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_1570572
_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         'La, C52 H96 K Si4, 0.5(C7 H8)'
_chemical_formula_sum            'C59 H104 K La Si4'
_chemical_formula_weight         1103.79
_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_Hall           'C 2c 2'
_space_group_name_H-M_alt        'C 2 2 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-09-30
_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            8
_cell_length_a                   18.1753(3)
_cell_length_b                   22.3961(3)
_cell_length_c                   29.9843(6)
_cell_measurement_reflns_used    57459
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.18
_cell_measurement_theta_min      1.36
_cell_volume                     12205.3(4)
_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
;
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 1.88, Darmstadt 2019
;
_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
;
 258 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  0.0426
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            55243
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.737
_diffrn_reflns_theta_min         1.358
_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    0.880
_exptl_absorpt_correction_T_max  0.7637
_exptl_absorpt_correction_T_min  0.5536
_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    1.201
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4720
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.293
_refine_diff_density_max         2.018
_refine_diff_density_min         -0.609
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details
;
 Flack x determined using 4515 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.026(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     812
_refine_ls_number_reflns         12895
_refine_ls_number_restraints     186
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0428
_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^)+(0.0793P)^2^+3.8785P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1151
_refine_ls_wR_factor_ref         0.1184
_reflns_Friedel_coverage         0.854
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                11014
_reflns_number_total             12895
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc03746k2.cif
_cod_data_source_block           lmm188_ph04
_cod_depositor_comments
'Adding full bibliography for 1570572--1570581.cif.'
_cod_database_code               1570572
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.782
_shelx_estimated_absorpt_t_min   0.638
_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. Rigid bond restraints
 C39B, C39A, C38, C40B, C40A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C39B \\sim C39A \\sim C38 \\sim C40B \\sim C40A: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
C34A \\sim C32A \\sim C33A \\sim Si2B: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
C51A \\sim C50B \\sim C52B \\sim Si4B: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
C28A \\sim C26A \\sim C27A \\sim Si2B: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
C51B \\sim C50A \\sim C52A \\sim Si4A: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
Si4A \\sim C12: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
Si4B \\sim C12: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
Si2A \\sim C4: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
