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_4345678
_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
'C74 H86 Cl4 N8 Zn2, C37 H40 Cl6 N4 Zn2, Cl, 2(O)'
_chemical_formula_sum            'C111 H126 Cl11 N12 O2 Zn4'
_chemical_formula_weight         2311.66
_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     direct
_audit_creation_date             2016-07-08
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                65.686(9)
_cell_angle_beta                 71.588(9)
_cell_angle_gamma                73.124(9)
_cell_formula_units_Z            1
_cell_length_a                   15.443(12)
_cell_length_b                   16.958(13)
_cell_length_c                   16.998(13)
_cell_measurement_reflns_used    9802
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.53
_cell_measurement_theta_min      2.21
_cell_volume                     3782(5)
_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      100.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0988
_diffrn_reflns_av_unetI/netI     0.0715
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            54978
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        21.260
_diffrn_reflns_theta_max         21.260
_diffrn_reflns_theta_min         1.531
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.861
_exptl_absorpt_correction_T_max  0.7446
_exptl_absorpt_correction_T_min  0.4944
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1150 before and 0.0636 after correction.
The Ratio of minimum to maximum transmission is 0.6640.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.015
_exptl_crystal_description       block
_exptl_crystal_F_000             1199
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.494
_refine_diff_density_min         -0.722
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.548
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     866
_refine_ls_number_reflns         8435
_refine_ls_number_restraints     988
_refine_ls_restrained_S_all      1.488
_refine_ls_R_factor_all          0.1766
_refine_ls_R_factor_gt           0.1310
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3751
_refine_ls_wR_factor_ref         0.4032
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5480
_reflns_number_total             8435
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00098_si_003.cif
_cod_data_source_block           NHC-Zn
_cod_depositor_comments
'Adding full bibliography for 4345678--4345679.cif.'
_cod_original_cell_volume        3783(5)
_cod_database_code               4345678
_shelx_estimated_absorpt_t_max   0.896
_shelx_estimated_absorpt_t_min   0.847
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.951(4) 0.049(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C46-N7
 1.45 with sigma of 0.01
 C46-N8
 1.45 with sigma of 0.01
 C66-N7
 1.2 with sigma of 0.01
 C66-N8
 1.2 with sigma of 0.01
 C45-C58
 1.54 with sigma of 0.02
 C57-C58
 1.54 with sigma of 0.02
 C58-C59
 1.54 with sigma of 0.02
 C43-C44
 1.39 with sigma of 0.02
 C44-C45
 1.39 with sigma of 0.02
 C45-C46
 1.39 with sigma of 0.02
 C46-C47
 1.39 with sigma of 0.02
 C43-C48
 1.39 with sigma of 0.02
 C47-C48
 1.39 with sigma of 0.02
 C47-C49
 1.39 with sigma of 0.02
 C49-C50
 1.39 with sigma of 0.02
 C45-C51
 1.39 with sigma of 0.02
 C50-C51
 1.39 with sigma of 0.02
 N5-C38
 1.39 with sigma of 0.02
 C38-C39
