Selective recognition of Fe3+ and CrO42- ions using Zn(II) metallacycle and Cd(II) coordination polymer and their heterogeneous catalytic application
Kumar, Girijesh; Rani, Pooja; Sharma, Anjali; Husain, Ahmad; Kumar, Gulshan; Kaur, Harpreet; Bhasin, K.k; CrystEngComm  (2019) –; doi:10.1039/C9CE01357A

data_7234880
_publ_section_title
;
 Selective recognition of Fe3+ and CrO42- ions using Zn(II) metallacycle
 and Cd(II) coordination polymer and their heterogeneous catalytic
 application
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C9CE01357A
_journal_year                    2019
_chemical_formula_moiety         'C48 H56 N14 O14 Zn2, N2 O6'
_chemical_formula_sum            'C48 H56 N16 O20 Zn2'
_chemical_formula_weight         1307.82
_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             2019-10-07
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2019.10.03 svn.r3662 for OlexSys, GUI svn.r5948)
;
_audit_update_record
;
2019-10-23 deposited with the CCDC.    2019-10-28 downloaded from the CCDC.
;
_cell_angle_alpha                93.775(3)
_cell_angle_beta                 102.159(2)
_cell_angle_gamma                112.230(3)
_cell_formula_units_Z            1
_cell_length_a                   9.3608(3)
_cell_length_b                   9.9545(4)
_cell_length_c                   17.4674(5)
_cell_measurement_reflns_used    12715
_cell_measurement_temperature    298
_cell_measurement_theta_max      27.1730
_cell_measurement_theta_min      3.3270
_cell_volume                     1453.70(9)
_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 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS n/a (Sheldrick, 2008)'
_diffrn_ambient_temperature      298
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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    -45.00 -19.00   0.50    7.00    --   -9.95 110.00 152.00   52
  2  \w     -9.00  50.00   0.50    7.00    --   10.22-110.00  57.00  118
  3  \w    -73.00   3.00   0.50    7.00    --   -9.95 -57.00  60.00  152
  4  \w    -52.00 -13.00   0.50    7.00    --   -9.95 125.00-150.00   78
  5  \w    -35.00  -8.00   0.50    7.00    --   10.22 120.00 116.64   54
  6  \w    -54.00 -29.00   0.50    7.00    --   10.22 -77.00-150.00   50
  7  \w    -19.00  22.00   0.50    7.00    --   10.22 -77.00-150.00   82
  8  \w    -19.00   6.00   0.50    7.00    --   10.22 -99.00  90.00   50
  9  \w    -30.00  -5.00   0.50    7.00    --   10.22 121.00 -98.95   50
 10  \w     11.00  37.00   0.50    7.00    --   10.22 -99.00  90.00   52
 11  \w    -51.00  24.00   0.50    7.00    --   10.22 -38.00 120.00  150
 12  \w    -24.00   1.00   0.50    7.00    --   10.22 121.00 156.61   50
 13  \w    -14.00  75.00   0.50    7.00    --   10.22  77.00 -30.00  178
 14  \w    -60.00  21.00   0.50    7.00    --   10.22 -19.00-180.00  162
 15  \w    -54.00  13.00   0.50    7.00    --   10.22 -38.00 -90.00  134
;
_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      -0.0000366000
_diffrn_orient_matrix_UB_12      -0.0673606000
_diffrn_orient_matrix_UB_13      0.0109691000
_diffrn_orient_matrix_UB_21      -0.0043454000
_diffrn_orient_matrix_UB_22      -0.0253179000
_diffrn_orient_matrix_UB_23      -0.0396878000
_diffrn_orient_matrix_UB_31      0.0845446000
_diffrn_orient_matrix_UB_32      0.0300684000
_diffrn_orient_matrix_UB_33      0.0087116000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0513
_diffrn_reflns_av_unetI/netI     0.0496
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18354
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.996
_diffrn_reflns_theta_min         3.337
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.913
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76001
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_description       block
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.423
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         5702
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0433
_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^)+(0.0584P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1082
_refine_ls_wR_factor_ref         0.1143
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4422
_reflns_number_total             5702
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce01357a2.cif
_cod_data_source_block           1
_cod_database_code               7234880
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Zn C H N O'
_shelx_estimated_absorpt_t_max   0.898
_shelx_estimated_absorpt_t_min   0.838
_reflns_odcompleteness_completeness 99.71
_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 N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N2(H2), N3(H3), C1(H1), C2(H2A), C3(H3A), C5(H5), C8(H8), C9(H9), C11(H11),
 C12(H12), C15(H15), C16(H16), C17(H17), C18(H18), C21(H21), C22(H22)
2.b Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C)
;
_shelx_res_checksum              48593
_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 1.427
_oxdiff_exptl_absorpt_empirical_full_min 0.753