Heavier congeners of CO and CO2as ligands: from zero-valent germanium (‘germylone’) to isolable monomeric GeX and GeX2complexes (X = S, Se, Te)
Xiong, Yun; Yao, Shenglai; Karni, Miriam; Kostenko, Arseni; Burchert, Alexander; Apeloig, Yitzhak; Driess, Matthias; Chem. Sci. 7 (2016) 5462–; doi:10.1039/C6SC01839D

data_1543300
_publ_section_title
;
 Heavier congeners of CO and CO2as ligands: from zero-valent germanium
 (&#x2018;germylone&#x2019;) to isolable monomeric GeX and GeX2complexes
 (X = S, Se, Te)
;
_journal_issue                   8
_journal_name_full               'Chem. Sci.'
_journal_page_first              5462
_journal_paper_doi               10.1039/C6SC01839D
_journal_volume                  7
_journal_year                    2016
_chemical_formula_sum            'C43 H64 Cl3 Ga Ge N4 O3 Te'
_chemical_formula_weight         1061.24
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_audit_update_record
;
2016-03-04 deposited with the CCDC.
2016-05-10 downloaded from the CCDC.
;
_cell_angle_alpha                69.253(2)
_cell_angle_beta                 83.744(2)
_cell_angle_gamma                84.543(2)
_cell_formula_units_Z            2
_cell_length_a                   11.3788(3)
_cell_length_b                   13.0772(3)
_cell_length_c                   17.5125(4)
_cell_measurement_reflns_used    9024
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      71.6050
_cell_measurement_theta_min      2.7140
_cell_volume                     2417.94(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_sigmaI/netI    0.0375
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -9
_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            14971
_diffrn_reflns_theta_full        67.49
_diffrn_reflns_theta_max         67.49
_diffrn_reflns_theta_min         2.71
_exptl_absorpt_coefficient_mu    7.950
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31666
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.197
_refine_diff_density_min         -1.761
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         8672
_refine_ls_number_restraints     88
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0560
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0966P)^2^+3.3777P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1475
_refine_ls_wR_factor_ref         0.1531
_reflns_number_gt                7814
_reflns_number_total             8672
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6sc01839d2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 1543298--1543302.cif.'
_cod_original_cell_volume        2417.94(10)
_cod_original_sg_symbol_H-M      p-1
_cod_database_code               1543300