Tuning the topology of a 2D metal–organic framework from 2D to 3D using modulator assisted synthesis
Hungwe, Johannes; Tshuma, Piwai; Gumbo, Maureen; Noa, Francoise M. Amombo; Öhrström, Lars; Mehlana, Gift; CrystEngComm 25 (2023) 1486–1494; doi:10.1039/D3CE00039G

data_7246263
_publ_section_title
;
 Tuning the topology of a 2D metal--organic framework from 2D to 3D using
 modulator assisted synthesis
;
_journal_issue                   10
_journal_name_full               CrystEngComm
_journal_page_first              1486
_journal_page_last               1494
_journal_paper_doi               10.1039/D3CE00039G
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C21 H20 La N4 O9, C3 H7 N O'
_chemical_formula_sum            'C24 H27 La N5 O10'
_chemical_formula_weight         684.41
_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_creation_date             2022-02-24
_audit_creation_method
;
Olex2 1.5-ac5-018
(compiled 2021.09.08 svn.r13c46975 for Rigaku Oxford Diffraction, GUI svn.r6396)
;
_audit_update_record
;
2022-03-03 deposited with the CCDC.	2023-02-10 downloaded from the CCDC.
;
_cell_angle_alpha                68.670(2)
_cell_angle_beta                 86.130(2)
_cell_angle_gamma                74.590(2)
_cell_formula_units_Z            2
_cell_length_a                   10.0590(2)
_cell_length_b                   11.1837(4)
_cell_length_c                   13.6668(3)
_cell_measurement_reflns_used    27121
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.8220
_cell_measurement_theta_min      3.4600
_cell_volume                     1379.94(7)
_computing_cell_refinement       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5-ac5-018 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-018 (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      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.955
_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      0.00  29.00   0.50    0.13    --   12.00  27.00 169.06   58
  2  \w     -9.00  18.00   0.50    0.13    --    4.00  34.00-163.01   54
  3  \w     -9.00  18.00   0.50    0.13    --    4.00  34.00 -87.77   54
  4  \w     -9.00  20.00   0.50    0.13    --    4.00  33.00 -53.89   58
  5  \w     -9.00  20.00   0.50    0.13    --    4.00  33.00 -23.66   58
  6  \w      0.00  29.00   0.50    0.13    --   12.00  27.00   2.98   58
  7  \w    -40.00  14.00   0.50    0.13    --  -47.71  38.00-120.00  108
  8  \w    -62.00 -32.00   0.50    0.51    -- -104.50  57.00-120.00   60
  9  \w    -62.00 -32.00   0.50    0.51    -- -104.50  57.00 -30.00   60
 10  \w    -62.00 -32.00   0.50    0.51    -- -104.50  57.00   0.00   60
 11  \w   -104.00 -21.00   0.50    0.13    --  -47.71 140.00 -58.00  166
 12  \w    -98.00 -16.00   0.50    0.13    --  -47.71 130.00 128.00  164
 13  \w   -115.00 -32.00   0.50    0.51    -- -104.50 130.00 128.00  166
 14  \w   -123.00 -32.00   0.50    0.51    -- -104.50 140.00 -58.00  182
 15  \w   -107.00 -32.00   0.50    0.51    -- -104.50 104.00-138.63  150
 16  \w    -21.00   5.00   0.50    0.13    --   -8.00 -32.00-169.53   52
 17  \w    -45.00 -19.00   0.50    0.13    --  -32.00 -21.00-165.77   52
 18  \w    -29.00  -3.00   0.50    0.13    --  -16.00 -27.00 -48.35   52
 19  \w    -70.00 -34.00   0.50    0.13    --  -47.71 -17.00 -15.13   72
 20  \w    -60.00 -31.00   0.50    0.13    --  -44.00 -18.00 -38.82   58
 21  \w   -122.00 -34.00   0.50    0.13    --  -47.71 -16.00 -63.74  176
 22  \w   -122.00 -34.00   0.50    0.13    --  -47.71 -16.00  52.34  176
 23  \w    -54.00 -27.00   0.50    0.13    --  -40.00 -19.00  79.75   54
 24  \w    -69.00 -23.00   0.50    0.13    --  -36.00 -17.00 160.79   92
 25  \w    -69.00 -27.00   0.50    0.13    --  -40.00 -17.00 153.95   84
 26  \w   -122.00 -34.00   0.50    0.13    --  -47.71 -15.00  98.64  176
 27  \w   -122.00 -34.00   0.50    0.13    --  -47.71 -16.00-127.42  176
 28  \w   -166.00 -77.00   0.50    0.51    --  -92.00 -12.00 -92.07  178
 29  \w   -174.00-100.00   0.50    0.51    -- -104.50 -17.00-164.79  148
 30  \w   -142.00 -55.00   0.50    0.13    --  -68.00 -17.00-125.98  174
 31  \w   -142.00 -85.00   0.50    0.13    --  -68.00 -17.00-147.53  114
 32  \w   -139.00 -51.00   0.50    0.13    --  -64.00 -17.00  37.99  176
 33  \w   -139.00 -51.00   0.50    0.13    --  -64.00 -17.00  70.40  176
 34  \w   -139.00 -51.00   0.50    0.13    --  -64.00 -17.00 158.62  176
 35  \w   -139.00 -51.00   0.50    0.13    --  -64.00 -17.00 141.05  176
 36  \w   -170.00 -82.00   0.50    0.51    --  -96.00 -16.00 171.26  176
 37  \w   -170.00 -82.00   0.50    0.51    --  -96.00 -16.00 132.47  176
 38  \w   -174.00 -91.00   0.50    0.51    -- -104.50 -16.00  71.81  166
 39  \w   -174.00 -91.00   0.50    0.51    -- -104.50 -16.00  91.08  166
 40  \w   -166.00 -78.00   0.50    0.51    --  -92.00 -16.00  29.37  176
 41  \w   -166.00 -78.00   0.50    0.51    --  -92.00 -16.00 112.98  176
