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_4125987
_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            'C29 H42 O Zr'
_chemical_formula_weight         497.85
_chemical_name_systematic
; 
 ? 
;
_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                80.409(2)
_cell_angle_beta                 89.735(2)
_cell_angle_gamma                70.163(2)
_cell_formula_units_Z            2
_cell_length_a                   8.4940(2)
_cell_length_b                   9.6405(4)
_cell_length_c                   17.2340(6)
_cell_measurement_reflns_used    2895
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      4.08
_cell_volume                     1306.88(8)
_computing_cell_refinement       'Collect (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'XP (BrukerAXS, 2000)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Nonius KappaCCD APEXII'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Montel mirror'
_diffrn_radiation_source         'rotating anode Nonius FR591'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.054
_diffrn_reflns_av_sigmaI/netI    0.0491
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9589
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         4.30
_exptl_absorpt_coefficient_mu    0.438
_exptl_absorpt_correction_T_max  0.9913
_exptl_absorpt_correction_T_min  0.9493
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.312
_refine_diff_density_min         -0.530
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         4524
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0555
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0371P)^2^+3.9443P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1250
_refine_ls_wR_factor_ref         0.1324
_reflns_number_gt                4037
_reflns_number_total             4524
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja7b02548_si_002.cif
_cod_data_source_block           erk8417
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4125987