Access to metastable [GeH2]n materials via a molecular “bottom-up” approach
Sinclair, Jocelyn; Medroa Del Pino, William; Aku-Dominguez, Kwami; Minami, Yohei; Kiran, Anagha; Ferguson, Michael J.; Yasuda, Makoto; Rivard, Eric; Dalton Transactions  (2021) –; doi:10.1039/D1DT02850B

data_7708823
_publ_section_title
;
 Access to metastable [GeH2]n materials via a molecular
 &#x201C;bottom-up&#x201D; approach
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02850B
_journal_year                    2021
_chemical_formula_moiety         'C12 H27 Ge K O3'
_chemical_formula_sum            'C12 H27 Ge K O3'
_chemical_formula_weight         331.02
_chemical_name_common            K[Ge(OtBu)3]
_chemical_name_systematic        (Tri-tert-butoxygermyl)potassium
_chemical_properties_physical    Moisture-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-07-06 deposited with the CCDC.	2021-11-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.8817(5)
_cell_length_b                   10.4187(6)
_cell_length_c                   18.1622(10)
_cell_measurement_reflns_used    2957
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      70.27
_cell_measurement_theta_min      4.87
_cell_volume                     1680.65(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2015)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0822
_diffrn_reflns_av_unetI/netI     0.0518
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            23475
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.601
_diffrn_reflns_theta_min         4.870
_exptl_absorpt_coefficient_mu    4.664
_exptl_absorpt_correction_T_max  0.8419
_exptl_absorpt_correction_T_min  0.6637
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., 
 J. Appl. Cryst. 48 (2015) 3-10 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_description       plate
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.017
_refine_diff_density_max         0.272
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details
; 
 Flack x determined using 1180 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.031(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         3381
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0361P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0794
_refine_ls_wR_factor_ref         0.0820
_reflns_Friedel_coverage         0.717
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.966
_reflns_number_gt                3025
_reflns_number_total             3381
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02850b3.cif
_cod_data_source_block           riv2036
_cod_database_code               7708823
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.721
_shelx_estimated_absorpt_t_max   0.925
_shelx_res_checksum              39320
_shelx_hkl_checksum              54289