Highly efficient removal of As(V) from aqueous solutions using a novel octanuclear Zn(II)-based polymer: Synthesis, structure, properties and optimization using a response surface methodology
Xiao, Yu; Zhang, Chong; Qin, Yan; Wu, Chengchen; Zheng, Xiao; Journal of Solid State Chemistry 264 (2018) 6–14; doi:10.1016/j.jssc.2018.04.030

data_1561023
_publ_section_title
;
 Highly efficient removal of As(V) from aqueous solutions using a novel
 octanuclear Zn(II)-based polymer: Synthesis, structure, properties and
 optimization using a response surface methodology
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              6
_journal_page_last               14
_journal_paper_doi               10.1016/j.jssc.2018.04.030
_journal_volume                  264
_journal_year                    2018
_chemical_formula_moiety         'C22 H18 N10 O24 Zn8'
_chemical_formula_sum            'C22 H18 N10 O24 Zn8'
_chemical_formula_weight         1329.42
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_cell_angle_alpha                78.901(12)
_cell_angle_beta                 85.319(12)
_cell_angle_gamma                75.131(14)
_cell_formula_units_Z            1
_cell_length_a                   6.8131(11)
_cell_length_b                   9.1255(15)
_cell_length_c                   13.2080(17)
_cell_measurement_reflns_used    1606
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.4730
_cell_measurement_theta_min      3.9530
_cell_volume                     778.4(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0233
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.895
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
  1 omega   -2.00   88.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       19.0173   57.0000   30.0000 90

  2 omega  -24.00    7.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.9782  -77.0000   30.0000 31

  3 omega  -12.00   61.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       19.0173  -99.0000  -90.0000 73

  4 omega  -52.00   73.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       19.0173    0.0000 -180.0000 125

  5 omega  -73.00    0.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.9782  -57.0000  120.0000 73
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0674008000
_diffrn_orient_matrix_UB_12      0.0449302000
_diffrn_orient_matrix_UB_13      0.0065264000
_diffrn_orient_matrix_UB_21      0.0232171000
_diffrn_orient_matrix_UB_22      0.0108066000
_diffrn_orient_matrix_UB_23      -0.0538416000
_diffrn_orient_matrix_UB_31      -0.0808331000
_diffrn_orient_matrix_UB_32      0.0674078000
_diffrn_orient_matrix_UB_33      -0.0075428000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_unetI/netI     0.0607
_diffrn_reflns_Laue_measured_fraction_full 0.895
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5102
_diffrn_reflns_point_group_measured_fraction_full 0.895
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.097
_diffrn_reflns_theta_min         3.513
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.182
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62301
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    2.836
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             652
_refine_diff_density_max         1.472
_refine_diff_density_min         -2.032
_refine_diff_density_rms         0.226
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.148
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         2749
_refine_ls_number_restraints     136
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.0858
_refine_ls_R_factor_gt           0.0724
_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^)+(0.0446P)^2^+22.9820P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1742
_refine_ls_wR_factor_ref         0.1821
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2283
_reflns_number_total             2749
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            JSSC-2018-264-6.cif
_cod_data_source_block           zn8
_cod_database_code               1561023
_chemical_oxdiff_formula         'C1 H1 O1 N1 Zn1'
_reflns_odcompleteness_completeness 99.62
_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 O(H) groups
 At 1.5 times of:
  All N(H,H) groups, All O(H,H) groups
2. Restrained distances
 O9-H9
 0.86 with sigma of 0.01
 O11-H11
 0.86 with sigma of 0.01
 O10-H10
 0.85 with sigma of 0.01
3. Rigid bond restraints
 C5
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O3, C5
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
O5 \\sim O8 \\sim O6 \\sim O9 \\sim O11 \\sim O12 \\sim O10 \\sim O2 \\sim O1
\\sim O7 \\sim O3 \\sim O4 \\sim O4': within 3.8A with sigma of 0.005 and sigma
for terminal atoms of 0.01
Uanis(O3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(O4')=1-FVAR(1)
 Sof(O4)=FVAR(1)
 Fixed Sof: Zn5(0.5)
6.a Riding coordinates:
 O11(H11), O10(H10)
6.b Rotating group:
 O12(H12A,H12B)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6)
;