Quantitative Raman microscopy to describe structural organisation in hollow microcrystals built from silicon catecholate and amines
Volkov, Victor V.; Blundell, Toby J.; Argent, Stephen; Perry, Carole Celia; Dalton Transactions  (2023) –; doi:10.1039/D3DT00856H

data_7712944
_publ_section_title
;
 Quantitative Raman microscopy to describe structural organisation in
 hollow microcrystals built from silicon catecholate and amines
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00856H
_journal_year                    2023
_chemical_formula_moiety         'C18 H12 O6 Si, C6 H18 N2'
_chemical_formula_sum            'C24 H30 N2 O6 Si'
_chemical_formula_weight         470.59
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-02
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2023.02.24 svn.rf166f9f3 for OlexSys, GUI svn.r6725)
;
_audit_update_record
;
2023-03-02 deposited with the CCDC.	2023-05-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.4420(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3695(2)
_cell_length_b                   21.4394(3)
_cell_length_c                   8.54050(10)
_cell_measurement_reflns_used    8899
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      35.5036699554
_cell_measurement_theta_min      2.77042211846
_cell_volume                     2234.21(5)
_computing_cell_refinement
'DIALS 2theta refinement, DIALS 2.1.1-gcdd629a7b-release'
_computing_data_collection       'GDA 8.44; generic data acquisition software'
_computing_data_reduction
;
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
DIALS 2.1.1-gcdd629a7b-release (Winter, G. et al., 2018)
pointless (Evans, P., 2006)
XIA2 0.6.366-ga657f9d9-dials-2.1 (Winter, G., 2010)
;
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_detector                 'Photon counting pixel array'
_diffrn_detector_area_resol_mean 0.0350
_diffrn_detector_type            'Dectris Pilatus 2M'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'Fixed \c 3-circle diffractometer'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       '\f and \w rotation with 0.1 degree frames'
_diffrn_measurement_specimen_support 'MiTeGen MicroMount'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_unetI/netI     0.0605
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2782
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         27.336
_diffrn_reflns_theta_min         2.981
_diffrn_source                   Synchrotron
_diffrn_source_type              'Undulator, I19, DLS, RAL'
_exptl_absorpt_coefficient_mu    0.140
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.9965277769058909
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
CCP4 7.0.078: AIMLESS, version 0.7.4 : 13/12/18
Scaling & analysis of unmerged intensities, absorption correction using spherical harmonics
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_description       needle
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.652
_refine_diff_density_min         -0.614
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         2782
_refine_ls_number_restraints     326
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0834
_refine_ls_R_factor_gt           0.0792
_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^)+(0.0894P)^2^+13.8866P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2435
_refine_ls_wR_factor_ref         0.2467
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2532
_reflns_number_total             2782
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00856h2.cif
_cod_data_source_block           shelxt_a
_cod_database_code               7712944
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.999
_shelx_estimated_absorpt_t_min   0.979
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.712(5)
 0.288(5)
2. 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
3. Uiso/Uaniso restraints and constraints
N2 \\sim N1 \\sim H1 \\sim C10 \\sim C11 \\sim C12 \\sim H10A \\sim H10B \\sim
C13 \\sim H11A \\sim H11B \\sim H11C \\sim H12A \\sim H12B \\sim H12C \\sim
H13A \\sim H13B \\sim H2 \\sim C14 \\sim C15 \\sim H14A \\sim H14B \\sim H14C
\\sim H15A \\sim H15B \\sim H15C: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: N1(0.5) H1(0.5) N2(0.5) H2(0.5) C10(0.5) H10A(0.5) H10B(0.5)
 C11(0.5) H11A(0.5) H11B(0.5) H11C(0.5) C12(0.5) H12A(0.5) H12B(0.5) H12C(0.5)
 C13(0.5) H13A(0.5) H13B(0.5) C14(0.5) H14A(0.5) H14B(0.5) H14C(0.5) C15(0.5)
 H15A(0.5) H15B(0.5) H15C(0.5)
6.a Ternary CH refined with riding coordinates:
 N1(H1), N2(H2)
6.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C13(H13A,H13B)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9)
6.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C)
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in perfluoroether oil'
_olex2_submission_special_instructions 'No special instructions were received'