 42  \w   -174.00 -91.00   0.50    0.51    -- -104.50 -16.00 -48.85  166
 43  \w   -159.00 -70.00   0.50    0.51    --  -84.00 -15.00  -3.77  178
 44  \w   -174.00 -91.00   0.50    0.51    -- -104.50 -15.00  -7.81  166
 45  \w   -167.00 -78.00   0.50    0.51    --  -92.00 -15.00 -51.03  178
 46  \w   -174.00 -90.00   0.50    0.51    -- -104.50 -14.00 -91.59  168
 47  \w   -166.00 -78.00   0.50    0.51    --  -92.00 -16.00-128.33  176
 48  \w   -174.00 -91.00   0.50    0.51    -- -104.50 -16.00-132.13  166
 49  \w   -174.00-117.00   0.50    0.51    -- -104.50-125.00-180.00  114
 50  \w   -119.00 -64.00   0.50    0.13    --  -47.71-140.00-117.00  110
 51  \w   -173.00 -64.00   0.50    0.51    -- -104.50-140.00-117.00  218
 52  \w   -174.00-117.00   0.50    0.51    -- -104.50-125.00   0.00  114
 53  \w   -174.00 -71.00   0.50    0.51    -- -104.50-130.00  56.00  206
 54  \w   -119.00 -71.00   0.50    0.13    --  -47.71-130.00  56.00   96
 55  \w     36.00 106.00   0.50    0.51    --  108.35 -99.00  90.00  140
 56  \w     36.00 106.00   0.50    0.51    --  108.35 -99.00  60.00  140
 57  \w     36.00 116.00   0.50    0.51    --  108.35-130.00  56.00  160
 58  \w     28.00 104.00   0.50    0.13    --   47.71-140.00-117.00  152
 59  \w     36.00 123.00   0.50    0.51    --  108.35-140.00-117.00  174
 60  \w     22.00  98.00   0.50    0.13    --   47.71-130.00  56.00  152
 61  \w     36.00  69.00   0.50    0.51    --  108.35 -57.00  60.00   66
 62  \w     36.00  69.00   0.50    0.51    --  108.35 -57.00  90.00   66
 63  \w     36.00  69.00   0.50    0.51    --  108.35 -57.00 -60.00   66
 64  \w     36.00  69.00   0.50    0.51    --  108.35 -57.00-150.00   66
 65  \w    -27.00  30.00   0.50    0.13    --   47.71 -19.00 -90.00  114
 66  \w     70.00 120.00   0.50    0.13    --   47.71 140.00 -58.00  100
 67  \w    138.00 178.00   0.50    0.51    --  108.35  77.00-180.00   80
 68  \w    138.00 178.00   0.50    0.51    --  108.35  77.00 -90.00   80
 69  \w     70.00 173.00   0.50    0.51    --  108.35 140.00 -58.00  206
 70  \w    117.00 178.00   0.50    0.51    --  108.35 125.00  30.00  122
 71  \w     77.00 178.00   0.50    0.51    --  108.35 130.00 128.00  202
;
_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      0.1573661000
_diffrn_orient_matrix_UB_12      -0.0188820000
_diffrn_orient_matrix_UB_13      -0.0050762000
_diffrn_orient_matrix_UB_21      0.0124470000
_diffrn_orient_matrix_UB_22      -0.0609532000
_diffrn_orient_matrix_UB_23      0.1208911000
_diffrn_orient_matrix_UB_31      0.0185752000
_diffrn_orient_matrix_UB_32      -0.1391971000
_diffrn_orient_matrix_UB_33      -0.0043628000
_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  0.0439
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            43727
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.606
_diffrn_reflns_theta_min         3.474
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.519
_exptl_absorpt_correction_T_max  0.819
_exptl_absorpt_correction_T_min  0.672
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.119a (Rigaku Oxford Diffraction, 2021)
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 light white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_description       block
_exptl_crystal_F_000             686
_exptl_crystal_size_max          0.047
_exptl_crystal_size_mid          0.038
_exptl_crystal_size_min          0.027
_refine_diff_density_max         0.535
_refine_diff_density_min         -0.600
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       0.00051(8)
_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   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         5615
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0264
_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^)+(0.0317P)^2^+1.7666P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0651
_refine_ls_wR_factor_ref         0.0660
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5301
_reflns_number_total             5615
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00039g1.cif
_cod_data_source_block           msu4_chiral_autored
_cod_depositor_comments
'Adding full bibliography for 7246262--7246263.cif.'
_cod_database_code               7246263
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C47  H61  La2  N10  O18  '
_chemical_oxdiff_usercomment     'no friedels eq'
_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.a Aromatic/amide H refined with riding coordinates:
 C19(H19), C4(H4), C21(H21), C12(H12), C22(H22), C14(H14), C6(H6), C15(H15),
 C7(H7), C32(H32), C37(H37)
2.b Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C), C40(H40A,H40B,H40C), C39(H39A,H39B,H39C), C34(H34A,H34B,
 H34C)
;
_shelx_res_checksum              15058
_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 1.310
_oxdiff_exptl_absorpt_empirical_full_min 0.706