Si2B \\sim C4: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C46B \\sim C44B \\sim C45B: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
C54 \\sim C53: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C54 \\sim C59 \\sim C58 \\sim C57 \\sim C56 \\sim C55: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
4. Others
 Fixed Sof: H38A(0.5) H38(0.5) C39A(0.5) H39A(0.5) H39B(0.5) H39C(0.5)
 C40A(0.5) H40A(0.5) H40B(0.5) H40C(0.5) C40B(0.5) H40D(0.5) H40E(0.5)
 H40F(0.5) C39B(0.5) H39D(0.5) H39E(0.5) H39F(0.5) Si4A(0.5) Si4B(0.5)
 C50B(0.5) H50B(0.5) C51A(0.5) H51A(0.5) H51B(0.5) H51C(0.5) C47B(0.5)
 H47B(0.5) C52B(0.5) H52A(0.5) H52B(0.5) H52C(0.5) C46B(0.5) H46A(0.5)
 H46B(0.5) H46C(0.5) C49B(0.5) H49A(0.5) H49B(0.5) H49C(0.5) C44B(0.5)
 H44B(0.5) C49A(0.5) H49D(0.5) H49E(0.5) H49F(0.5) C48B(0.5) H48A(0.5)
 H48B(0.5) H48C(0.5) C48A(0.5) H48D(0.5) H48E(0.5) H48F(0.5) C47A(0.5)
 H47A(0.5) C45B(0.5) H45A(0.5) H45B(0.5) H45C(0.5) C44A(0.5) H44A(0.5)
 C46A(0.5) H46D(0.5) H46E(0.5) H46F(0.5) C45A(0.5) H45D(0.5) H45E(0.5)
 H45F(0.5) C50A(0.5) H50A(0.5) C51B(0.5) H51D(0.5) H51E(0.5) H51F(0.5)
 C52A(0.5) H52D(0.5) H52E(0.5) H52F(0.5) Si2B(0.4) Si2A(0.6) C28B(0.6)
 H28A(0.6) H28B(0.6) H28C(0.6) C30B(0.6) H30A(0.6) H30B(0.6) H30C(0.6)
 C26B(0.6) H26B(0.6) C34B(0.6) H34A(0.6) H34B(0.6) H34C(0.6) C27B(0.6)
 H27A(0.6) H27B(0.6) H27C(0.6) C33B(0.6) H33A(0.6) H33B(0.6) H33C(0.6)
 C32B(0.6) H32B(0.6) C29B(0.6) H29B(0.6) C31B(0.6) H31A(0.6) H31B(0.6)
 H31C(0.6) C32A(0.4) H32A(0.4) C33A(0.4) H33D(0.4) H33E(0.4) H33F(0.4)
 C34A(0.4) H34D(0.4) H34E(0.4) H34F(0.4) C29A(0.4) H29A(0.4) C31A(0.4)
 H31D(0.4) H31E(0.4) H31F(0.4) C30A(0.4) H30D(0.4) H30E(0.4) H30F(0.4)
 C26A(0.4) H26A(0.4) C27A(0.4) H27D(0.4) H27E(0.4) H27F(0.4) C28A(0.4)
 H28D(0.4) H28E(0.4) H28F(0.4) C57(0.5) H57(0.5) C58(0.5) H58(0.5) C59(0.5)
 H59(0.5) C54(0.5) C55(0.5) H55(0.5) C56(0.5) H56(0.5) C53(0.5) H53A(0.5)
 H53B(0.5) H53C(0.5)
5.a Ternary CH refined with riding coordinates:
 C20(H20), C17(H17), C23(H23), C38(H38A), C38(H38), C35(H35), C41(H41),
 C50B(H50B), C47B(H47B), C44B(H44B), C47A(H47A), C44A(H44A), C50A(H50A),
 C26B(H26B), C32B(H32B), C29B(H29B), C32A(H32A), C29A(H29A), C26A(H26A)
5.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C10(H10), C6(H6), C8(H8), C3(H3), C11(H11), C16(H16), C2(H2),
 C13(H13), C14(H14), C5(H5), C15(H15), C57(H57), C58(H58), C59(H59), C55(H55),
 C56(H56)
5.c Fitted hexagon refined as free rotating group:
 C57(C58,C59,C54,C55,C56)
5.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C24(H24A,H24B,H24C), C18(H18A,H18B,H18C), C22(H22A,H22B,
 H22C), C43(H43A,H43B,H43C), C36(H36A,H36B,H36C), C19(H19A,H19B,H19C), C42(H42A,
 H42B,H42C), C37(H37A,H37B,H37C), C25(H25A,H25B,H25C), C39A(H39A,H39B,H39C),
 C40A(H40A,H40B,H40C), C40B(H40D,H40E,H40F), C39B(H39D,H39E,H39F), C51A(H51A,
 H51B,H51C), C52B(H52A,H52B,H52C), C46B(H46A,H46B,H46C), C49B(H49A,H49B,H49C),
 C49A(H49D,H49E,H49F), C48B(H48A,H48B,H48C), C48A(H48D,H48E,H48F), C45B(H45A,
 H45B,H45C), C46A(H46D,H46E,H46F), C45A(H45D,H45E,H45F), C51B(H51D,H51E,H51F),
 C52A(H52D,H52E,H52F), C28B(H28A,H28B,H28C), C30B(H30A,H30B,H30C), C34B(H34A,
 H34B,H34C), C27B(H27A,H27B,H27C), C33B(H33A,H33B,H33C), C31B(H31A,H31B,H31C),
 C33A(H33D,H33E,H33F), C34A(H34D,H34E,H34F), C31A(H31D,H31E,H31F), C30A(H30D,
 H30E,H30F), C27A(H27D,H27E,H27F), C28A(H28D,H28E,H28F), C53(H53A,H53B,H53C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              62225
_shelx_hkl_checksum              63803
_shelx_fab_checksum              98746
_olex2_submission_special_instructions 'No special instructions were received'