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_1567681
_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 H49 Ge N3 Se Si2'
_chemical_formula_sum            'C39 H49 Ge N3 Se Si2'
_chemical_formula_weight         767.56
_chemical_name_systematic        DPMGe(Se)N(TMS)2
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_audit_creation_date             2021-07-01
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-10-21 deposited with the CCDC.	2022-09-01 downloaded from the CCDC.
;
_cell_angle_alpha                86.969(4)
_cell_angle_beta                 77.252(4)
_cell_angle_gamma                73.433(4)
_cell_formula_units_Z            2
_cell_length_a                   8.9661(6)
_cell_length_b                   11.2946(8)
_cell_length_c                   19.9064(13)
_cell_measurement_reflns_used    9986
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.32
_cell_measurement_theta_min      2.16
_cell_volume                     1884.5(2)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.9955
_diffrn_measured_fraction_theta_max 0.9892
_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  0.0889
_diffrn_reflns_av_unetI/netI     0.0629
_diffrn_reflns_Laue_measured_fraction_full 0.9955
_diffrn_reflns_Laue_measured_fraction_max 0.9892
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            45430
_diffrn_reflns_point_group_measured_fraction_full 0.9955
_diffrn_reflns_point_group_measured_fraction_max 0.9892
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         26.47
_diffrn_reflns_theta_min         1.88
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.873
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5645
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1409 before and 0.0807 after correction.
The Ratio of minimum to maximum transmission is 0.7573.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_description       block
_exptl_crystal_F_000             796
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         4.6401
_refine_diff_density_min         -2.3605
_refine_diff_density_rms         0.3077
_refine_ls_d_res_high            0.7972
_refine_ls_d_res_low             10.8251
_refine_ls_goodness_of_fit_ref   1.0690
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    76
_refine_ls_number_parameters     415
_refine_ls_number_reflns         7711
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0690
_refine_ls_R_factor_all          0.1096
_refine_ls_R_factor_gt           0.0903
_refine_ls_shift/su_max          0.0009
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1347P)^2^+28.7673P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2538
_refine_ls_wR_factor_ref         0.2706
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              -10
_reflns_limit_k_max              14
_reflns_limit_k_min              -14
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                6043
_reflns_number_total             7711
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2sc01869a2.cif
_cod_data_source_block           pm395_0m_a
_cod_depositor_comments
'Adding full bibliography for 1567676--1567686.cif.'
_cod_database_code               1567681
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(C12) = Uanis(C7)
Uanis(N2) = Uanis(C12)
2. Rigid body (RIGU) restrains
 N2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Aromatic/amide H refined with riding coordinates:
 C20(H20), C18(H18), C13(H13), C4(H4), C27(H27), C14(H14), C30(H30), C5(H5),
 C9(H9), C6(H6), C2(H2), C10(H10), C3(H3)
3.b Idealised Me refined as rotating group:
 C34(H34a,H34b,H34c), C37(H37a,H37b,H37c), C00R(H00a,H00b,H00c), C22(H22a,H22b,
 H22c), C32(H32a,H32b,H32c), C23(H23a,H23b,H23c), C38(H38a,H38b,H38c), C33(H33a,
 H33b,H33c), C35(H35a,H35b,H35c), C26(H26a,H26b,H26c), C36(H36a,H36b,H36c),
 C29(H29a,H29b,H29c)
;
_olex2_submission_special_instructions 'No special instructions were received'