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_1570576
_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 Pr Si4'
_chemical_formula_sum            'C52 H96 K Pr Si4'
_chemical_formula_weight         1013.65
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-05-13
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-07-19 deposited with the CCDC.	2023-12-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.154(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.9574(4)
_cell_length_b                   17.5114(4)
_cell_length_c                   21.5769(5)
_cell_measurement_reflns_used    46500
_cell_measurement_temperature    150
_cell_measurement_theta_max      29.53
_cell_measurement_theta_min      1.57
_cell_volume                     5607.5(2)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area WinXpose 2.0.22.0 (STOE, 2016)
;
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
 246 frames, detector distance = 100 mm
;
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.5 mm diameter, multiple pinhole'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_unetI/netI     0.0511
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            60046
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.541
_diffrn_reflns_theta_min         1.569
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.000
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.059
_exptl_absorpt_correction_T_max  0.8811
_exptl_absorpt_correction_T_min  0.5137
_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            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2168
_exptl_crystal_size_max          0.241
_exptl_crystal_size_mid          0.192
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.731
_refine_diff_density_min         -0.532
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     558
_refine_ls_number_reflns         15602
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0743
_refine_ls_R_factor_gt           0.0393
_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^)+(0.0212P)^2^+7.9684P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0684
_refine_ls_wR_factor_ref         0.0792
_reflns_d_resolution_high        0.721
_reflns_d_resolution_low         12.977
_reflns_Friedel_coverage         0.000
_reflns_limit_h_max              20
_reflns_limit_h_min              -20
_reflns_limit_k_max              24
_reflns_limit_k_min              -24
_reflns_limit_l_max              25
_reflns_limit_l_min              -29
_reflns_number_gt                11333
_reflns_number_total             15602
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc03746k2.cif
_cod_data_source_block           ah146_toluol
_cod_depositor_comments
'Adding full bibliography for 1570572--1570581.cif.'
_cod_database_code               1570576
_shelx_shelxl_version_number     2018/3
_publ_section_exptl
;
Any special experimental details
;
_shelx_estimated_absorpt_t_max   0.849
_shelx_estimated_absorpt_t_min   0.784
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C47(H47), C41(H41), C23(H23), C32(H32), C17(H17), C26(H26), C20(H20),
 C44(H44), C50(H50), C35(H35), C38(H38), C29(H29)
1.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C14(H14), C7(H7), C13(H13), C8(H8), C4(H4), C3(H3), C11(H11),
 C15(H15), C16(H16), C10(H10), C2(H2)
1.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C52(H52A,H52B,H52C), C45(H45A,H45B,H45C), C28(H28A,H28B,
 H28C), C18(H18A,H18B,H18C), C42(H42A,H42B,H42C), C25(H25A,H25B,H25C), C46(H46A,
 H46B,H46C), C24(H24A,H24B,H24C), C34(H34A,H34B,H34C), C51(H51A,H51B,H51C),
 C49(H49A,H49B,H49C), C33(H33A,H33B,H33C), C36(H36A,H36B,H36C), C43(H43A,H43B,
 H43C), C31(H31A,H31B,H31C), C40(H40A,H40B,H40C), C22(H22A,H22B,H22C), C27(H27A,
 H27B,H27C), C39(H39A,H39B,H39C), C30(H30A,H30B,H30C), C21(H21A,H21B,H21C),
 C37(H37A,H37B,H37C)
;
_shelx_res_checksum              82574
_shelx_hkl_checksum              78602
_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'