Metal ion-driven formation of 2<i>H</i>-silolides and -germolides.
Liu, Chenghuan; Schmidtmann, Marc; Müller, Thomas; Chemical communications (Cambridge, England) 60 (2024) 11295–11298; doi:10.1039/d4cc03984j

data_7133649
_publ_section_title
;
 Metal ion-driven formation of 2<i>H</i>-silolides and -germolides.
;
_journal_issue                   80
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              11295
_journal_page_last               11298
_journal_paper_doi               10.1039/d4cc03984j
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C49 H75 K N2 O6 Si4 Te2'
_chemical_formula_sum            'C49 H75 K N2 O6 Si4 Te2'
_chemical_formula_weight         1194.798
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_Int_Tables_number      14
_audit_creation_date             2022-12-06
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-07-05 deposited with the CCDC.	2024-08-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.4752(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.6369(8)
_cell_length_b                   11.8608(4)
_cell_length_c                   22.6135(9)
_cell_measurement_reflns_used    9984
_cell_measurement_temperature    100
_cell_measurement_theta_max      34.851
_cell_measurement_theta_min      2.272
_cell_volume                     5643.6(4)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.9999
_diffrn_measured_fraction_theta_max 1.0000
_diffrn_measurement_device_type  'Bruker Photon III CPAD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_unetI/netI     0.0151
_diffrn_reflns_Laue_measured_fraction_full 0.9999
_diffrn_reflns_Laue_measured_fraction_max 1.0000
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            387403
_diffrn_reflns_point_group_measured_fraction_full 0.9999
_diffrn_reflns_point_group_measured_fraction_max 1.0000
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         34.97
_diffrn_reflns_theta_min         1.85
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.237
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9400
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0593 before and 0.0507 after correction.
The Ratio of minimum to maximum transmission is 0.9400.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_description       block
_exptl_crystal_F_000             2440.083
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.1031
_refine_diff_density_min         -0.8536
_refine_diff_density_rms         0.0882
_refine_ls_d_res_high            0.6200
_refine_ls_d_res_low             10.9955
_refine_ls_goodness_of_fit_ref   1.0480
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    162
_refine_ls_number_parameters     774
_refine_ls_number_reflns         24788
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.0473
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0287
_refine_ls_shift/su_max          0.0010
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0206P)^2^+4.5262P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0620
_refine_ls_wR_factor_ref         0.0643
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              33
_reflns_limit_h_min              -34
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              36
_reflns_limit_l_min              0
_reflns_number_gt                22517
_reflns_number_total             24788
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4cc03984j3.cif
_cod_data_source_block           lch1117te
_cod_depositor_comments
'Adding full bibliography for 7133645--7133649.cif.'
_cod_database_code               7133649
_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 body (RIGU) restrains
 O1C, O2C, O3C, C38C, C39C, C40C, C41C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Fixed Sof: O4(0.85) O5(0.85) O21(0.85) C42(0.85) H42a(0.85) H42b(0.85)
 C43(0.85) H43a(0.85) H43b(0.85) C44(0.85) H44a(0.85) H44b(0.85) C45(0.85)
 H45a(0.85) H45b(0.85) C46(0.85) H46a(0.85) H46b(0.85) C47(0.85) H47a(0.85)
 H47b(0.85) C48(0.85) H48a(0.85) H48b(0.85) C49(0.85) H49a(0.85) H49b(0.85)
 O1(0.55) O2(0.55) C38(0.55) H38a(0.55) H38b(0.55) C39(0.55) H39a(0.55)
 H39b(0.55) C40(0.55) H40a(0.55) H40b(0.55) C41(0.55) H41a(0.55) H41b(0.55)
 O3(0.55) O1B(0.15) O2B(0.15) O3B(0.15) O4B(0.15) O5B(0.15) O6B(0.15)
 C38B(0.15) H38c(0.15) H38d(0.15) C39B(0.15) H39c(0.15) H39d(0.15) C40B(0.15)
 H40c(0.15) H40d(0.15) C41B(0.15) H41c(0.15) H41d(0.15) C42B(0.15) H42c(0.15)
 H42d(0.15) C43B(0.15) H43c(0.15) H43d(0.15) C44B(0.15) H44c(0.15) H44d(0.15)
 C45B(0.15) H45c(0.15) H45d(0.15) C46B(0.15) H46c(0.15) H46d(0.15) C47B(0.15)
 H47c(0.15) H47d(0.15) C48B(0.15) H48c(0.15) H48d(0.15) C49B(0.15) H49c(0.15)
 H49d(0.15) O1C(0.3) O2C(0.3) O3C(0.3) C38C(0.3) H38e(0.3) H38f(0.3) C39C(0.3)
 H39e(0.3) H39f(0.3) C40C(0.3) H40e(0.3) H40f(0.3) C41C(0.3) H41e(0.3) H41f(0.3)
4.a Secondary CH2 refined with riding coordinates:
 C38(H38a,H38b), C39(H39a,H39b), C40(H40a,H40b), C41(H41a,H41b), C42(H42a,
 H42b), C43(H43a,H43b), C44(H44a,H44b), C45(H45a,H45b), C46(H46a,H46b),
 C47(H47a,H47b), C48(H48a,H48b), C49(H49a,H49b), C38B(H38c,H38d), C39B(H39c,
 H39d), C40B(H40c,H40d), C41B(H41c,H41d), C42B(H42c,H42d), C43B(H43c,H43d),
 C44B(H44c,H44d), C45B(H45c,H45d), C46B(H46c,H46d), C47B(H47c,H47d), C48B(H48c,
 H48d), C49B(H49c,H49d), C38C(H38e,H38f), C39C(H39e,H39f), C40C(H40e,H40f),
 C41C(H41e,H41f)
4.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29)
4.c Idealised Me refined as rotating group:
 C17(H17a,H17b,H17c), C18(H18a,H18b,H18c), C19(H19a,H19b,H19c), C20(H20a,H20b,
 H20c), C21(H21a,H21b,H21c), C22(H22a,H22b,H22c), C31(H31a,H31b,H31c), C32(H32a,
 H32b,H32c), C33(H33a,H33b,H33c), C35(H35a,H35b,H35c), C36(H36a,H36b,H36c),
 C37(H37a,H37b,H37c)
;
_olex2_submission_special_instructions 'No special instructions were received'