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_4125997
_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 H51 B F10 O2 Zr'
_chemical_formula_weight         951.91
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 102.420(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.7497(11)
_cell_length_b                   13.5222(6)
_cell_length_c                   29.0199(14)
_cell_measurement_reflns_used    9805
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      25.3599
_cell_measurement_theta_min      2.3621
_cell_volume                     8718.4(7)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection
;

APEX2 v.2014.1-1 (Bruker AXS Inc., 2014)

;
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'XP (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'MX mirror'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1211
_diffrn_reflns_av_unetI/netI     0.0524
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            191799
_diffrn_reflns_theta_full        25.42
_diffrn_reflns_theta_max         25.42
_diffrn_reflns_theta_min         2.07
_diffrn_source                   'Mo ImS'
_diffrn_source_type              'micro focus tube'
_exptl_absorpt_coefficient_mu    0.334
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.82
_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            yellow
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3920
_exptl_crystal_size_max          0.237
_exptl_crystal_size_mid          0.187
_exptl_crystal_size_min          0.084
_refine_diff_density_max         0.560
_refine_diff_density_min         -0.518
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1212
_refine_ls_number_reflns         16049
_refine_ls_number_restraints     319
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0397
_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^)+(0.0266P)^2^+9.8624P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0876
_reflns_number_gt                12277
_reflns_number_total             16049
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b02548_si_002.cif
_cod_data_source_block           erk8697
_cod_database_code               4125997
_shelx_res_checksum              9585
_shelx_hkl_checksum              69625