A Functional Zn(II) Metallacycle Formed from an N-Heterocyclic Carbene Precursor: A Molecular Sensor for Selective Recognition of Fe(3+) and IO4(-) Ions.
Kumar, Girijesh; Guda, Ramu; Husain, Ahmad; Bodapati, Ramakrishna; Das, Samar K.; Inorganic chemistry 56 (2017) 5017–5025; doi:10.1021/acs.inorgchem.7b00098

data_4345679
_publ_section_title
;
 A Functional Zn(II) Metallacycle Formed from an N-Heterocyclic Carbene
 Precursor: A Molecular Sensor for Selective Recognition of Fe(3+) and
 IO4(-) Ions.
;
_journal_issue                   9
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5017
_journal_page_last               5025
_journal_paper_doi               10.1021/acs.inorgchem.7b00098
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         '2(C37 H43 N4), 6(O), 1.33(Br), 0.67(Cl)'
_chemical_formula_sum            'C74 H86 Br1.33 Cl0.68 N8 O6'
_chemical_formula_weight         1313.31
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-07-08
_audit_creation_method
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Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.9774(8)
_cell_length_b                   16.3898(4)
_cell_length_c                   23.4059(7)
_cell_measurement_reflns_used    3562
_cell_measurement_temperature    173
_cell_measurement_theta_max      68.3920
_cell_measurement_theta_min      3.7540
_cell_volume                     7280.1(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.3291
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_details
;
  1 omega   -6.00   20.00   1.0000    8.0450
omega____ theta____ kappa____ phi______ frames
    -      -33.5000   57.0000  -30.0000 26

  2 omega  -69.00  -19.00   1.0000    8.0450
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  -19.0000 -180.0000 50

  3 omega  -47.00  -21.00   1.0000    8.0450
omega____ theta____ kappa____ phi______ frames
    -      -33.5000   57.0000  -30.0000 26

  4 omega   23.00   49.00   1.0000    8.0450
omega____ theta____ kappa____ phi______ frames
    -       35.5136 -125.0000   90.0000 26

  5 omega  -31.00    4.00   1.0000    8.0450
omega____ theta____ kappa____ phi______ frames
    -       35.5136  -57.0000   90.0000 35

  6 omega   41.00   74.00   1.0000    8.0450
omega____ theta____ kappa____ phi______ frames
    -       35.5136  -99.0000  150.0000 33

  7 omega   50.00  100.00   1.0000    8.0450
omega____ theta____ kappa____ phi______ frames
    -       35.5136   57.0000  -60.0000 50

  8 omega   23.00   65.00   1.0000    8.0450
omega____ theta____ kappa____ phi______ frames
    -       35.5136 -125.0000  150.0000 42

  9 omega    9.00   52.00   1.0000    8.0450
omega____ theta____ kappa____ phi______ frames
    -       35.5136  -57.0000   90.0000 43

 10 omega   79.00  109.00   1.0000   25.1750
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000  120.0000 30

 11 omega   40.00   86.00   1.0000   25.1750
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000 -177.0000 46

 12 omega   46.00   99.00   1.0000   25.1750
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -90.0000 53

 13 omega  101.00  160.00   1.0000   25.1750
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000  -90.0000 59

 14 omega   38.00   91.00   1.0000   25.1750
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  150.0000 53

 15 omega   40.00   65.00   1.0000   25.1750
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -120.0000 25

 16 omega   42.00   99.00   1.0000   25.1750
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -30.0000 57

 17 omega   59.00   89.00   1.0000   25.1750
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -180.0000 30
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0638023000
_diffrn_orient_matrix_UB_12      -0.0352675000
_diffrn_orient_matrix_UB_13      0.0324102000
_diffrn_orient_matrix_UB_21      0.0476004000
_diffrn_orient_matrix_UB_22      -0.0185003000
_diffrn_orient_matrix_UB_23      0.0517289000
_diffrn_orient_matrix_UB_31      -0.0160523000
_diffrn_orient_matrix_UB_32      0.0851063000
_diffrn_orient_matrix_UB_33      0.0246172000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_av_unetI/netI     0.0532
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            20154
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.911
_diffrn_reflns_theta_min         3.777
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.635
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.23972
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
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    1.198
_exptl_crystal_description       block
_exptl_crystal_F_000             2767
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.997
_refine_diff_density_min         -0.421
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         7003
_refine_ls_number_restraints     423
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.1157
_refine_ls_R_factor_gt           0.0717
_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^)+(0.1295P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2061
_refine_ls_wR_factor_ref         0.2402
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4150
_reflns_number_total             7003
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00098_si_002.cif
_cod_data_source_block           NHC-L
_cod_depositor_comments
'Adding full bibliography for 4345678--4345679.cif.'
_cod_database_code               4345679
_chemical_oxdiff_formula         'C H O N Cl'
_chemical_oxdiff_usercomment     RAMU
_shelx_estimated_absorpt_t_max   0.791
_shelx_estimated_absorpt_t_min   0.736
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Restrained distances
 C28-C27A
 1.54 with sigma of 0.01
 C28-C29A
 1.54 with sigma of 0.01
 C28-C27B
 1.54 with sigma of 0.01
 C28-C29B
 1.54 with sigma of 0.01
 C37-N4 = C33-N4
 1.39 with sigma of 0.01
 C1-N1 = C5-N1
 1.39 with sigma of 0.01
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(C27A) = Uanis(C27B)
Uanis(C29A) = Uanis(C29B)
5. Others
 Sof(C27B)=Sof(H27D)=Sof(H27E)=Sof(H27F)=Sof(C29B)=Sof(H29D)=Sof(H29E)=
 Sof(H29F)=Sof(H28A)=1-FVAR(1)
 Sof(C27A)=Sof(H27A)=Sof(H27B)=Sof(H27C)=Sof(C29A)=Sof(H29A)=Sof(H29B)=
 Sof(H29C)=Sof(H28)=FVAR(1)
 Fixed Sof: Br1(0.663) Cl1(0.337)
6.a Ternary CH refined with riding coordinates:
 C31(H31), C28(H28), C28(H28A), C13(H13), C16(H16)
6.b Aromatic/amide H refined with riding coordinates:
 C20(H20), C7(H7), C19(H19), C23(H23), C18(H18), C11(H11), C34(H34), C25(H25),
 C36(H36), C37(H37), C4(H4), C33(H33), C5(H5), C2(H2), C1(H1)
6.c Idealised Me refined as rotating group:
 C27A(H27A,H27B,H27C), C29A(H29A,H29B,H29C), C27B(H27D,H27E,H27F), C29B(H29D,
 H29E,H29F), C32(H32A,H32B,H32C), C12(H12A,H12B,H12C), C30(H30A,H30B,H30C),
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              63793
_shelx_hkl_checksum              97270
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'