Synthesis and X-ray characterization of antipyrine-tethered organosilanes and their magnetic nanoparticles: potent anti-oxidants and receptors for Sn(ii) ions
Singh, Gurjaspreet; Suman,; Satija, Pinky; Singh, Akshpreet; Shilpy,; González-Silvera, D.; Espinosa Ruiz, Cristobal; Esteban, M. Angeles; Sahoo, Subash Chandra; New Journal of Chemistry 44 (2020) 15157–15168; doi:10.1039/D0NJ03300F

data_7059870
_publ_section_title
;
 Synthesis and X-ray characterization of antipyrine-tethered organosilanes
 and their magnetic nanoparticles: potent anti-oxidants and receptors for
 Sn(ii) ions
;
_journal_issue                   35
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              15157
_journal_page_last               15168
_journal_paper_doi               10.1039/D0NJ03300F
_journal_volume                  44
_journal_year                    2020
_chemical_compound_source        synthesized
_chemical_formula_moiety         'C34 H39 N6 O5 Si'
_chemical_formula_sum            'C34 H39 N6 O5 Si'
_chemical_formula_weight         639.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-02-18
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2017.02.24 svn.r3390 for Rigaku Oxford Diffraction, GUI svn.r5318)
;
_audit_update_record
;
2020-02-18 deposited with the CCDC.	2020-07-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 118.622(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.3291(12)
_cell_length_b                   12.5871(5)
_cell_length_c                   18.0230(13)
_cell_measurement_reflns_used    7747
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.3960
_cell_measurement_theta_min      3.4140
_cell_volume                     3450.8(5)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (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 0.964
_diffrn_measured_fraction_theta_max 0.841
_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    -30.00  54.00   0.50   30.00    --   -9.79  66.00  24.00  168
  2  \w    -47.00  12.00   0.50   30.00    --   -9.79 107.00 108.00  118
  3  \w      5.00  54.00   0.50   30.00    --   -9.79  58.00-125.00   98
  4  \w    -51.00 -25.00   0.50   30.00    --   -9.79 125.00  30.00   52
  5  \w    -73.00 -19.00   0.50   30.00    --   -9.79 -57.00  60.00  108
  6  \w      0.00  54.00   0.50   30.00    --   -9.79  38.00 -30.00  108
  7  \w     27.00  57.00   0.50   30.00    --   10.07-125.00   0.00   60
;
_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      0.0069323000
_diffrn_orient_matrix_UB_12      -0.0375269000
_diffrn_orient_matrix_UB_13      -0.0255716000
_diffrn_orient_matrix_UB_21      0.0458312000
_diffrn_orient_matrix_UB_22      0.0102010000
_diffrn_orient_matrix_UB_23      0.0225458000
_diffrn_orient_matrix_UB_31      0.0050685000
_diffrn_orient_matrix_UB_32      -0.0407845000
_diffrn_orient_matrix_UB_33      0.0291538000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_unetI/netI     0.0603
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.841
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22492
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.841
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.034
_diffrn_reflns_theta_min         3.129
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.117
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47296
_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            yellow
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_description       neddle
_exptl_crystal_F_000             1356
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.387
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     430
_refine_ls_number_reflns         6567
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1505
_refine_ls_R_factor_gt           0.0679
_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^)+(0.1167P)^2^+0.2000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1908
_refine_ls_wR_factor_ref         0.2364
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3009
_reflns_number_total             6567
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj03300f2.cif
_cod_data_source_block           3e
_cod_depositor_comments          'Adding full bibliography for 7059870.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7059870
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O Si'
_diffrn_oxdiff_ac3_digest_frames
;
014c9e79db3a92d2e83b2943bfb27b945f007122609
;
_diffrn_oxdiff_ac3_digest_hkl
;
01bbd483f34346722d5228ebee00434ef7bed4
;
_reflns_odcompleteness_completeness 89.51
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 C5, C6B, C6B
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 C5, C6A, C6A
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
3. Others
 Fixed Sof: H5A(0.5) H5B(0.5) C6B(0.5) H6BA(0.5) H6BB(0.5) H6BC(0.5) C6A(0.5)
 H6AA(0.5) H6AB(0.5) H6AC(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C9(H9A,H9B), C8(H8A,H8B), C7(H7A,H7B), C5(H5A,H5B)
4.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C23(H23), C14(H14), C20(H20), C15(H15), C34(H34), C19(H19),
 C17(H17), C30(H30), C18(H18), C32(H32), C31(H31), C33(H33), C1(H1), C3(H3)
4.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C4(H4A,H4B,H4C), C2(H2A,H2B,H2C),
 C6B(H6BA,H6BB,H6BC), C6A(H6AA,H6AB,H6AC)
;
_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 1.901
_oxdiff_exptl_absorpt_empirical_full_min 0.477