Synthesis and characterization of poly(tetraphenylimidazole)s and their application in the detection of fluoride ions
Aradhyula, Basava Punna Rao; Ranga Naidu Chinta, Ramu V.; Dhanunjayarao, Kunchala; Venkatasubbaiah, Krishnan; RSC Advances 10 (2020) 13149–13154; doi:10.1039/D0RA01559H

data_7240241
_publ_section_title
;
 Synthesis and characterization of poly(tetraphenylimidazole)s and their
 application in the detection of fluoride ions
;
_journal_issue                   22
_journal_name_full               'RSC Advances'
_journal_page_first              13149
_journal_page_last               13154
_journal_paper_doi               10.1039/D0RA01559H
_journal_volume                  10
_journal_year                    2020
_chemical_formula_moiety         'C51 H44 N2 O Si'
_chemical_formula_sum            'C51 H44 N2 O Si'
_chemical_formula_weight         728.97
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2019-09-23
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2017.01.05 svn.r3372 for Rigaku Oxford Diffraction, GUI svn.r5289)
;
_audit_update_record
;
2020-01-07 deposited with the CCDC.	2020-03-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.6548(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.7258(2)
_cell_length_b                   17.0253(2)
_cell_length_c                   17.5571(3)
_cell_measurement_reflns_used    15476
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      77.0140
_cell_measurement_theta_min      2.6000
_cell_volume                     4238.48(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_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            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.984
_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   -108.00 -35.00   0.50    0.86    --  -38.50 -27.00  98.00  146
  2  \w    -42.00  31.00   0.50    0.86    --  -38.50  27.00 -99.00  146
  3  \w     51.00 119.00   0.50    0.86    --   49.31  27.00 -99.00  136
  4  \w     11.00  37.00   0.50    0.86    --   49.31 -27.00  98.00   52
  5  \w    115.00 173.00   0.50    3.53    --  106.38  27.00 -99.00  116
  6  \w     38.00 110.00   0.50    3.53    --  106.38 -27.00  98.00  144
  7  \w    -42.00  -1.00   0.50    0.86    --  -38.50  57.00  30.00   82
  8  \w    -31.00  23.00   0.50    0.86    --  -38.50  37.00 -60.00  108
  9  \w     62.00  88.00   0.50    0.86    --   49.31-125.00 -60.00   52
 10  \w     45.00  92.00   0.50    3.53    --  106.38 -45.00 -60.00   94
 11  \w     80.00 107.00   0.50    3.53    --  106.38 -94.00-120.00   54
 12  \w     43.00 111.00   0.50    3.53    --  106.38 -45.00-180.00  136
 13  \w     40.00  66.00   0.50    3.53    --  106.38 -94.00-120.00   52
 14  \w     44.00  70.00   0.50    3.53    --  106.38 -15.00-120.00   52
 15  \w     53.00 109.00   0.50    3.53    --  106.38 -94.00 -60.00  112
 16  \w     50.00 109.00   0.50    3.53    --  106.38 -94.00-180.00  118
 17  \w     99.00 149.00   0.50    3.53    --  106.38  15.00 -30.00  100
 18  \w     84.00 118.00   0.50    3.53    --  106.38 -61.00-120.00   68
 19  \w    136.00 168.00   0.50    3.53    --  106.38  45.00-150.00   64
 20  \w    108.00 143.00   0.50    3.53    --  106.38  45.00 -30.00   70
 21  \w     48.00  75.00   0.50    3.53    --  106.38 -61.00-120.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0483840000
_diffrn_orient_matrix_UB_12      -0.0313760000
_diffrn_orient_matrix_UB_13      -0.0614630000
_diffrn_orient_matrix_UB_21      0.0957086000
_diffrn_orient_matrix_UB_22      0.0004144000
_diffrn_orient_matrix_UB_23      0.0631977000
_diffrn_orient_matrix_UB_31      -0.0173511000
_diffrn_orient_matrix_UB_32      -0.0848814000
_diffrn_orient_matrix_UB_33      0.0230918000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_av_unetI/netI     0.0275
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25771
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.492
_diffrn_reflns_theta_min         3.117
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.777
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56242
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.142
_exptl_crystal_description       block
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.287
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     507
_refine_ls_number_reflns         8533
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0535
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0866P)^2^+0.6472P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1564
_refine_ls_wR_factor_ref         0.1627
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7192
_reflns_number_total             8533
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ra01559h2.cif
_cod_data_source_block           kv-ab-2
_cod_depositor_comments          'Adding full bibliography for 7240241.cif.'
_cod_original_cell_volume        4238.49(13)
_cod_database_code               7240241
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C51 H44 N2 Si'
_diffrn_oxdiff_ac3_digest_frames
;
01948973022758abd81874566367016bd4000324365
;
_diffrn_oxdiff_ac3_digest_hkl
;
011da3280b748b641578842eeee648e4f6c1e0
;
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C23(H23), C24(H24), C20(H20), C27(H27), C29(H29), C26(H26), C30(H30),
 C51(H51), C6(H6), C10(H10), C17(H17), C14(H14), C19(H19), C34(H34), C47(H47),
 C49(H49), C2(H2), C5(H5), C48(H48), C32(H32), C33(H33), C50(H50), C18(H18),
 C4(H4), C45(H45), C11(H11), C12(H12), C43(H43), C13(H13), C41(H41), C3(H3),
 C44(H44), C42(H42)
2.b Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C39(H39A,H39B,H39C), C38(H38A,H38B,H38C)
;
_shelx_res_checksum              97762
_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 2.834
_oxdiff_exptl_absorpt_empirical_full_min 0.596