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_1564755
_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         'C36 H32 Cu2 N4 O9, 1(H2 O)'
_chemical_formula_sum            'C36 H34 Cu2 N4 O10'
_chemical_formula_weight         809.767
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_contact_author_name
;
;
_audit_creation_date             2019-01-27
_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                 113.248(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   35.6022(10)
_cell_length_b                   10.8915(3)
_cell_length_c                   20.6144(5)
_cell_measurement_reflns_used    12264
_cell_measurement_temperature    298.33(10)
_cell_measurement_theta_max      31.0680
_cell_measurement_theta_min      1.9670
_cell_volume                     7344.4(4)
_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      298.33(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.796
_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    -70.00 -22.00   0.50    3.00    --   -3.93 -57.00-120.00   96
  2  \w     -2.00  39.00   0.50    3.00    --    6.20 -99.00-120.00   82
  3  \w      7.00  35.00   0.50    3.00    --    6.20 -99.00  90.00   56
  4  \w    -74.00  10.00   0.50    3.00    --   -3.93 -57.00 -30.00  168
;
_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      -0.0076006000
_diffrn_orient_matrix_UB_12      -0.0004897000
_diffrn_orient_matrix_UB_13      0.0198369000
_diffrn_orient_matrix_UB_21      -0.0040658000
_diffrn_orient_matrix_UB_22      -0.0646610000
_diffrn_orient_matrix_UB_23      -0.0011796000
_diffrn_orient_matrix_UB_31      0.0340022000
_diffrn_orient_matrix_UB_32      -0.0078441000
_diffrn_orient_matrix_UB_33      0.0086829000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_unetI/netI     0.0616
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.796
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            25338
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.796
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.938
_diffrn_reflns_theta_min         1.971
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.219
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46316
_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            blue
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_description       rhombus
_exptl_crystal_F_000             3312
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.870
_refine_diff_density_min         -0.627
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         9268
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0370
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0621P)^2^+8.1805P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1030
_refine_ls_wR_factor_ref         0.1100
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7283
_reflns_number_total             9268
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-507-119598.cif
_cod_data_source_block           CP5
_cod_database_code               1564755
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.82
_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. Others
 Fixed Sof: O10(0.5) H10A(0.5) H10B(0.5) O11(0.25) H11A(0.25) H11B(0.25)
 Fixed U11: O11(0.198478)
 Fixed U12: O11(0.013369)
 Fixed U13: O11(-0.012542)
 Fixed U22: O11(0.08286)
 Fixed U23: O11(0.03622)
 Fixed U33: O11(0.0995)
3.a Riding coordinates:
 O5(H5A,H5B), O10(H10A,H10B), O11(H11A,H11B)
3.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C24(H24A,H24B), C25(H25A,H25B),
 C26(H26A,H26B)
3.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C10(H10), C11(H11), C12(H12), C13(H13),
 C17(H17), C19(H19), C20(H20), C22(H22), C23(H23), C27(H27), C28(H28), C30(H30),
  C31(H31), C34(H34)
;
_shelx_res_checksum              62684
_shelx_hkl_checksum              70802
_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 1.796
_oxdiff_exptl_absorpt_empirical_full_min 0.697