Synthesis, crystal structures and properties of five novel coordination polymers and application in removing heavy metals from water
Li, Kan; Li, Jing-jing; Zhao, Ni; Di, Bin; Ma, Ying; Xu, Li-li; Inorganica Chimica Acta 507 (2020) 119598–; doi:10.1016/j.ica.2020.119598

data_1564751
_publ_section_title
;
 Synthesis, crystal structures and properties of five novel coordination
 polymers and application in removing heavy metals from water
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119598
_journal_paper_doi               10.1016/j.ica.2020.119598
_journal_volume                  507
_journal_year                    2020
_chemical_formula_moiety         'C18 H15 N2 O4 Zn, 5(H2 O)'
_chemical_formula_sum            'C18 H25 N2 O9 Zn'
_chemical_formula_weight         478.77
_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     dual
_audit_contact_author_name
;
;
_audit_creation_date             2019-01-13
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 109.775(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7277(4)
_cell_length_b                   16.5367(5)
_cell_length_c                   12.4359(5)
_cell_measurement_reflns_used    11072
_cell_measurement_temperature    298.19(10)
_cell_measurement_theta_max      30.4670
_cell_measurement_theta_min      2.0170
_cell_volume                     2076.04(14)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_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_environment      air
_diffrn_ambient_temperature      298.19(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.795
_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    -36.00   9.00   0.50    0.21    --   -3.93 -37.00  76.00   90
  2  \w     -2.00  39.00   0.50    0.21    --    6.28 -99.00  60.00   82
  3  \w    -13.00  40.00   0.50    0.21    --    6.28 -99.00 150.00  106
  4  \w    -12.00  36.00   0.50    0.21    --    6.28 -99.00   0.00   96
  5  \w    -16.00  65.00   0.50    0.21    --   -3.93  37.00-128.00  162
  6  \w    -77.00 -49.00   0.50    0.21    --   -3.93 -37.00  76.00   56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0570573000
_diffrn_orient_matrix_UB_12      0.0181249000
_diffrn_orient_matrix_UB_13      -0.0062990000
_diffrn_orient_matrix_UB_21      -0.0241476000
_diffrn_orient_matrix_UB_22      -0.0090389000
_diffrn_orient_matrix_UB_23      -0.0592347000
_diffrn_orient_matrix_UB_31      -0.0331622000
_diffrn_orient_matrix_UB_32      0.0378067000
_diffrn_orient_matrix_UB_33      -0.0111606000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.795
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21446
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.795
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.098
_diffrn_reflns_theta_min         2.017
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.236
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81755
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_description       needle
_exptl_crystal_F_000             996
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.013
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         5306
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0596P)^2^+1.4990P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1049
_refine_ls_wR_factor_ref         0.1120
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4220
_reflns_number_total             5306
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-507-119598.cif
_cod_data_source_block           CP1
_cod_database_code               1564751
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.89
_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 C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Riding coordinates:
 O5(H5A,H5B), O8(H8C,H8D), O7(H7C,H7D), O9(H9A,H9B), O6(H6C,H6D)
2.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C7(H7A,H7B), C6(H6A,H6B)
2.c Aromatic/amide H refined with riding coordinates:
 C17(H17), C11(H11), C12(H12), C10(H10), C13(H13), C1(H1), C5(H5), C2(H2),
 C4(H4)
;
_shelx_res_checksum              44904
_shelx_hkl_checksum              80054
_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 1.281
_oxdiff_exptl_absorpt_empirical_full_min 0.716