Mononuclear organogermanium(IV) catalysts for a [3 + 2] cycloaddition reaction.
Basu, Debayan; Ghosh, Barshali; Srivastava, Diship; Patra, Niladri; Nayek, Hari Pada; Dalton transactions (Cambridge, England : 2003) 53 (2024) 5648–5657; doi:10.1039/d4dt00239c

data_7715198
_publ_section_title
;
 Mononuclear organogermanium(IV) catalysts for a [3 + 2] cycloaddition
 reaction.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5648
_journal_page_last               5657
_journal_paper_doi               10.1039/d4dt00239c
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C26 H20 Ge N2 O5'
_chemical_formula_sum            'C26 H20 Ge N2 O5'
_chemical_formula_weight         513.03
_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
_audit_creation_date             2023-08-14
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-01-25 deposited with the CCDC.	2024-02-20 downloaded from the CCDC.
;
_cell_angle_alpha                81.627(4)
_cell_angle_beta                 89.040(4)
_cell_angle_gamma                82.921(4)
_cell_formula_units_Z            4
_cell_length_a                   11.1870(5)
_cell_length_b                   12.4501(6)
_cell_length_c                   16.3530(8)
_cell_measurement_reflns_used    6161
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.8570
_cell_measurement_theta_min      2.6190
_cell_volume                     2236.18(19)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, EosS2'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_av_unetI/netI     0.0694
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19042
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.937
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.412
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_description       block
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.355
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.936
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     615
_refine_ls_number_reflns         9148
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.936
_refine_ls_R_factor_all          0.0830
_refine_ls_R_factor_gt           0.0418
_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^)+(0.0328P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0741
_refine_ls_wR_factor_ref         0.0825
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5916
_reflns_number_total             9148
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00239c2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7715197--7715198.cif.'
_cod_database_code               7715198
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C7(H7), C9(H9), C10(H10), C11(H11), C16(H16),
 C17(H17), C18(H18), C19(H19), C20(H20), C22(H22), C23(H23), C24(H24), C25(H25),
  C26(H26), C28(H28), C29(H29), C31(H31), C33(H33), C35(H35), C36(H36),
 C37(H37), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C48(H48), C49(H49),
  C50(H50), C51(H51), C52(H52)
1.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C40(H40A,H40B,H40C)
;
_shelx_res_checksum              32261
_olex2_submission_special_instructions 'No special instructions were received'