Air and water stable germacarbonyl compounds
Mahawar, Pritam; Shukla, Pratima; Chandra Joshi, Prakash; Singh, Dharmendra; Kumar, Hemant; Mukherjee, Goutam; Nagendran, Selvarajan; Chemical Science 13 (2022) 12382–12388; doi:10.1039/D2SC01869A

data_1567684
_publ_section_title
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 Air and water stable germacarbonyl compounds
;
_journal_issue                   42
_journal_name_full               'Chemical Science'
_journal_page_first              12382
_journal_page_last               12388
_journal_paper_doi               10.1039/D2SC01869A
_journal_volume                  13
_journal_year                    2022
_chemical_formula_moiety         'C35 H36 Ge N2 O S'
_chemical_formula_sum            'C35 H36 Ge N2 O S'
_chemical_formula_weight         605.33
_chemical_name_systematic        DPMGe(S)OEt
_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'
_symmetry_Int_Tables_number      14
_audit_creation_date             2021-10-10
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6396)
;
_audit_update_record
;
2021-10-21 deposited with the CCDC.	2022-09-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.287(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.9611(5)
_cell_length_b                   14.0451(5)
_cell_length_c                   15.5244(6)
_cell_measurement_reflns_used    9750
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      3.13
_cell_volume                     3114.79(19)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.9988
_diffrn_measured_fraction_theta_max 0.9977
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0612
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_Laue_measured_fraction_full 0.9988
_diffrn_reflns_Laue_measured_fraction_max 0.9977
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            89570
_diffrn_reflns_point_group_measured_fraction_full 0.9988
_diffrn_reflns_point_group_measured_fraction_max 0.9977
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         2.00
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.080
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6717
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0743 before and 0.0563 after correction.
The Ratio of minimum to maximum transmission is 0.9008.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_description       block
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.4519
_refine_diff_density_min         -0.4092
_refine_diff_density_rms         0.0921
_refine_ls_d_res_high            0.7497
_refine_ls_d_res_low             10.1953
_refine_ls_goodness_of_fit_ref   1.0217
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    57
_refine_ls_number_parameters     368
_refine_ls_number_reflns         7734
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0217
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.0009
_refine_ls_shift/su_mean         0.0002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0530P)^2^+0.5140P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0889
_refine_ls_wR_factor_ref         0.0942
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -19
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              -11
_reflns_number_gt                6223
_reflns_number_total             7734
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2sc01869a2.cif
_cod_data_source_block           pm162_0m_a
_cod_depositor_comments
'Adding full bibliography for 1567676--1567686.cif.'
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               1567684
_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.a Secondary CH2 refined with riding coordinates:
 C34(H34a,H34b)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C18(H18), C3(H3), C7(H7), C8(H8), C11(H11), C20(H20), C15(H15),
 C13(H13), C12(H12), C27(H27), C29(H29), C14(H14)
2.c Idealised Me refined as rotating group:
 C23(H23a,H23b,H23c), C22(H22a,H22b,H22c), C32(H32a,H32b,H32c), C24(H24a,H24b,
 H24c), C31(H31a,H31b,H31c), C33(H33a,H33b,H33c), C35(H35a,H35b,H35c)
;
_olex2_submission_special_instructions 'No special instructions were received'