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_1570577
_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_absolute_configuration unk
_chemical_formula_moiety         'C52 H96 Er K Si4, C7 H8'
_chemical_formula_sum            'C59 H104 Er K Si4'
_chemical_formula_weight         1132.14
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F -2d 2'
_space_group_name_H-M_alt        'F 2 d d'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-10-07
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6405)
;
_audit_update_record
;
2023-07-19 deposited with the CCDC.	2023-12-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   16.0025(3)
_cell_length_b                   32.4257(7)
_cell_length_c                   46.6302(7)
_cell_measurement_reflns_used    63041
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.14
_cell_measurement_theta_min      1.48
_cell_volume                     24196.1(8)
_computing_cell_refinement
;
X-Area Recipe 1.34.0.0 (STOE, 2019)
;
_computing_data_collection
;
X-Area WinXpose 2.0.22.0 (STOE, 2016)
;
_computing_data_reduction
;
X-Area Integrate 1.77.0.0 (STOE, 2019)
X-Area LANA 1.77.1.0 (STOE, 2019)
;
_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      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 0.996
_diffrn_measurement_details
;
 287 frames, detector distance = 120 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  0.0211
_diffrn_reflns_av_unetI/netI     0.0245
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -58
_diffrn_reflns_number            52731
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.734
_diffrn_reflns_theta_min         1.485
_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    1.569
_exptl_absorpt_correction_T_max  0.6959
_exptl_absorpt_correction_T_min  0.4541
_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, Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136-140.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             9616
_exptl_crystal_size_max          0.691
_exptl_crystal_size_mid          0.414
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.846
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.174(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     691
_refine_ls_number_reflns         12760
_refine_ls_number_restraints     116
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0282
_refine_ls_R_factor_gt           0.0239
_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^)+(0.0415P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0585
_refine_ls_wR_factor_ref         0.0592
_reflns_Friedel_coverage         0.922
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                11495
_reflns_number_total             12760
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc03746k2.cif
_cod_data_source_block           lmm181
_cod_depositor_comments
'Adding full bibliography for 1570572--1570581.cif.'
_cod_database_code               1570577
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.704
_shelx_estimated_absorpt_t_min   0.410
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.826(7)
 0.174(7)
2. 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
3. Restrained distances
 C43A-C45A \\sim C44A-C43A
 with sigma of 0.01
 C45B-C43B \\sim C43B-C44B
 with sigma of 0.01
 C48-C46 \\sim C47-C46
 with sigma of 0.01
 C18-C17 \\sim C19-C17
 with sigma of 0.02
4. Rigid bond restraints
 C45B, C43B, C44B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C62 \\sim C63 \\sim C61 \\sim C60 \\sim C65 \\sim C64: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
C59 \\sim C60: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C53 \\sim C58 \\sim C57 \\sim C56 \\sim C55 \\sim C54: within 2A with sigma of
0.001 and sigma for terminal atoms of 0.002 within 2A
C53 \\sim C52: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C17: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002 within
2A
C18 \\sim C17 \\sim C19: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C45A \\sim C43A \\sim C44A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
6. Others
 Fixed Sof: C44B(0.6) H44A(0.6) H44B(0.6) H44C(0.6) C43B(0.6) H43B(0.6)
 H43A(0.5) H43(0.5) C42B(0.5) H42A(0.5) H42B(0.5) H42C(0.5) C58(0.5) H58(0.5)
 C57(0.5) H57(0.5) C56(0.5) H56(0.5) C55(0.5) H55(0.5) C54(0.5) H54(0.5)
 C53(0.5) C42A(0.5) H42D(0.5) H42E(0.5) H42F(0.5) C62(0.5) H62(0.5) C63(0.5)
 H63(0.5) C64(0.5) H64(0.5) C65(0.5) H65(0.5) C60(0.5) C61(0.5) H61(0.5)
 C59(0.5) H59A(0.5) H59B(0.5) H59C(0.5) C45B(0.6) H45A(0.6) H45B(0.6) H45C(0.6)
 C52(0.5) H52A(0.5) H52B(0.5) H52C(0.5) C45A(0.4) H45D(0.4) H45E(0.4) H45F(0.4)
 C43A(0.4) H43C(0.4) C44A(0.4) H44D(0.4) H44E(0.4) H44F(0.4)
7.a Ternary CH refined with riding coordinates:
 C49(H49), C26(H26), C29(H29), C32(H32), C43B(H43B), C23(H23), C20(H20),
 C17(H17), C38(H38), C35(H35), C43(H43A), C43(H43), C43A(H43C), C46(H46)
7.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C16(H16), C15(H15), C4(H4), C14(H14), C7(H7), C5(H5), C11(H11),
 C10(H10), C2(H2), C3(H3), C8(H8), C58(H58), C57(H57), C56(H56), C55(H55),
 C54(H54), C62(H62), C63(H63), C64(H64), C65(H65), C61(H61)
7.c Fitted hexagon refined as free rotating group:
 C58(C57,C56,C55,C54,C53), C62(C63,C64,C65,C60,C61)
7.d Idealised Me refined as rotating group:
 C51(H51A,H51B,H51C), C50(H50A,H50B,H50C), C30(H30A,H30B,H30C), C31(H31A,H31B,
 H31C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C27(H27A,H27B,H27C), C28(H28A,
 H28B,H28C), C44B(H44A,H44B,H44C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C),
 C22(H22A,H22B,H22C), C21(H21A,H21B,H21C), C19(H19A,H19B,H19C), C18(H18A,H18B,
 H18C), C40(H40A,H40B,H40C), C39(H39A,H39B,H39C), C37(H37A,H37B,H37C), C36(H36A,
 H36B,H36C), C41(H41A,H41B,H41C), C42B(H42A,H42B,H42C), C42A(H42D,H42E,H42F),
 C59(H59A,H59B,H59C), C45B(H45A,H45B,H45C), C52(H52A,H52B,H52C), C45A(H45D,H45E,
 H45F), C44A(H44D,H44E,H44F), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C)
;
_shelx_res_checksum              31974
_shelx_hkl_checksum              78681
_olex2_submission_special_instructions 'No special instructions were received'