Structures and magnetic studies of four new Ni(ii) coordination polymers built using symmetrical tetracarboxylate and N-donor linkers
Zhang, Xiaoyu; Qin, Tianrui; Liu, Yichen; An, Ning; Afzal, Mohd; Alarifi, Abdullah; Muddassir, Mohd.; Sakiyama, Hiroshi; Mohanty, Aurobinda; Dong, Xiuyan; New Journal of Chemistry 47 (2023) 21214–21224; doi:10.1039/D3NJ03643J

data_7062838
_publ_section_title
;
 Structures and magnetic studies of four new Ni(ii) coordination polymers
 built using symmetrical tetracarboxylate and N-donor linkers
;
_journal_issue                   46
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              21214
_journal_page_last               21224
_journal_paper_doi               10.1039/D3NJ03643J
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C21 H17 N2 Ni O6, C18 H11 O8'
_chemical_formula_sum            'C39 H28 N2 Ni O14'
_chemical_formula_weight         807.34
_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
_audit_creation_date             2023-07-15
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6405)
;
_audit_update_record
;
2023-07-18 deposited with the CCDC.	2023-10-09 downloaded from the CCDC.
;
_cell_angle_alpha                68.685(10)
_cell_angle_beta                 66.871(9)
_cell_angle_gamma                88.769(8)
_cell_formula_units_Z            2
_cell_length_a                   11.5719(10)
_cell_length_b                   11.9790(12)
_cell_length_c                   14.2548(15)
_cell_measurement_reflns_used    4075
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.9160
_cell_measurement_theta_min      3.6490
_cell_volume                     1675.8(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1281
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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     14.00 100.00   1.00    1.00    --   36.81  37.00 -90.00   86
  2  \w     17.00  43.00   1.00    1.00    --   36.81 -77.00-180.00   26
  3  \w     54.00  91.00   1.00    1.00    --   36.81-125.00 -90.00   37
  4  \w     32.00  58.00   1.00    1.00    --   36.81 -99.00 -90.00   26
  5  \w     19.00  46.00   1.00    1.00    --   36.81-125.00 150.00   27
  6  \w     58.00  90.00   1.00    1.00    --   36.81-125.00 150.00   32
  7  \w    -32.00  62.00   1.00    1.00    --   36.81 -77.00  60.00   94
  8  \w     42.00  99.00   1.00    1.00    --   36.81  57.00   0.00   57
  9  \w    -25.00   1.00   1.00    1.00    --   36.81 -37.00  90.00   26
 10  \w     -3.00  22.00   1.00    1.00    --   36.81 -99.00 -90.00   25
 11  \w     11.00  59.00   1.00    1.00    --   36.81 -37.00  90.00   48
 12  \w     24.00  62.00   1.00    1.00    --   36.81 -99.00   0.00   38
 13  \w    -20.00   8.00   1.00    1.00    --   36.81 -77.00-180.00   28
 14  \w    -22.00  55.00   1.00    1.00    --   36.81 -19.00-120.00   77
 15  \w    120.00 164.00   1.00    1.00    --  108.00 111.00 120.00   44
 16  \w     37.00 109.00   1.00    1.00    --  108.00-111.00-120.00   72
 17  \w    100.00 176.00   1.00    1.00    --  108.00  50.00  60.00   76
 18  \w    145.00 177.00   1.00    1.00    --  108.00  31.00 148.00   32
 19  \w     39.00 126.00   1.00    1.00    --  108.00 -50.00-150.00   87
 20  \w    130.00 173.00   1.00    1.00    --  108.00  25.00 -30.00   43
 21  \w     98.00 124.00   1.00    1.00    --  108.00  25.00 -30.00   26
 22  \w     87.00 112.00   1.00    1.00    --  108.00-111.00 120.00   25
 23  \w     51.00  98.00   1.00    1.00    --  108.00 -77.00  60.00   47
 24  \w     40.00  66.00   1.00    1.00    --  108.00-111.00 120.00   26
 25  \w     84.00 139.00   1.00    1.00    --  108.00  31.00 148.00   55
 26  \w     65.00 142.00   1.00    1.00    --  108.00 -91.00 -90.00   77
 27  \w    104.00 144.00   1.00    1.00    --  108.00 111.00   0.00   40
 28  \w    145.00 174.00   1.00    1.00    --  108.00  25.00   0.00   29
 29  \w     71.00  96.00   1.00    1.00    --  108.00-111.00-180.00   25
 30  \w     82.00 107.00   1.00    1.00    --  108.00-111.00  30.00   25
 31  \w     37.00 127.00   1.00    1.00    --  108.00 -37.00 -30.00   90
 32  \w     41.00 107.00   1.00    1.00    --  108.00 -50.00  90.00   66
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0768083000
_diffrn_orient_matrix_UB_12      -0.1160960000
_diffrn_orient_matrix_UB_13      0.0198673000
_diffrn_orient_matrix_UB_21      -0.1244222000
_diffrn_orient_matrix_UB_22      0.0495435000
_diffrn_orient_matrix_UB_23      0.0475077000
_diffrn_orient_matrix_UB_31      0.0022672000
_diffrn_orient_matrix_UB_32      0.0592826000
_diffrn_orient_matrix_UB_33      -0.1165320000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_unetI/netI     0.0536
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10807
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.237
_diffrn_reflns_theta_max         67.237
_diffrn_reflns_theta_min         3.655
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.538
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86763
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.600
_exptl_crystal_description       block
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.324
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     527
_refine_ls_number_reflns         5991
_refine_ls_number_restraints     1472
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0477
_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^)+(0.0549P)^2^+0.3747P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1179
_refine_ls_wR_factor_ref         0.1302
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4702
_reflns_number_total             5991
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj03643j2.cif
_cod_data_source_block           exp_10929
_cod_depositor_comments
'Adding full bibliography for 7062838--7062841.cif.'
_cod_database_code               7062838
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.849
_shelx_estimated_absorpt_t_min   0.837
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 C9-C9_$1
 1.33 with sigma of 0.01
3. Rigid bond restraints
 C5, C6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 3.8A with sigma of 0.02 and sigma
for terminal atoms of 0.04 within 3.8A
5. Others
 Sof(C9')=Sof(H9')=1-FVAR(1)
 Sof(C9)=Sof(H9)=FVAR(1)
6.a Riding coordinates:
 O13(H13A,H13B)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C9(H9), C9'(H9'), C10(H10), C11(H11), C12(H12),
 C14(H14), C15(H15), C17(H17), C18(H18), C19(H19), C24(H24), C26(H26), C28(H28),
  C29(H29), C30(H30), C32(H32), C34(H34), C36(H36)
6.c Idealised tetrahedral OH refined as rotating group:
 O4(H4), O6(H6), O7(H7A), O12(H12A)
;
_shelx_res_checksum              76179
_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 1.144
_oxdiff_exptl_absorpt_empirical_full_min 0.796