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_7130291
_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         'C48 H80 Ge2 K2 La2 O2 Si4, C8 H16 O2'
_chemical_formula_sum            'C56 H96 Ge2 K2 La2 O4 Si4'
_chemical_formula_weight         1446.88
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
;
2022-05-17 deposited with the CCDC.	2022-06-17 downloaded from the CCDC.
;
_cell_angle_alpha                108.346(4)
_cell_angle_beta                 103.835(4)
_cell_angle_gamma                94.719(4)
_cell_formula_units_Z            1
_cell_length_a                   9.8748(4)
_cell_length_b                   13.1071(7)
_cell_length_c                   13.4761(7)
_cell_measurement_reflns_used    29836
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.31
_cell_measurement_theta_min      2.16
_cell_volume                     1583.87(15)
_computing_cell_refinement
;
X-Area Recipe 1.34.0.0 (STOE, 2019)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.154.0 (STOE, 2019)
;
_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      100
_diffrn_detector                 Pilatus200K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.803
_diffrn_measurement_details
;
 493 frames, detector distance = 40 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_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  0.0427
_diffrn_reflns_av_unetI/netI     0.0515
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.803
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17504
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.803
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.426
_diffrn_reflns_theta_min         2.323
_diffrn_source                   'Mo Genix 3D HF'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    2.509
_exptl_absorpt_correction_T_max  0.6083
_exptl_absorpt_correction_T_min  0.2575
_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            'dark orange'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.327
_refine_diff_density_min         -2.018
_refine_diff_density_rms         0.186
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         8411
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0516
_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^)+(0.0978P)^2^+0.5262P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1378
_refine_ls_wR_factor_ref         0.1439
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6980
_reflns_number_total             8411
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc02810g2.cif
_cod_data_source_block           lmmxf206
_cod_original_cell_volume        1583.87(14)
_cod_database_code               7130291
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.634
_shelx_estimated_absorpt_t_min   0.520
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C27A \\sim C28A \\sim O2A \\sim C25A \\sim C26A: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
C25B \\sim C26B \\sim C27B \\sim C28B \\sim O2B: within 2A with sigma of 0.001
and sigma for terminal atoms of 0.002 within 2A
3. Others
 Fixed Sof: H21C(0.5) H21D(0.5) H21A(0.5) H21B(0.5) H23C(0.5) H23D(0.5)
 H23A(0.5) H23B(0.5) C22B(0.5) H22A(0.5) H22B(0.5) C22(0.5) H22C(0.5) H22D(0.5)
 C25B(0.5) H25A(0.5) H25B(0.5) C28B(0.5) H28A(0.5) H28B(0.5) C27B(0.5)
 H27A(0.5) H27B(0.5) C26B(0.5) H26A(0.5) H26B(0.5) O2A(0.5) C25A(0.5) H25C(0.5)
 H25D(0.5) C26A(0.5) H26C(0.5) H26D(0.5) C28A(0.5) H28C(0.5) H28D(0.5)
 C27A(0.5) H27C(0.5) H27D(0.5) O2B(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C21(H21C,H21D), C21(H21A,H21B), C23(H23C,H23D), C23(H23A,
 H23B), C22B(H22A,H22B), C22(H22C,H22D), C25B(H25A,H25B), C28B(H28A,H28B),
 C27B(H27A,H27B), C26B(H26A,H26B), C25A(H25C,H25D), C26A(H26C,H26D), C28A(H28C,
 H28D), C27A(H27C,H27D)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C8(H8), C6(H6), C2(H2), C3(H3), C7(H7), C5(H5), C4(H4)
4.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C13(H13A,H13B,H13C), C19(H19A,H19B,H19C), C14(H14A,H14B,
 H14C), C17(H17A,H17B,H17C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C15(H15A,
 H15B,H15C)
;
_shelx_res_checksum              2922
_shelx_hkl_checksum              48975
_olex2_submission_special_instructions 'No special instructions were received'