The first report of X-ray characterized organosilatrane-based receptors for the electrochemical analysis of Al3+ ions
Singh, Gurjaspreet; Sharma, Sanjay; Singh, Akshpreet; Kaur, Ranjeet; Pawan,; Mohit,; Rana, Shweta; Sahoo, Subash Chandra; Kaur, Amarjit; New Journal of Chemistry 45 (2021) 16083–16091; doi:10.1039/D1NJ02893F

data_7060905
_publ_section_title
;
 The first report of X-ray characterized organosilatrane-based receptors
 for the electrochemical analysis of Al3+ ions
;
_journal_issue                   35
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              16083
_journal_page_last               16091
_journal_paper_doi               10.1039/D1NJ02893F
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C30 H32.5 N3 O4 Si'
_chemical_formula_sum            'C30 H32.5 N3 O4 Si'
_chemical_formula_weight         527.18
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-12-03
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2021-02-11 deposited with the CCDC.	2021-07-23 downloaded from the CCDC.
;
_cell_angle_alpha                64.575(6)
_cell_angle_beta                 71.386(5)
_cell_angle_gamma                85.694(5)
_cell_formula_units_Z            2
_cell_length_a                   9.8540(5)
_cell_length_b                   12.4096(9)
_cell_length_c                   13.1516(6)
_cell_measurement_reflns_used    8992
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.5060
_cell_measurement_theta_min      3.3240
_cell_volume                     1372.88(16)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.936
_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     13.00  40.00   0.50   15.00    --   -9.95  69.00 136.00   54
  2  \w    -55.00 -30.00   0.50   15.00    --   -9.95 -69.00   3.00   50
  3  \w      8.00  65.00   0.50   15.00    --   10.22  69.00 136.00  114
  4  \w    -54.00  18.00   0.50   15.00    --   10.22 -69.00   3.00  144
  5  \w    -57.00 -15.00   0.50   15.00    --   -9.95 125.00   0.00   84
  6  \w    -58.00 -33.00   0.50   15.00    --   -9.95 125.00 -90.00   50
  7  \w    -62.00 -36.00   0.50   15.00    --   -9.95 -38.00-150.00   52
  8  \w    -35.00  55.00   0.50   15.00    --   -9.95  77.00 -90.00  180
  9  \w    -57.00  -6.00   0.50   15.00    --   -9.95 125.00-180.00  102
 10  \w    -28.00  -3.00   0.50   15.00    --   -9.95  57.00-180.00   50
 11  \w     23.00  53.00   0.50   15.00    --   -9.95  57.00-180.00   60
 12  \w    -34.00   1.00   0.50   15.00    --   10.22 119.00 137.29   70
 13  \w    -19.00  37.00   0.50   15.00    --   10.22 -99.00-150.00  112
 14  \w     -4.00  41.00   0.50   15.00    --   10.22 -99.00 -30.00   90
 15  \w    -60.00  21.00   0.50   15.00    --   10.22 -19.00  30.00  162
 16  \w    -29.00  -4.00   0.50   15.00    --   10.22 120.00  52.63   50
 17  \w    -37.00  -6.00   0.50   15.00    --   10.22 127.00-155.70   62
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0049603000
_diffrn_orient_matrix_UB_12      -0.0622070000
_diffrn_orient_matrix_UB_13      0.0163341000
_diffrn_orient_matrix_UB_21      -0.0664112000
_diffrn_orient_matrix_UB_22      -0.0119617000
_diffrn_orient_matrix_UB_23      0.0462366000
_diffrn_orient_matrix_UB_31      -0.0369364000
_diffrn_orient_matrix_UB_32      0.0036821000
_diffrn_orient_matrix_UB_33      -0.0395523000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0975
_diffrn_reflns_av_unetI/netI     0.0790
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.936
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19002
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.434
_diffrn_reflns_theta_min         3.240
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.126
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93349
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_description       rod
_exptl_crystal_F_000             559
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.269
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         5863
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.1104
_refine_ls_R_factor_gt           0.0713
_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^)+(0.1193P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1893
_refine_ls_wR_factor_ref         0.2352
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3521
_reflns_number_total             5863
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj02893f3.cif
_cod_data_source_block           gjp-sic
_cod_depositor_comments          'Adding full bibliography for 7060905.cif.'
_cod_original_formula_sum        'C30 H32.50 N3 O4 Si'
_cod_database_code               7060905
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Si C H N O'
_diffrn_oxdiff_ac3_digest_frames
;
01b026395e5ccdd876ea83eef132fb965701486578d
;
_diffrn_oxdiff_ac3_digest_hkl
;
01fab681411278391f62b7b7f4c512fdd404d7
;
_reflns_odcompleteness_completeness 99.75
_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
2. Rigid body (RIGU) restrains
 C2A, C3A, C5A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C2B, C3B, C5B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Fixed Sof: C2A(0.5) H2AA(0.5) H2AB(0.5) C2B(0.5) H2BA(0.5) H2BB(0.5) C3A(0.6)
 H3AA(0.6) H3AB(0.6) C3B(0.4) H3BA(0.4) H3BB(0.4) C5A(0.5) H5AA(0.5) H5AB(0.5)
 C5B(0.5) H5B(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C7(H7A,H7B), C17(H17A,H17B), C4(H4A,H4B), C6(H6A,
 H6B), C1(H1A,H1B), C2A(H2AA,H2AB), C2B(H2BA,H2BB), C3A(H3AA,H3AB), C3B(H3BA,
 H3BB), C5A(H5AA,H5AB)
4.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C16(H16), C13(H13), C12(H12), C15(H15), C28(H28), C22(H22),
 C27(H27), C25(H25), C26(H26), C23(H23), C20(H20), C19(H19), C5B(H5B)
;
_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 1.247
_oxdiff_exptl_absorpt_empirical_full_min 0.726