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_1564754
_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 H17 N2 Ni O5'
_chemical_formula_sum            'C18 H17 N2 Ni O5'
_chemical_formula_weight         400.04
_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     dual
_audit_contact_author_name
;
;
_audit_creation_date             2019-02-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                103.527(3)
_cell_angle_beta                 102.627(2)
_cell_angle_gamma                100.436(3)
_cell_formula_units_Z            2
_cell_length_a                   7.3286(2)
_cell_length_b                   9.3775(3)
_cell_length_c                   13.3478(4)
_cell_measurement_reflns_used    9000
_cell_measurement_temperature    298.46(10)
_cell_measurement_theta_max      31.0410
_cell_measurement_theta_min      2.2830
_cell_volume                     843.81(5)
_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      298.46(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.801
_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     22.00  78.00   0.50    1.00    --    6.20  77.00 120.00  112
  2  \w    -14.00  12.00   0.50    1.00    --    6.20  77.00 120.00   52
  3  \w    -76.00  10.00   0.50    1.00    --   -3.93 -57.00 120.00  172
  4  \w      6.00  33.00   0.50    1.00    --    6.20-101.00 118.00   54
  5  \w      4.00  38.00   0.50    1.00    --    6.20 -99.00   0.00   68
  6  \w    -12.00  39.00   0.50    1.00    --    6.20 -99.00 -60.00  102
  7  \w    -14.00  11.00   0.50    1.00    --   -3.93 -57.00-150.00   50
  8  \w    -63.00 -37.00   0.50    1.00    --   -3.93 -57.00-150.00   52
  9  \w    -65.00  21.00   0.50    1.00    --    6.20 -57.00  30.00  172
;
_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      -0.0566569000
_diffrn_orient_matrix_UB_12      -0.0156732000
_diffrn_orient_matrix_UB_13      -0.0534993000
_diffrn_orient_matrix_UB_21      0.0045757000
_diffrn_orient_matrix_UB_22      0.0781789000
_diffrn_orient_matrix_UB_23      0.0078933000
_diffrn_orient_matrix_UB_31      0.0850509000
_diffrn_orient_matrix_UB_32      0.0089807000
_diffrn_orient_matrix_UB_33      -0.0174135000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_unetI/netI     0.0303
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.801
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12566
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.801
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.828
_diffrn_reflns_theta_min         2.304
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.183
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62933
_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            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_description       needle
_exptl_crystal_F_000             414
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         4249
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0292
_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^)+(0.0343P)^2^+0.3158P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0732
_refine_ls_wR_factor_ref         0.0750
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3810
_reflns_number_total             4249
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-507-119598.cif
_cod_data_source_block           CP4
_cod_database_code               1564754
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.871
_shelx_estimated_absorpt_t_min   0.703
_reflns_odcompleteness_completeness 99.91
_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 Rotating group:
 O5(H5A,H5B)
2.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B)
2.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C10(H10), C11(H11), C12(H12), C13(H13),
 C18(H18)
;
_shelx_res_checksum              35875
_shelx_hkl_checksum              32004
_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 1.956
_oxdiff_exptl_absorpt_empirical_full_min 0.578