Silole and germole complexes of lanthanum and cerium
Sun, Xiaofei; Münzfeld, Luca; Jin, Da; Hauser, Adrian; Roesky, Peter W.; Chemical Communications  (2022) –; doi:10.1039/D2CC02810G

data_7130289
_publ_section_title
;
 Silole and germole complexes of lanthanum and cerium
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC02810G
_journal_year                    2022
_chemical_formula_moiety         'C42 H60 K La O3 Si3, 1.5(C4 H8 O)'
_chemical_formula_sum            'C48 H72 K La O4.5 Si3'
_chemical_formula_weight         983.33
_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             2021-10-01
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6405)
;
_audit_update_record
;
2022-05-17 deposited with the CCDC.	2022-06-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.727(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.4366(9)
_cell_length_b                   21.1309(11)
_cell_length_c                   15.9329(9)
_cell_measurement_reflns_used    50007
_cell_measurement_temperature    150
_cell_measurement_theta_max      29.63
_cell_measurement_theta_min      1.65
_cell_volume                     4950.4(5)
_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 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
 193 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  0.0180
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            36418
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.509
_diffrn_reflns_theta_min         1.652
_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    1.060
_exptl_absorpt_correction_T_max  0.4227
_exptl_absorpt_correction_T_min  0.2810
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.73
_exptl_crystal_size_mid          0.571
_exptl_crystal_size_min          0.466
_refine_diff_density_max         1.157
_refine_diff_density_min         -0.650
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     592
_refine_ls_number_reflns         13702
_refine_ls_number_restraints     184
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0305
_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^)+(0.0431P)^2^+3.1039P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0767
_refine_ls_wR_factor_ref         0.0809
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11376
_reflns_number_total             13702
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc02810g2.cif
_cod_data_source_block           lmmxf304a
_cod_original_formula_sum        'C48 H72 K La O4.50 Si3'
_cod_database_code               7130289
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.638
_shelx_estimated_absorpt_t_min   0.512
_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. Restrained distances
 C39A-C40A = C41A-C42A
 1.53 with sigma of 0.02
 C39B-C40B = C41B-C42B
 1.53 with sigma of 0.02
 C40A-C41A
 1.54 with sigma of 0.02
 O3B-C39B = O3B-C42B
 1.44 with sigma of 0.02
 O3A-C39A = O3A-C42A
 1.44 with sigma of 0.02
 C40B-C41B
 1.54 with sigma of 0.02
 O1-C31 = O1-C34
 1.44 with sigma of 0.02
 O3B-C40B = O3B-C41B = C39B-C41B = C40B-C42B
 2.38 with sigma of 0.04
 O3A-C40A = O3A-C41A = C39A-C41A = C40A-C42A
 2.38 with sigma of 0.04
 O3B-C39B \\sim O3B-C42B
 with sigma of 0.02
 C48-C47 \\sim C49-C50
 with sigma of 0.02
 C40B-C42B \\sim C39B-C41B
 with sigma of 0.04
 C39B-C40B \\sim C40B-C41B \\sim C41B-C42B
 with sigma of 0.02
 C39A-C40A \\sim C40A-C41A \\sim C41A-C42A
 with sigma of 0.02
 C40A-C42A \\sim C39A-C41A
 with sigma of 0.04
 O3A-C39A \\sim O3A-C42A
 with sigma of 0.02
 O3A-C40A \\sim O3A-C41A
 with sigma of 0.04
 O3B-C40B \\sim O3B-C41B
 with sigma of 0.04
 O1-C31 \\sim O1-C34
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C50 \\sim O5 \\sim C47 \\sim C48 \\sim C49: within 2A with sigma of 0.1 and
sigma for terminal atoms of 0.2 within 2A
C50 \\sim C49 \\sim O5 \\sim C47 \\sim C48: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
O3A \\sim C39A \\sim C40A \\sim C41A \\sim C42A: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
Uanis(C39B) \\sim Ueq, Uanis(O3B) \\sim Ueq, Uanis(C40B) \\sim Ueq, Uanis(C41B)
\\sim Ueq, Uanis(C42B) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
4. Rigid body (RIGU) restrains
 O3B, C39B, C40B, C41B, C42B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O3A, C39A, C40A, C41A, C42A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C50(0.5) H50A(0.5) H50B(0.5) O5(0.5) C49(0.5) H49A(0.5) H49B(0.5)
 C47(0.5) H47A(0.5) H47B(0.5) C48(0.5) H48A(0.5) H48B(0.5) O3A(0.5) C39A(0.5)
 H39A(0.5) H39B(0.5) C40A(0.5) H40A(0.5) H40B(0.5) C41A(0.5) H41A(0.5)
 H41B(0.5) C42A(0.5) H42A(0.5) H42B(0.5) O3B(0.5) C39B(0.5) H39C(0.5) H39D(0.5)
 C40B(0.5) H40C(0.5) H40D(0.5) C41B(0.5) H41C(0.5) H41D(0.5) C42B(0.5)
 H42C(0.5) H42D(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C35(H35A,H35B), C36(H36A,H36B), C46(H46A,H46B), C45(H45A,H45B), C43(H43A,
 H43B), C44(H44A,H44B), C38(H38A,H38B), C37(H37A,H37B), C50(H50A,H50B),
 C49(H49A,H49B), C47(H47A,H47B), C48(H48A,H48B), C39A(H39A,H39B), C40A(H40A,
 H40B), C41A(H41A,H41B), C42A(H42A,H42B), C39B(H39C,H39D), C40B(H40C,H40D),
 C41B(H41C,H41D), C42B(H42C,H42D), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,
 H33B), C34(H34A,H34B)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C26(H26), C7(H7), C6(H6), C8(H8), C3(H3), C5(H5), C30(H30), C20(H20),
 C4(H4), C21(H21), C24(H24), C28(H28), C1(H1), C27(H27), C23(H23), C29(H29),
 C22(H22)
6.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C15(H15A,H15B,H15C), C14(H14A,H14B,H14C), C16(H16A,H16B,
 H16C), C13(H13A,H13B,H13C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              23763
_shelx_hkl_checksum              76253
_olex2_submission_special_instructions 'No special instructions were received'