Halogen-free GeO<sub>2</sub> conversion: electrochemical reduction vs. complexation in (DTBC)<sub>2</sub>Ge[Py(CN)<sub>n</sub>] (n = 0…2) complexes.
Nikolaevskaya, Elena N.; Saverina, Evgeniya A.; Starikova, Alyona A.; Farhati, Amel; Kiskin, Mikhail A.; Syroeshkin, Mikhail A.; Egorov, Mikhail P.; Jouikov, Viatcheslav V.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 17127–17133; doi:10.1039/c8dt03397h

data_7047959
_publ_section_title
;
 Halogen-free GeO<sub>2</sub> conversion: electrochemical reduction vs.
 complexation in (DTBC)<sub>2</sub>Ge[Py(CN)<sub>n</sub>] (n = 0&#x2026;2)
 complexes.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17127
_journal_page_last               17133
_journal_paper_doi               10.1039/c8dt03397h
_journal_volume                  47
_journal_year                    2018
_chemical_formula_sum            'C54 H64 Ge N4 O4'
_chemical_formula_weight         905.68
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2018-10-29 deposited with the CCDC.
2018-11-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.243(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.0823(15)
_cell_length_b                   22.183(2)
_cell_length_c                   7.3630(8)
_cell_measurement_reflns_used    2599
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.29
_cell_measurement_theta_min      2.28
_cell_volume                     2456.7(4)
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.1035
_diffrn_reflns_av_unetI/netI     0.1188
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            20699
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         1.354
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.672
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_description       parallelograme
_exptl_crystal_F_000             960
_exptl_crystal_preparation       Electrochemistry
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene'
_refine_diff_density_max         0.680
_refine_diff_density_min         -0.871
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         6079
_refine_ls_number_restraints     161
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1010
_refine_ls_R_factor_gt           0.0513
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0650P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1246
_refine_ls_wR_factor_ref         0.1605
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3520
_reflns_number_total             6079
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03397h2.cif
_cod_data_source_block           2
_cod_depositor_comments          'Adding full bibliography for 7047959.cif.'
_cod_database_code               7047959
_shelxl_version_number           2014/6
_shelx_res_checksum              96612