It's not just the size that matters: crystal engineering of lanthanide-based coordination polymers.
Hauser, Adrian; Münzfeld, Luca; Uhlmann, Cedric; Lebedkin, Sergei; Schlittenhardt, Sören; Ruan, Ting-Ting; Kappes, Manfred M.; Ruben, Mario; Roesky, Peter W.; Chemical science 15 (2024) 1338–1347; doi:10.1039/d3sc03746k

data_1570579
_publ_section_title
;
 It's not just the size that matters: crystal engineering of
 lanthanide-based coordination polymers.
;
_journal_issue                   4
_journal_name_full               'Chemical science'
_journal_page_first              1338
_journal_page_last               1347
_journal_paper_doi               10.1039/d3sc03746k
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C52 H96 K Lu Si4'
_chemical_formula_sum            'C52 H96 K Lu Si4'
_chemical_formula_weight         1047.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-10-10
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-11-22 deposited with the CCDC.	2023-12-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.330(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.843(2)
_cell_length_b                   17.3279(17)
_cell_length_c                   21.557(2)
_cell_measurement_reflns_used    24568
_cell_measurement_temperature    130
_cell_measurement_theta_max      29.50
_cell_measurement_theta_min      1.81
_cell_volume                     5499.1(11)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection       'X-Area Pilatus3_SV 1.31.150.0 (STOE, 2018)'
_computing_data_reduction
;
X-Area Integrate 1.73.1.0 (STOE, 2018)
X-Area LANA 1.73.2.0 (STOE, 2018)
;
_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    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      130
_diffrn_detector                 'EIGER2 1M CDTE'
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.805
_diffrn_measurement_details
;
 247 frames, detector distance = 40 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '1.2 0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_av_unetI/netI     0.1000
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.805
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            34000
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.805
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.188
_diffrn_reflns_theta_min         1.815
_diffrn_source                   Axo_Mo
_diffrn_source_current           0.830
_diffrn_source_power             0.050
_diffrn_source_voltage           60
_exptl_absorpt_coefficient_mu    1.989
_exptl_absorpt_correction_T_max  0.8199
_exptl_absorpt_correction_T_min  0.2522
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270.
Afterwards scaling of reflection intensities was performed within STOE LANA.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2216
_exptl_crystal_size_max          0.204
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.064
_refine_diff_density_max         0.661
_refine_diff_density_min         -0.937
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.885
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     547
_refine_ls_number_reflns         13139
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      0.885
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0327
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0223P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0555
_refine_ls_wR_factor_ref         0.0602
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8578
_reflns_number_total             13139
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc03746k2.cif
_cod_data_source_block           cu287
_cod_depositor_comments
'Adding full bibliography for 1570572--1570581.cif.'
_cod_original_cell_volume        5499.3(11)
_cod_database_code               1570579
_shelx_shelxl_version_number     2018/3
_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. Restrained distances
 C8-C1 \\sim C7-C8
 with sigma of 0.0001
3. Uiso/Uaniso restraints and constraints
C8 \\sim C1 \\sim C7: within 2A with sigma of 0.0001 and sigma for terminal
atoms of 0.0002 within 2A
4.a Ternary CH refined with riding coordinates:
 C29(H29), C20(H20), C17(H17), C44(H44), C26(H26), C32(H32), C50(H50),
 C47(H47), C23(H23), C35(H35), C41(H41), C38(H38)
4.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C2(H2), C15(H15), C6(H6), C13(H13), C10(H10), C11(H11), C14(H14),
 C8(H8), C3(H3), C5(H5), C7(H7)
4.c Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C52(H52A,H52B,H52C), C27(H27A,H27B,H27C), C30(H30A,H30B,
 H30C), C49(H49A,H49B,H49C), C19(H19A,H19B,H19C), C43(H43A,H43B,H43C), C48(H48A,
 H48B,H48C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C24(H24A,H24B,H24C),
 C37(H37A,H37B,H37C), C22(H22A,H22B,H22C), C18(H18A,H18B,H18C), C39(H39A,H39B,
 H39C), C51(H51A,H51B,H51C), C33(H33A,H33B,H33C), C46(H46A,H46B,H46C), C28(H28A,
 H28B,H28C), C25(H25A,H25B,H25C), C31(H31A,H31B,H31C), C45(H45A,H45B,H45C),
 C36(H36A,H36B,H36C), C21(H21A,H21B,H21C)
;
_shelx_res_checksum              24869
_shelx_hkl_checksum              47212
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in mineral oil'
_olex2_submission_special_instructions 'No special instructions were received'
_stoe_detector_distance          '40.0 mm'
_stoe_detector_pixelsize_x       '0.075 mm'
_stoe_detector_pixelsize_y       '0.075 mm'
_stoe_detector_size_x            '8.0 cm'
_stoe_detector_size_y            '7.7 cm'
_stoe_evaluation_integration_a   10.1
_stoe_evaluation_integration_b   -0.1
_stoe_evaluation_integration_ems 0.014
_stoe_evaluation_lana_bis_l_even_max -
_stoe_evaluation_lana_bis_l_odd_max -
_stoe_evaluation_lana_bos_l_even_max 4
_stoe_evaluation_lana_bos_l_odd_max 1
_stoe_evaluation_lana_completeness 80.3
_stoe_evaluation_lana_dxs_max_order 1
_stoe_evaluation_lana_dys_max_order 1
_stoe_evaluation_lana_fs_max_order 3
_stoe_evaluation_lana_max_2theta_available 60.4
_stoe_evaluation_lana_max_2theta_desired 60.4
_stoe_evaluation_lana_mean_redundancy 2.6
_stoe_evaluation_lana_number_refls_after_or 34030
_stoe_evaluation_lana_number_refls_outliers 3900
_stoe_evaluation_lana_number_refls_total 37930
_stoe_evaluation_lana_number_refls_unique 13142
_stoe_evaluation_lana_number_refls_written 34030
_stoe_evaluation_lana_or_c1      0.035
_stoe_evaluation_lana_or_c2      0
_stoe_evaluation_lana_or_c3      0
_stoe_evaluation_lana_or_c4      0.7
_stoe_evaluation_lana_point_group 2/m
_stoe_evaluation_lana_table
;
2Theta           6.4   12.8   19.2   25.6   32.0   38.4   44.8   51.2   57.6
<Resolution>    5.48   3.01   2.08   1.59   1.28   1.08   0.93   0.83   0.75
N(total)         199    958   2518   4522   7065   7852   7279   6044   1493
<Redundancy>     2.3    2.8    3.5    3.7    3.9    3.2    2.3    1.7    1.2
Complet. [%%]    97.2   98.5   99.7  100.0  100.0   99.6   98.7   92.3   29.1
<I/sigma>       63.8   32.4   24.9   14.7   10.9    7.8    4.5    2.8    1.7
R(int)         0.045  0.026  0.020  0.026  0.034  0.045  0.073  0.108  0.142
;
_stoe_measurement_identifier     CU287
_stoe_measurement_max_exposure_per_frame '10.0 s'
_stoe_measurement_mean_exposure_per_frame '10.0 s'
_stoe_measurement_min_exposure_per_frame '10.0 s'
_stoe_measurement_total_exposure_time '41 min'
_stoe_measurement_total_frame_number 247
_stoe_measurement_total_run_number 6
_stoe_measurement_tube_power     '49.8 W'