Efficient Reduction of Carbon Dioxide to Methanol Equivalents Catalyzed by Two-Coordinate Amido–Germanium(II) and −Tin(II) Hydride Complexes
Hadlington, Terrance J.; Kefalidis, Christos E.; Maron, Laurent; Jones, Cameron; ACS Catalysis 7 (2017) 1853–; doi:10.1021/acscatal.6b03306

data_4514053
_publ_section_title
;
 Efficient Reduction of Carbon Dioxide to Methanol Equivalents Catalyzed
 by Two-Coordinate Amido--Germanium(II) and &#x2212;Tin(II) Hydride
 Complexes
;
_journal_issue                   3
_journal_name_full               'ACS Catalysis'
_journal_page_first              1853
_journal_paper_doi               10.1021/acscatal.6b03306
_journal_volume                  7
_journal_year                    2017
_chemical_formula_sum            'C50 H64 B Ge N O3 Si'
_chemical_formula_weight         838.51
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                91.00(3)
_cell_angle_beta                 91.60(3)
_cell_angle_gamma                98.10(3)
_cell_formula_units_Z            2
_cell_length_a                   9.930(2)
_cell_length_b                   14.880(3)
_cell_length_c                   15.290(3)
_cell_measurement_reflns_used    8702
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      2.92
_cell_volume                     2235.3(8)
_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-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker Apex X8'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0201
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8702
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.92
_exptl_absorpt_coefficient_mu    0.754
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_correction_T_min  0.921
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav (Blessing)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             892
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.937
_refine_diff_density_min         -1.095
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     537
_refine_ls_number_reflns         8702
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0671
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0627P)^2^+7.3087P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1708
_refine_ls_wR_factor_ref         0.1733
_reflns_number_gt                8052
_reflns_number_total             8702
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cs6b03306_si_004.cif
_cod_data_source_block           compound7
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4514053