CO-Reduction Chemistry: Reaction of a CO-Derived Formylhydridoborate with Carbon Monoxide, with Carbon Dioxide, and with Dihydrogen.
Jian, Zhongbao; Kehr, Gerald; Daniliuc, Constantin G.; Wibbeling, Birgit; Wiegand, Thomas; Siedow, Melanie; Eckert, Hellmut; Bursch, Markus; Grimme, Stefan; Erker, Gerhard; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b02548

data_4125993
_publ_section_title
;
 CO-Reduction Chemistry: Reaction of a CO-Derived Formylhydridoborate with
 Carbon Monoxide, with Carbon Dioxide, and with Dihydrogen.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b02548
_journal_year                    2017
_chemical_formula_sum            'C48 H48 B F10 N O3 S Zr'
_chemical_formula_weight         1010.96
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a'
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   25.3643(14)
_cell_length_b                   25.3643(14)
_cell_length_c                   33.4936(19)
_cell_measurement_reflns_used    6083
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      64.8978
_cell_measurement_theta_min      3.4850
_cell_volume                     21548(2)
_computing_cell_refinement       'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_data_collection
'APEX2 v.2014.1-----1 (Bruker AXS Inc., 2014)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_molecular_graphics
'APEX2 v.2014.1-----1 (Bruker AXS Inc., 2014)'
_computing_publication_material
'APEX2 v.2014.1-----1 (Bruker AXS Inc., 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'KappaCCD APEXII'
_diffrn_measurement_method       'phi / omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'CuK\a '
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1488
_diffrn_reflns_av_unetI/netI     0.1060
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            55783
_diffrn_reflns_theta_full        66.52
_diffrn_reflns_theta_max         66.52
_diffrn_reflns_theta_min         3.48
_diffrn_source                   'fine--focus sealed tube'
_exptl_absorpt_coefficient_mu    2.653
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
'Bruker AXS (2014). SADABS, Version 2014/2, Bruker AXS Inc., Madison,
Wisconsin, USA.'
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             8288
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.040
_platon_squeeze_details
;
Two badly disordered pentane molecules were found in the 
asymmetrical unit and could not be satisfactorily refined. The program 
SQUEEZE (Spek, A.L. (2015). Acta Cryst. C71, 9-18) was therefore used to
remove mathematically the effect of the solvent.
The quoted formula and derived parameters are not included the squeezed
solvent molecules. 
;
_refine_diff_density_max         0.909
_refine_diff_density_min         -1.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     599
_refine_ls_number_reflns         9394
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.1085
_refine_ls_R_factor_gt           0.0754
_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^)+(0.1202P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1905
_refine_ls_wR_factor_ref         0.2122
_reflns_number_gt                6194
_reflns_number_total             9394
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b02548_si_002.cif
_cod_data_source_block           erk8621
_cod_original_cell_volume        21548.(3)
_cod_database_code               4125993
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              56947
_shelx_hkl_checksum              34777
_shelx_fab_checksum              83598