Synthesis and characterisation of neodymium-based MOFs for application in carbon dioxide reduction to syngas
Marazani, Linia Gedi; Gumbo, Maureen; Moyo, Lendly; Makhubela, Banothile C. E.; Mehlana, Gift; New Journal of Chemistry 48 (2024) 15025–15035; doi:10.1039/D4NJ01420K

data_7063377
_publ_section_title
;
 Synthesis and characterisation of neodymium-based MOFs for application in
 carbon dioxide reduction to syngas
;
_journal_issue                   34
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              15025
_journal_page_last               15035
_journal_paper_doi               10.1039/D4NJ01420K
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety         'C168 H128 N32 Nd8 O60, 7(C3 H7 N O)'
_chemical_formula_sum            'C189 H177 N39 Nd8 O67'
_chemical_formula_weight         5220.61
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-07-06
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-07-08 deposited with the CCDC.	2024-07-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.5206(12)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   27.4090(3)
_cell_length_b                   11.1853(2)
_cell_length_c                   16.97965(19)
_cell_measurement_reflns_used    20187
_cell_measurement_temperature    143.8(3)
_cell_measurement_theta_max      75.1970
_cell_measurement_theta_min      3.2350
_cell_volume                     5148.13(12)
_computing_cell_refinement       'CrysAlisPro 1.171.43.125a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.125a 64-bit (release 04-06-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.125a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      143.8(3)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.946
_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    -78.00   1.00   0.50    0.49    --  -42.72 103.00 -12.00  158
  2  \w      5.00  78.00   0.50    0.49    --   42.72-103.00-114.00  146
  3  \w    -92.00 -31.00   0.50    1.97    -- -104.50 103.00 -12.00  122
  4  \w   -174.00-103.00   0.50    1.97    -- -104.50-103.00-114.00  142
  5  \w     36.00  92.00   0.50    1.97    --  109.22-103.00-114.00  112
  6  \w    110.00 178.00   0.50    1.97    --  109.22 103.00 -12.00  136
  7  \w    -15.00  35.00   0.50    0.49    --  -42.72  38.00 -90.00  100
  8  \w    -15.00  35.00   0.50    0.49    --  -42.72  38.00  60.00  100
  9  \w     27.00  54.00   0.50    0.49    --   42.72  61.00 158.24   54
 10  \w     29.00  60.00   0.50    0.49    --   42.72  54.00 144.91   62
 11  \w     27.00  54.00   0.50    0.49    --   42.72  61.00 -12.15   54
 12  \w     28.00  60.00   0.50    0.49    --   42.72  58.00-173.34   64
 13  \w     28.00  60.00   0.50    0.49    --   42.72  58.00  23.85   64
 14  \w     27.00  56.00   0.50    0.49    --   42.72  60.00  88.96   58
 15  \w     27.00  54.00   0.50    0.49    --   42.72  61.00-130.84   54
 16  \w     27.00  54.00   0.50    0.49    --   42.72  61.00 178.68   54
 17  \w     27.00  54.00   0.50    0.49    --   42.72  61.00 113.35   54
 18  \w   -132.00 -89.00   0.50    1.97    -- -104.50 -15.00 150.00   86
 19  \w    -98.00 -33.00   0.50    1.97    -- -104.50 119.00-117.58  130
 20  \w   -101.00 -33.00   0.50    1.97    -- -104.50 125.00-120.00  136
 21  \w    -92.00 -31.00   0.50    1.97    -- -104.50  93.00 -20.07  122
 22  \w   -132.00 -89.00   0.50    1.97    -- -104.50 -15.00  60.00   86
 23  \w   -132.00 -89.00   0.50    1.97    -- -104.50 -15.00 -90.00   86
 24  \w    -72.00 -30.00   0.50    1.97    -- -104.50  77.00-180.00   84
 25  \w   -132.00 -89.00   0.50    1.97    -- -104.50 -15.00-150.00   86
 26  \w   -163.00 -90.00   0.50    1.97    -- -104.50 -30.00 -90.00  146
 27  \w   -132.00 -89.00   0.50    1.97    -- -104.50 -15.00 -60.00   86
