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_1567677
_publ_section_title
;
 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         'C39 H36 Ge N2 S'
_chemical_formula_sum            'C39 H36 Ge N2 S'
_chemical_formula_weight         637.37
_chemical_name_systematic        DPMGe(S)Ph
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-09-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-10-21 deposited with the CCDC.	2022-09-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.409(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.9949(5)
_cell_length_b                   21.1802(14)
_cell_length_c                   19.6152(13)
_cell_measurement_reflns_used    9853
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      28.25
_cell_measurement_theta_min      2.31
_cell_volume                     3276.8(4)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0576
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            102855
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.341
_diffrn_reflns_theta_min         2.314
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.028
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6843
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1119 before and 0.0717 after correction.
The Ratio of minimum to maximum transmission is 0.9177.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_description       block
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.496
_refine_diff_density_min         -0.984
_refine_diff_density_rms         0.124
_refine_ls_extinction_coef       0.0035(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         8110
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.0953
_refine_ls_R_factor_gt           0.0887
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0733P)^2^+21.9943P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2482
_refine_ls_wR_factor_ref         0.2521
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7205
_reflns_number_total             8110
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc01869a2.cif
_cod_data_source_block           pm328_0m_a
_cod_depositor_comments
'Adding full bibliography for 1567676--1567686.cif.'
_cod_database_code               1567677
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C38(H38), C34(H34), C9(H9), C18(H18), C10(H10), C37(H37), C31(H31), C28(H28),
 C35(H35), C36(H36), C2(H2), C13(H13), C14(H14), C20(H20), C6(H6), C4(H4),
 C5(H5), C3(H3)
2.b Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C32(H32A,H32B,H32C), C27(H27A,H27B,H27C), C29(H29A,H29B,
 H29C), C21(H21A,H21B,H21C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              53274
_shelx_hkl_checksum              77567
_olex2_submission_special_instructions 'No special instructions were received'