Synthesis, crystal structure and Hirshfeld surface analysis of Fmoc-β-amino butyric acid and Fmoc carbamate
Abubakar Magaji, Mubarak; Chen, Beining; Robertson, Craig Collumbine; Acta Crystallographica Section E Crystallographic Communications 81 (2025) –; doi:10.1107/S2056989025003810

data_2023504
_publ_section_title
;
 Synthesis, crystal structure and Hirshfeld surface analysis of
 Fmoc-\b-amino butyric acid and Fmoc carbamate
;
_journal_coeditor_code           VU2009
_journal_issue                   6
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi               10.1107/S2056989025003810
_journal_volume                  81
_journal_year                    2025
_chemical_absolute_configuration ad
_chemical_formula_iupac          'C19 H19 N O4'
_chemical_formula_moiety         'C19 H19 N O4'
_chemical_formula_sum            'C19 H19 N O4'
_chemical_formula_weight         325.35
_chemical_name_systematic
;
3-{[(9<i>H</i>-Fluoren-9-ylmethoxy)carbonyl]amino}butanoic acid
;
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   4.8393(2)
_cell_length_b                   12.4928(4)
_cell_length_c                   27.3101(9)
_cell_measurement_reflns_used    3582
_cell_measurement_temperature    100.0(10)
_cell_measurement_theta_max      66.641
_cell_measurement_theta_min      3.236
_cell_volume                     1651.07(10)
_computing_cell_refinement
;
SAINT V8.40B (Bruker, 2023)
;
_computing_data_collection
;
APEX5 (Bruker, 2023)
;
_computing_data_reduction
;
SAINT V8.40B (Bruker, 2023)
;
_computing_molecular_graphics
;
Olex2 1.5 (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
Olex2 1.5 (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL  (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2018/2</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100.0(10)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Venture Photon III'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0806
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            25780
_diffrn_reflns_theta_full        66.838
_diffrn_reflns_theta_max         66.838
_diffrn_reflns_theta_min         3.236
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.753
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6641
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_description       needle
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.026
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.117
_refine_diff_density_min         -0.171
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 992 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   -0.05(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         2922
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0324
_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^)+(0.0304P)^2^+0.2044P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0693
_refine_ls_wR_factor_ref         0.0731
_reflns_number_gt                2590
_reflns_number_total             2922
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            vu2009.cif
_cod_data_source_block           1
_cod_database_code               2023504
_shelx_estimated_absorpt_t_min   0.806
_shelx_estimated_absorpt_t_max   0.993
_shelx_hkl_checksum              47522
_shelx_res_checksum              46904