 28  \w     35.00  92.00   0.50    1.97    --  109.22 -95.00 -60.00  114
 29  \w    109.00 178.00   0.50    1.97    --  109.22  77.00-180.00  138
 30  \w     94.00 139.00   0.50    1.97    --  109.22  15.00  30.00   90
 31  \w     94.00 139.00   0.50    1.97    --  109.22  15.00 150.00   90
 32  \w     35.00  79.00   0.50    1.97    --  109.22 -77.00  60.00   88
 33  \w     35.00  79.00   0.50    1.97    --  109.22 -77.00 -90.00   88
 34  \w    -15.00  25.00   0.50    0.49    --  -42.72  38.00 150.00   80
 35  \w     29.00  60.00   0.50    0.49    --   42.72  54.00 -88.74   62
 36  \w     28.00  60.00   0.50    0.49    --   42.72  55.00  52.67   64
 37  \w     27.00  56.00   0.50    0.49    --   42.72  60.00 -62.79   58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0498125000
_diffrn_orient_matrix_UB_12      0.0596772000
_diffrn_orient_matrix_UB_13      -0.0071684000
_diffrn_orient_matrix_UB_21      0.0268854000
_diffrn_orient_matrix_UB_22      -0.1180670000
_diffrn_orient_matrix_UB_23      0.0249656000
_diffrn_orient_matrix_UB_31      -0.0051978000
_diffrn_orient_matrix_UB_32      -0.0382755000
_diffrn_orient_matrix_UB_33      -0.0879778000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0549
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            43842
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.692
_diffrn_reflns_theta_min         3.261
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.901
_exptl_absorpt_correction_T_max  0.786
_exptl_absorpt_correction_T_min  0.206
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.125a (Rigaku Oxford Diffraction, 2024)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.684
_exptl_crystal_description       block
_exptl_crystal_F_000             2600
_exptl_crystal_size_max          0.196
_exptl_crystal_size_mid          0.084
_exptl_crystal_size_min          0.029
_refine_diff_density_max         3.179
_refine_diff_density_min         -1.931
_refine_diff_density_rms         0.137
_refine_ls_extinction_coef       0.000103(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     679
_refine_ls_number_reflns         10133
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0541
_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^)+(0.0687P)^2^+33.3776P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1361
_refine_ls_wR_factor_ref         0.1417
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8615
_reflns_number_total             10133
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj01420k2.cif
_cod_data_source_block           exp_1222_auto
_cod_depositor_comments
'Adding full bibliography for 7063377--7063378.cif.'
_cod_original_cell_volume        5148.13(13)
_cod_database_code               7063377
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C46 H50 N10 O16 Nd2 '
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C2) = Uanis(C1)
Uanis(C1) = Uanis(N7) = Uanis(C8) = Uanis(O74) = Uanis(C2)
3. Rigid body (RIGU) restrains
 C1, C2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: O74(0.75) C8(0.75) H8(0.75) C1(0.75) H1A(0.75) H1B(0.75) H1C(0.75)
 C2(0.75) H2A(0.75) H2B(0.75) H2C(0.75) N7(0.75)
5.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C3(H3), C14(H14), C19(H19), C22(H22), C10(H10), C13(H13), C16(H16),
 C20(H20), C40(H40), C64(H64), C38(H38), C31(H31), C32(H32), C51(H51), C37(H37),
  C49(H49), C59(H59), C34(H34), C69(H69), C57(H57), C8(H8)
5.b Idealised Me refined as rotating group:
 C72(H72A,H72B,H72C), C67(H67A,H67B,H67C), C62(H62A,H62B,H62C), C71(H71A,H71B,
 H71C), C66(H66A,H66B,H66C), C61(H61A,H61B,H61C), C1(H1A,H1B,H1C), C2(H2A,H2B,
 H2C)
;
_shelx_res_checksum              96332
_shelx_hkl_checksum              38973
_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 1.457
_oxdiff_exptl_absorpt_empirical_full_min 0.763