b01393

data_4516965
_publ_section_title
;
 Pentapeptide Nanoreactor as a Platform for Halogenations, Diels-Alder
 Reaction, and Morita-Baylis-Hillman Reaction.
;
_journal_issue                   9
_journal_name_full               'ACS omega'
_journal_page_first              13872
_journal_page_last               13878
_journal_paper_doi               10.1021/acsomega.9b01393
_journal_volume                  4
_journal_year                    2019
_chemical_absolute_configuration S
_chemical_formula_moiety         '0.04(C46 H55 N5 O8), 0.08(C6 H4 Cl2)'
_chemical_formula_sum            'C58 H68 Cl4 N5 O8'
_chemical_formula_weight         1105.0159
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-03-29
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.394(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.2684(2)
_cell_length_b                   24.0869(6)
_cell_length_c                   11.3063(3)
_cell_measurement_reflns_used    11168
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.0310
_cell_measurement_theta_min      1.9530
_cell_volume                     2796.37(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_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9580
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -16.00  116.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       28.5461   77.0000   60.0000 132

  2 omega  -16.00  116.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       28.5461   77.0000 -120.0000 132

  3 omega  -66.00   50.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1399   57.0000 -180.0000 116

  4 omega -123.00  -55.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1399  178.0000 -180.0000 68

  5 omega  -20.00   14.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1399  -99.0000   90.0000 34

  6 omega  -48.00   67.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       28.5461  -57.0000  -30.0000 115
;
_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      0.0358337000
_diffrn_orient_matrix_UB_12      0.0091369000
_diffrn_orient_matrix_UB_13      0.0501799000
_diffrn_orient_matrix_UB_21      -0.0013261000
_diffrn_orient_matrix_UB_22      -0.0273153000
_diffrn_orient_matrix_UB_23      0.0234290000
_diffrn_orient_matrix_UB_31      0.0590059000
_diffrn_orient_matrix_UB_32      -0.0061532000
_diffrn_orient_matrix_UB_33      -0.0295144000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_unetI/netI     0.0469
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            21179
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         1.691
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.270
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52430
_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_density_diffrn    1.312
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.389
_exptl_crystal_size_mid          0.254
_exptl_crystal_size_min          0.215
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details
;
 Flack x determined using 3890 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.837
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     682
_refine_ls_number_reflns         9716
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.837
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0368
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1072
_refine_ls_wR_factor_ref         0.1132
_reflns_Friedel_coverage         0.919
_reflns_Friedel_fraction_full    0.968
_reflns_Friedel_fraction_max     0.968
_reflns_number_gt                8988
_reflns_number_total             9716
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao9b01393_si_002.cif
_cod_data_source_block           ffaff_dcb
_cod_database_code               4516965
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H N O'
_reflns_odcompleteness_completeness 86.56
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
2.a Ternary CH refined with riding coordinates:
 C28(H28), C15(H15), C37(H37), C6(H6)
2.b Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C7(H7A,H7B), C29(H29A,H29B), C38(H38A,H38B)
2.c Aromatic/amide H refined with riding coordinates:
 N5(H5), N4(H4), N3(H3), N2(H2), N1(H1), C21(H21), C9(H9), C40(H40), C10(H10),
 C35(H35), C18(H18), C20(H20), C19(H19), C42(H42), C12(H12), C41(H41), C32(H32),
  C43(H43), C34(H34), C13(H13), C33(H33), C44(H44), C31(H31), C11(H11),
 C22(H22), C55(H55), C58(H58), C57(H57), C56(H56), C50(H50), C51(H51), C52(H52),
  C49(H49)
2.d Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C1(H1A,H1B,H1C), C25(H25A,H25B,H25C), C3(H3A,H3B,H3C),
 C2(H2A,H2B,H2C), C46(H46A,H46B,H46C)
;
_olex2_date_sample_data_collection 2017-03-28
_olex2_submission_special_instructions 'No special instructions were received'