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_1543298
_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            'C39 H52 Cl3 Ga Ge N8'
_chemical_formula_weight         881.55
_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 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_audit_update_record
;
2016-03-04 deposited with the CCDC.
2016-05-10 downloaded from the CCDC.
;
_cell_angle_alpha                109.690(3)
_cell_angle_beta                 90.728(2)
_cell_angle_gamma                112.290(3)
_cell_formula_units_Z            2
_cell_length_a                   12.8149(4)
_cell_length_b                   13.6703(4)
_cell_length_c                   14.6341(4)
_cell_measurement_reflns_used    11030
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      73.6050
_cell_measurement_theta_min      3.2300
_cell_volume                     2204.15(14)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_sigmaI/netI    0.0357
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14861
_diffrn_reflns_theta_full        67.49
_diffrn_reflns_theta_max         67.49
_diffrn_reflns_theta_min         3.25
_exptl_absorpt_coefficient_mu    3.541
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.15591
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.685
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         7940
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0458
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0672P)^2^+2.9264P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1244
_refine_ls_wR_factor_ref         0.1268
_reflns_number_gt                7328
_reflns_number_total             7940
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6sc01839d2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 1543298--1543302.cif.'
_cod_original_cell_volume        2204.15(11)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1543298