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_1570578
_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 Ce K Si4, 0.5(C4 H10 O)'
_chemical_formula_sum            'C54 H101 Ce K O0.5 Si4'
_chemical_formula_weight         1049.92
_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     iterative
_audit_creation_date             2022-05-30
_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                 102.374(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.4286(5)
_cell_length_b                   15.4560(2)
_cell_length_c                   18.8223(4)
_cell_measurement_reflns_used    88471
_cell_measurement_temperature    150
_cell_measurement_theta_max      29.59
_cell_measurement_theta_min      1.64
_cell_volume                     6089.1(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
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.84, Darmstadt 2018
;
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 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 0.996
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
 318 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  0.0373
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            88420
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.541
_diffrn_reflns_theta_min         1.638
_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    0.926
_exptl_absorpt_correction_T_max  0.5591
_exptl_absorpt_correction_T_min  0.3735
_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            'dark green'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.145
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2248
_exptl_crystal_size_max          0.565
_exptl_crystal_size_mid          0.394
_exptl_crystal_size_min          0.234
_refine_diff_density_max         0.951
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     594
_refine_ls_number_reflns         16911
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0318
_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^)+(0.0479P)^2^+3.4460P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0806
_refine_ls_wR_factor_ref         0.0894
_reflns_d_resolution_high        0.721
_reflns_d_resolution_low         12.434
_reflns_Friedel_coverage         0.000
_reflns_limit_h_max              26
_reflns_limit_h_min              -25
_reflns_limit_k_max              21
_reflns_limit_k_min              -21
_reflns_limit_l_max              25
_reflns_limit_l_min              -29
_reflns_number_gt                13243
_reflns_number_total             16911
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc03746k2.cif
_cod_data_source_block           ah141zkzk-2
_cod_depositor_comments
'Adding full bibliography for 1570572--1570581.cif.'
_cod_original_formula_sum        'C54 H101 Ce K O0.50 Si4'
_cod_database_code               1570578
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: O1(0.5) C53(0.5) H53A(0.5) H53B(0.5) C55(0.5) H55A(0.5) H55B(0.5)
 C56(0.5) H56A(0.5) H56B(0.5) H56C(0.5) C54(0.5) H54A(0.5) H54B(0.5) H54C(0.5)
3.a Ternary CH refined with riding coordinates:
 C29(H29), C32(H32), C23(H23), C44(H44), C50(H50), C41(H41), C17(H17),
 C38(H38), C35(H35), C26(H26), C20(H20), C47(H47)
3.b Secondary CH2 refined with riding coordinates:
 C53(H53A,H53B), C55(H55A,H55B)
3.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C5(H5), C4(H4), C11(H11), C2(H2), C7(H7), C16(H16),
 C10(H10), C8(H8), C3(H3), C15(H15)
3.d Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C52(H52A,H52B,H52C), C31(H31A,H31B,H31C), C30(H30A,H30B,
 H30C), C37(H37A,H37B,H37C), C43(H43A,H43B,H43C), C28(H28A,H28B,H28C), C51(H51A,
 H51B,H51C), C21(H21A,H21B,H21C), C33(H33A,H33B,H33C), C18(H18A,H18B,H18C),
 C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C45(H45A,H45B,H45C), C22(H22A,H22B,
 H22C), C27(H27A,H27B,H27C), C39(H39A,H39B,H39C), C46(H46A,H46B,H46C), C19(H19A,
 H19B,H19C), C42(H42A,H42B,H42C), C48(H48A,H48B,H48C), C40(H40A,H40B,H40C),
 C36(H36A,H36B,H36C), C49(H49A,H49B,H49C), C56(H56A,H56B,H56C), C54(H54A,H54B,
 H54C)
;
_shelx_res_checksum              13551
_shelx_hkl_checksum              83362
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holdern in mineral oil'
_olex2_submission_special_instructions 'No special instructions were received'