Single crystal formation in core-shell capsules.
Mettler, Marie; Dewandre, Adrien; Tumanov, Nikolay; Wouters, Johan; Septavaux, Jean; Chemical communications (Cambridge, England)  (2023) –; doi:10.1039/d3cc03727d

data_7132179
_publ_section_title
;
 Single crystal formation in core-shell capsules.
;
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_paper_doi               10.1039/d3cc03727d
_journal_year                    2023
_chemical_formula_moiety         'C2 H5 N O2'
_chemical_formula_sum            'C2 H5 N O2'
_chemical_formula_weight         75.07
_chemical_name_common            'glycine, beta polymorph'
_chemical_name_systematic        'aminoacetic acid, beta polymorph'
_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   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   dual
_audit_creation_date             2023-04-04
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_cell_angle_alpha                90
_cell_angle_beta                 113.232(14)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.0947(6)
_cell_length_b                   6.2681(5)
_cell_length_c                   5.3883(6)
_cell_measurement_reflns_used    950
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      32.1460
_cell_measurement_theta_min      4.1150
_cell_volume                     158.12(3)
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2015/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      295.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1856
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.926
_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     79.00 105.00   1.00   15.00    --   19.23 178.00-150.00   26
  2  \w    -43.00  47.00   1.00   15.00    --  -19.54  38.00-120.00   90
  3  \w    -49.00  33.00   1.00   15.00    --  -19.54  77.00 -30.00   82
  4  \w     10.00  36.00   1.00   15.00    --   19.38  77.00  60.00   26
  5  \w    -58.00 -18.00   1.00   15.00    --  -19.54  19.00  90.00   40
  6  \w    -10.00  49.00   1.00   15.00    --  -19.54  19.00  90.00   59
  7  \w    -77.00   5.00   1.00   15.00    --  -19.54 -57.00 -60.00   82
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0868674000
_diffrn_orient_matrix_UB_12      0.0398862000
_diffrn_orient_matrix_UB_13      0.1296825000
_diffrn_orient_matrix_UB_21      0.0820324000
_diffrn_orient_matrix_UB_22      0.0582135000
_diffrn_orient_matrix_UB_23      -0.0570313000
_diffrn_orient_matrix_UB_31      -0.0931768000
_diffrn_orient_matrix_UB_32      0.0884492000
_diffrn_orient_matrix_UB_33      -0.0210698000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_av_unetI/netI     0.0398
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.926
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            1996
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.895
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.752
_diffrn_reflns_theta_min         4.116
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.140
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.976
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_description       block
_exptl_crystal_F_000             80
_exptl_crystal_preparation
;
crystallized and measured in a plactic sphere
;
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.073
_refine_diff_density_max         0.256
_refine_diff_density_min         -0.244
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     66
_refine_ls_number_reflns         1053
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0443P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0887
_refine_ls_wR_factor_ref         0.0970
_reflns_Friedel_coverage         0.794
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.860
_reflns_number_gt                921
_reflns_number_total             1053
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc03727d2.cif
_cod_data_source_block           nt1021_Glycine_full
_cod_database_code               7132179
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         C2H5NO2
_shelx_estimated_absorpt_t_max   0.990
_shelx_estimated_absorpt_t_min   0.966
_olex2_refinement_description
;
;
_shelx_res_checksum              12755
_shelx_hkl_checksum              90564
_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 1.069
_oxdiff_exptl_absorpt_empirical_full_min 0.914