A novel potentiometric self-plasticizing polypyrrole sensor based on a bidentate bis-NHC ligand for determination of Hg(ii) cation
Said, Nur Rahimah; Rezayi, Majid; Narimani, Leila; Abdul Manan, Ninie Suhana; Alias, Yatimah; RSC Adv. 5 (2015) 76263–; doi:10.1039/C5RA10950G

data_7222103
_publ_section_title
;
 A novel potentiometric self-plasticizing polypyrrole sensor based on a
 bidentate bis-NHC ligand for determination of Hg(ii) cation
;
_journal_issue                   93
_journal_name_full               'RSC Adv.'
_journal_page_first              76263
_journal_paper_doi               10.1039/C5RA10950G
_journal_volume                  5
_journal_year                    2015
_chemical_formula_moiety         '2(Br), C39 H39 N5 O2 S'
_chemical_formula_sum            'C39 H39 Br2 N5 O2 S'
_chemical_formula_weight         801.63
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_block_doi                 10.5517/cc148zhw
_audit_creation_date             2015-08-17
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-08-19 deposited with the CCDC.
2015-08-24 downloaded from the CCDC.
;
_cell_angle_alpha                108.720(5)
_cell_angle_beta                 100.073(5)
_cell_angle_gamma                108.177(5)
_cell_formula_units_Z            4
_cell_length_a                   14.7495(9)
_cell_length_b                   15.5216(8)
_cell_length_c                   19.1751(10)
_cell_measurement_reflns_used    5272
_cell_measurement_temperature    100.2(8)
_cell_measurement_theta_max      25.8680
_cell_measurement_theta_min      3.1620
_cell_volume                     3761.1(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100.2(8)
_diffrn_detector_area_resol_mean 10.4041
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega    9.00   63.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       13.8089   37.0000 -150.0000 54

  2 omega   35.00   95.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       13.8089 -178.0000  -30.0000 60

  3 omega  -42.00   37.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       13.8089  -57.0000    0.0000 79

  4 omega  -11.00   75.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       13.8089   37.0000  150.0000 86

  5 omega   21.00   74.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       13.8089   37.0000    0.0000 53

  6 omega  -15.00   18.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.9651  -99.0000 -180.0000 33

  7 omega  -35.00   11.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.9651  -57.0000 -120.0000 46

  8 omega  -19.00    6.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.9651  -37.0000  -90.0000 25
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0141420000
_diffrn_orient_matrix_UB_12      -0.0213426000
_diffrn_orient_matrix_UB_13      -0.0409767000
_diffrn_orient_matrix_UB_21      -0.0501864000
_diffrn_orient_matrix_UB_22      -0.0061235000
_diffrn_orient_matrix_UB_23      -0.0018239000
_diffrn_orient_matrix_UB_31      0.0103554000
_diffrn_orient_matrix_UB_32      0.0475896000
_diffrn_orient_matrix_UB_33      -0.0004417000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0849
_diffrn_reflns_av_unetI/netI     0.1749
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            44481
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.500
_diffrn_reflns_theta_min         2.929
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.251
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36482
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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    1.416
_exptl_crystal_description       block
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.217
_refine_diff_density_min         -2.811
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     849
_refine_ls_number_reflns         15582
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.1610
_refine_ls_R_factor_gt           0.0977
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1699P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2737
_refine_ls_wR_factor_ref         0.3140
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8447
_reflns_number_total             15582
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra10950g1.cif
_cod_data_source_block           exp_5465
_cod_depositor_comments
;
2017-03-01
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '4(Br), 2(C39 H39 N5 O2 S)'
_cod_original_formula_sum        'C78 H78 Br4 N10 O4 S2'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     1603.26
_cod_database_code               7222103
_chemical_oxdiff_formula         'C H N O S Br'
_shelx_estimated_absorpt_t_max   0.763
_shelx_estimated_absorpt_t_min   0.674
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.50
_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. Uiso/Uaniso restraints and constraints
Uanis(C14) = Uanis(N1) = Uanis(C7) = Uanis(C55) = Uanis(C33) = Uanis(C42) =
Uanis(C43)
3.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C16(H16A,H16B), C57(H57A,H57B), C7(H7A,H7B), C56(H56A,H56B),
 C46(H46A,H46B), C54(H54A,H54B), C17(H17A,H17B), C65(H65A,H65B), C55(H55A,H55B),
  C18(H18A,H18B), C26(H26A,H26B)
3.b Aromatic/amide H refined with riding coordinates:
 C31(H31), C69(H69), C30(H30), C45(H45), C21(H21), C5(H5), C4(H4), C2(H2),
 C70(H70), C37(H37), C20(H20), C10(H10), C42(H42), C3(H3), C61(H61), C51(H51),
 C71(H71), C68(H68), C76(H76), C9(H9), C67(H67), C6(H6), C77(H77), C43(H43),
 C22(H22), C44(H44), C48(H48), C38(H38), C23(H23), C29(H29), C60(H60), C50(H50),
  C11(H11), C14(H14), C41(H41), C35(H35), C34(H34), C12(H12), C59(H59),
 C74(H74), C53(H53), C25(H25), C62(H62), C49(H49), C73(H73), C64(H64), C32(H32),
  C28(H28)
3.c Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C78(H78A,H78B,H78C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'