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_7708822
_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         'C13 H26 Ge N2 O2'
_chemical_formula_sum            'C13 H26 Ge N2 O2'
_chemical_formula_weight         314.95
_chemical_name_systematic        ImMe2-Ge(OtBu)2
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_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            16
_cell_length_a                   17.4359(6)
_cell_length_b                   16.6515(6)
_cell_length_c                   24.2090(8)
_cell_measurement_reflns_used    9877
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      69.82
_cell_measurement_theta_min      3.67
_cell_volume                     7028.7(4)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0593
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            70160
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.162
_diffrn_reflns_theta_min         3.651
_exptl_absorpt_coefficient_mu    2.351
_exptl_absorpt_correction_T_max  0.8921
_exptl_absorpt_correction_T_min  0.7163
_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    1.191
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2656
_exptl_crystal_size_max          0.159
_exptl_crystal_size_mid          0.139
_exptl_crystal_size_min          0.117
_refine_diff_density_max         0.388
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         6690
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0411P)^2^+5.9602P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0869
_refine_ls_wR_factor_ref         0.0992
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5102
_reflns_number_total             6690
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02850b3.cif
_cod_data_source_block           riv2071
_cod_database_code               7708822
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.706
_shelx_estimated_absorpt_t_max   0.770
_shelx_res_checksum              97471
_shelx_hkl_checksum              50487