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_7130290
_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         'C40 H56 Ce2 Ge K2 O Si2, 0.75(C4 H8 O)'
_chemical_formula_sum            'C44 H64 Ce2 Ge K2 O2 Si2'
_chemical_formula_weight         1112.16
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 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                 96.258(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.9801(7)
_cell_length_b                   23.8817(16)
_cell_length_c                   31.570(3)
_cell_measurement_reflns_used    24575
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.21
_cell_measurement_theta_min      2.31
_cell_volume                     9728.0(13)
_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 0.977
_diffrn_measured_fraction_theta_max 0.802
_diffrn_measurement_details
;
 1014 frames, detector distance = 140 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  0.0220
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.802
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            25797
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.802
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.419
_diffrn_reflns_theta_min         2.313
_diffrn_source                   'Mo Genix 3D HF'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    2.707
_exptl_absorpt_correction_T_max  0.8022
_exptl_absorpt_correction_T_min  0.4924
_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    1.519
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4464
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.133
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.271
_refine_diff_density_min         -0.499
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     563
_refine_ls_number_reflns         9825
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0299
_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^)+(0.0458P)^2^+1.2612P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0730
_refine_ls_wR_factor_ref         0.0766
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8048
_reflns_number_total             9825
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc02810g2.cif
_cod_data_source_block           lmmxf248
_cod_original_cell_volume        9727.9(12)
_cod_database_code               7130290
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.877
_shelx_estimated_absorpt_t_min   0.614
_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
 C45B-C46B \\sim C46B-C47B \\sim C47B-C48B
 with sigma of 0.02
 O2-C44 \\sim O2-C41
 with sigma of 0.02
 C46B-C48B \\sim C45B-C47B
 with sigma of 0.04
 O3B-C45B \\sim O3B-C48B
 with sigma of 0.02
 O3A-C45A \\sim O3A-C48A
 with sigma of 0.01
 C47A-C48A \\sim C45A-C46A
 with sigma of 0.01
 O3B-C46B \\sim O3B-C47B
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
O2 \\sim C44 \\sim C42 \\sim C41: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
O3B \\sim C45B \\sim C46B \\sim C47B \\sim C48B: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
O3A \\sim C48A \\sim C47A \\sim C46A \\sim C45A: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
4. Rigid body (RIGU) restrains
 O2, C44, C42, C41
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O3B, C45B, C46B, C47B, C48B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: O2(0.5) C44(0.5) H44A(0.5) H44B(0.5) C42(0.5) H42A(0.5) H42B(0.5)
 C41(0.5) H41A(0.5) H41B(0.5) C43(0.5) H43A(0.5) H43B(0.5) C48A(0.3) H48A(0.3)
 H48B(0.3) C46A(0.3) H46A(0.3) H46B(0.3) O3A(0.3) C45A(0.3) H45A(0.3) H45B(0.3)
 C47A(0.3) H47A(0.3) H47B(0.3) O3B(0.2) C45B(0.2) H45C(0.2) H45D(0.2) C46B(0.2)
 H46C(0.2) H46D(0.2) C47B(0.2) H47C(0.2) H47D(0.2) C48B(0.2) H48C(0.2) H48D(0.2)
6.a Free rotating group:
 O2(C44,C42,C41), O3B(C45B,C46B,C47B,C48B)
6.b Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C40(H40A,H40B), C39(H39A,H39B), C38(H38A,H38B), C44(H44A,
 H44B), C42(H42A,H42B), C41(H41A,H41B), C43(H43A,H43B), C48A(H48A,H48B),
 C46A(H46A,H46B), C45A(H45A,H45B), C47A(H47A,H47B), C45B(H45C,H45D), C46B(H46C,
 H46D), C47B(H47C,H47D), C48B(H48C,H48D)
6.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C4(H4), C32(H32), C3(H3), C1(H1), C2(H2), C8(H8), C33(H33), C34(H34),
 C31(H31), C35(H35), C28(H28), C29(H29), C36(H36), C7(H7), C6(H6), C25(H25),
 C21(H21), C24(H24), C27(H27), C26(H26), C23(H23), C30(H30), C22(H22)
6.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C19(H19A,H19B,H19C), C15(H15A,H15B,H15C), C13(H13A,H13B,
 H13C), C16(H16A,H16B,H16C), C14(H14A,H14B,H14C), C17(H17A,H17B,H17C), C18(H18A,
 H18B,H18C)
;
_shelx_res_checksum              92757
_shelx_hkl_checksum              56292
_olex2_submission_special_instructions 'No special instructions were received'