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_7132177
_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         'Cl Na'
_chemical_formula_sum            'Cl Na'
_chemical_formula_weight         58.44
_chemical_name_common            'rock salt'
_chemical_name_systematic        'sodium chloride'
_space_group_crystal_system      cubic
_space_group_IT_number           225
_space_group_name_Hall           '-F 4 2 3'
_space_group_name_H-M_alt        'F m -3 m'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   dual
_audit_creation_date             2023-04-05
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.6357(3)
_cell_length_b                   5.6357(3)
_cell_length_c                   5.6357(3)
_cell_measurement_reflns_used    206
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      32.2330
_cell_measurement_theta_min      6.2540
_cell_volume                     178.996(17)
_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 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3712
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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     -6.00  38.00   1.00    5.00    --   19.07  77.00-150.00   44
  2  \w    -17.00  35.00   1.00    5.00    --   19.07 -77.00 -30.00   52
  3  \w    -83.00 -20.00   1.00    5.00    --  -19.23 -38.00  60.00   63
;
_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      -0.1023072000
_diffrn_orient_matrix_UB_12      -0.0683046000
_diffrn_orient_matrix_UB_13      -0.0265340000
_diffrn_orient_matrix_UB_21      0.0181122000
_diffrn_orient_matrix_UB_22      0.0204207000
_diffrn_orient_matrix_UB_23      -0.1228213000
_diffrn_orient_matrix_UB_31      0.0709564000
_diffrn_orient_matrix_UB_32      -0.1038025000
_diffrn_orient_matrix_UB_33      -0.0067250000
_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  0.0228
_diffrn_reflns_av_unetI/netI     0.0131
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       3
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -3
_diffrn_reflns_number            212
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.295
_diffrn_reflns_theta_min         6.270
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.774
_exptl_absorpt_correction_T_max  0.904
_exptl_absorpt_correction_T_min  0.833
_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    2.169
_exptl_crystal_description       block
_exptl_crystal_F_000             112
_exptl_crystal_preparation
;
crystallized and measured in a plactic sphere
;
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.059
_refine_diff_density_max         0.107
_refine_diff_density_min         -0.092
_refine_diff_density_rms         0.032
_refine_ls_extinction_coef       0.044(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.246
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     4
_refine_ls_number_reflns         26
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.246
_refine_ls_R_factor_all          0.0102
_refine_ls_R_factor_gt           0.0102
_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^)+0.1711P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0239
_refine_ls_wR_factor_ref         0.0239
_reflns_Friedel_coverage         0.000
_reflns_number_gt                26
_reflns_number_total             26
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc03727d2.cif
_cod_data_source_block           nt1009_NaCl_in_capsule
_cod_original_cell_volume        179.00(3)
_cod_database_code               7132177
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         NaCl
_shelx_estimated_absorpt_t_max   0.903
_shelx_estimated_absorpt_t_min   0.777
_olex2_refinement_description
;
;
_shelx_res_checksum              61053
_shelx_hkl_checksum              57208
_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 1.085
_oxdiff_exptl_absorpt_empirical_full_min 0.912