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_4514025
_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            'C52 H69 B N O3.5 Si Sn'
_chemical_formula_weight         921.67
_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                88.763(3)
_cell_angle_beta                 86.920(3)
_cell_angle_gamma                85.612(3)
_cell_formula_units_Z            2
_cell_length_a                   10.1191(4)
_cell_length_b                   12.9066(5)
_cell_length_c                   18.7646(7)
_cell_measurement_reflns_used    9556
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      3.05
_cell_volume                     2439.63(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-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0395
_diffrn_reflns_av_sigmaI/netI    0.0511
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19657
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    0.590
_exptl_absorpt_correction_T_max  0.891
_exptl_absorpt_correction_T_min  0.751
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav (Blessing)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             970
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.311
_refine_diff_density_min         -0.458
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     578
_refine_ls_number_reflns         9556
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0414
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0578P)^2^+1.3419P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1009
_refine_ls_wR_factor_ref         0.1086
_reflns_number_gt                8141
_reflns_number_total             9556
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cs6b03306_si_007.cif
_cod_data_source_block           compound11
_cod_depositor_comments
'Adding full bibliography for 4514024--4514026.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C52 H69 B N O3.50 Si Sn'
_cod_database_code               4514025