Catalytic CO2 Activation Assisted by Rhenium Hydride/B(C6F5)3 Frustrated Lewis Pairs-Metal Hydrides Functioning as FLP Bases
Yanfeng Jiang; Olivier Blacque; Thomas Fox; Heinz Berke; Journal of the American Chemical Society 135 (2013) 7751–7760; doi:10.1021/ja402381d

data_4119791
_publ_contact_author             'Dr. Blacque, Olivier'
_publ_contact_author_email       oblacque@aci.uzh.ch
_publ_contact_author_fax         '+41 44 63 54 681'
_publ_contact_author_phone       '+41 44 63 54 651'
_publ_section_title
;
 Catalytic CO2 Activation Assisted by Rhenium Hydride/B(C6F5)3 Frustrated
 Lewis Pairs-Metal Hydrides Functioning as FLP Bases
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7751
_journal_page_last               7760
_journal_paper_doi               10.1021/ja402381d
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C9 H20 N, C H O2'
_chemical_formula_sum            'C10 H21 N O2'
_chemical_formula_weight         187.28
_chemical_name_systematic        ' 2,2,6,6-Tetramethylpiperidinium formate'
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2013-03-04 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.6025(2)
_cell_length_b                   11.5901(1)
_cell_length_c                   9.6145(1)
_cell_measurement_reflns_used    10690
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      76.87
_cell_measurement_theta_min      2.25
_cell_volume                     2184.37(4)
_computing_cell_refinement
;
CrysAlisPro, version 1.171.36.20 ((Agilent Technologies, 2012)
;
_computing_data_collection
;
CrysAlisPro, version 1.171.36.20 (Agilent Technologies, 2012)
;
_computing_data_reduction
;
CrysAlisPro, version 1.171.36.20 (Agilent Technologies, 2012)
;
_computing_molecular_graphics
;
<i>ORTEP-3 for Windows</i> (Farrugia, 1997) and/or <i>Mercury</i> (Macrae et
al.,
2006)
;
_computing_publication_material
; 
<i>WinGX</i> (Farrugia, 1999), <i>PLATON for Windows</i> (Spek, 2003) and
<i>publCIF</i> (Westrip, 2010)
;
_computing_structure_refinement  ' SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    ' SHELXS97 (Sheldrick, 2008) '
_diffrn_ambient_temperature      183(2)
_diffrn_detector                 'Atlas CCD camera on \k goniostat'
_diffrn_detector_area_resol_mean 10.3801
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type
'Oxford Diffraction SuperNova, dual radiation diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_sigmaI/netI    0.0189
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            15119
_diffrn_reflns_theta_full        77.08
_diffrn_reflns_theta_max         77.08
_diffrn_reflns_theta_min         4.51
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.620
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_correction_T_min  0.824
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Version 1.171.36.20 (Agilent Technologies, 2011)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.139
_exptl_crystal_description       block
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         2422
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0735P)^2^+0.8152P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1389
_refine_ls_wR_factor_ref         0.1398
_reflns_number_gt                2352
_reflns_number_total             2422
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja402381d_si_003.cif
_cod_data_source_block           11
_cod_database_code               4119791