 1.39 with sigma of 0.02
 C39-C40
 1.39 with sigma of 0.02
 C40-C41
 1.39 with sigma of 0.02
 N5-C42
 1.39 with sigma of 0.02
 C41-C42
 1.39 with sigma of 0.02
 C52-C53
 1.39 with sigma of 0.02
 N6-C54
 1.39 with sigma of 0.02
 C53-C54
 1.39 with sigma of 0.02
 N6-C55
 1.39 with sigma of 0.02
 C52-C56
 1.39 with sigma of 0.02
 C55-C56
 1.39 with sigma of 0.02
 C22-C31A
 1.51 with sigma of 0.02
 C30A-C31A
 1.51 with sigma of 0.02
 C31A-C32A
 1.51 with sigma of 0.02
 C22-C31B
 1.51 with sigma of 0.02
 C30B-C31B
 1.51 with sigma of 0.02
 C31B-C32B
 1.51 with sigma of 0.02
 C10-C13A
 1.51 with sigma of 0.02
 C12A-C13A
 1.51 with sigma of 0.02
 C10-C13B
 1.51 with sigma of 0.02
 C12B-C13B
 1.51 with sigma of 0.02
 C13B-C14B
 1.51 with sigma of 0.02
 C13A-C14A
 1.51 with sigma of 0.02
 C47-C60A
 1.51 with sigma of 0.02
 C62A-C60A
 1.51 with sigma of 0.02
 C47-C60B
 1.51 with sigma of 0.02
 C60B-C61B
 1.51 with sigma of 0.02
 C60B-C62B
 1.51 with sigma of 0.02
 C60A-C61A
 1.51 with sigma of 0.02
 C16-C17
 1.51 with sigma of 0.02
 C16-C15
 1.51 with sigma of 0.02
4. 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
5. 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
6. Others
 Sof(Zn2B)=Sof(Cl5B)=Sof(Cl4B)=Sof(N6)=Sof(C49)=Sof(H49)=Sof(C50)=Sof(C51)=
 Sof(H51)=Sof(C52)=Sof(C53)=Sof(H53)=Sof(C54)=Sof(H54)=Sof(C55)=Sof(H55)=
 Sof(C56)=Sof(H56)=1-FVAR(1)
 Sof(Zn2A)=Sof(Cl3A)=Sof(Cl4A)=Sof(N5)=Sof(C38)=Sof(H38)=Sof(C39)=Sof(H39)=
 Sof(C40)=Sof(C41)=Sof(H41)=Sof(C42)=Sof(H42)=Sof(C43)=Sof(C44)=Sof(H44)=
 Sof(C48)=Sof(H48)=FVAR(1)
 Sof(N8)=1-FVAR(2)
 Sof(N7)=FVAR(2)
 Sof(C12B)=Sof(H12D)=Sof(H12E)=Sof(H12F)=Sof(C13B)=Sof(H13B)=Sof(C30B)=
 Sof(H30D)=Sof(H30E)=Sof(H30F)=Sof(C31B)=Sof(H31B)=Sof(C32B)=Sof(H32D)=
 Sof(H32E)=Sof(H32F)=Sof(C60B)=Sof(H60B)=Sof(C61B)=Sof(H61A)=Sof(H61B)=
 Sof(H61C)=Sof(C62B)=Sof(H62A)=Sof(H62B)=Sof(H62C)=Sof(C14B)=Sof(H14D)=
 Sof(H14E)=Sof(H14F)=1-FVAR(3)
 Sof(C12A)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(C13A)=Sof(H13A)=Sof(C30A)=
 Sof(H30A)=Sof(H30B)=Sof(H30C)=Sof(C31A)=Sof(H31A)=Sof(C32A)=Sof(H32A)=
 Sof(H32B)=Sof(H32C)=Sof(C14A)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C62A)=
 Sof(H62D)=Sof(H62E)=Sof(H62F)=Sof(C60A)=Sof(H60A)=Sof(C61A)=Sof(H61D)=
 Sof(H61E)=Sof(H61F)=FVAR(3)
 Sof(Cl3B)=1-FVAR(4)
 Sof(Cl5A)=FVAR(4)
 Fixed Sof: C63(0.5) C65(0.5) Cl9(0.5)
7.a Ternary CH refined with riding coordinates:
 C13A(H13A), C31A(H31A), C13B(H13B), C31B(H31B), C58(H58), C60B(H60B),
 C16(H16), C28(H28), C60A(H60A)
7.b Aromatic/amide H refined with riding coordinates:
 C38(H38), C39(H39), C41(H41), C42(H42), C44(H44), C48(H48), C49(H49),
 C51(H51), C53(H53), C54(H54), C55(H55), C56(H56), C1(H1), C2(H2), C4(H4),
 C5(H5), C7(H7), C11(H11), C18(H18), C19(H19), C20(H20), C23(H23), C25(H25),
 C33(H33), C34(H34), C36(H36), C37(H37)
7.c Idealised Me refined as rotating group:
 C12A(H12A,H12B,H12C), C30A(H30A,H30B,H30C), C32A(H32A,H32B,H32C), C12B(H12D,
 H12E,H12F), C30B(H30D,H30E,H30F), C32B(H32D,H32E,H32F), C57(H57A,H57B,H57C),
 C59(H59A,H59B,H59C), C61B(H61A,H61B,H61C), C62B(H62A,H62B,H62C), C17(H17A,H17B,
 H17C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C14A(H14A,H14B,H14C),
 C14B(H14D,H14E,H14F), C62A(H62D,H62E,H62F), C61A(H61D,H61E,H61F), C15(H15A,
 H15B,H15C)
;
_shelx_res_checksum              49085
_shelx_hkl_checksum              51189
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'