A Cobalt Hydride Catalyst for the Hydrogenation of CO2: Pathways for Catalysis and Deactivation
Jeletic, Matthew S.; Helm, Monte L.; Hulley, Elliott B.; Mock, Michael T.; Appel, Aaron M.; Linehan, John C.; ACS Catalysis 4 (2014) 3755–; doi:10.1021/cs5009927

data_4511996
_publ_section_title
;
 A Cobalt Hydride Catalyst for the Hydrogenation of CO2: Pathways for
 Catalysis and Deactivation
;
_journal_issue                   10
_journal_name_full               'ACS Catalysis'
_journal_page_first              3755
_journal_paper_doi               10.1021/cs5009927
_journal_volume                  4
_journal_year                    2014
_chemical_formula_moiety         'C15 H34 N4 P, C H O2'
_chemical_formula_sum            'C16 H35 N4 O2 P'
_chemical_formula_weight         346.45
_chemical_name_systematic        '[VerkaedeH][Formate)'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-09-20
_audit_creation_method
;
  Olex2 1.2-beta
  (compiled 2012.05.09 svn.r2324, GUI svn.r4230)
;
_cell_angle_alpha                72.135(2)
_cell_angle_beta                 84.493(3)
_cell_angle_gamma                64.509(2)
_cell_formula_units_Z            2
_cell_length_a                   9.4920(8)
_cell_length_b                   10.0652(9)
_cell_length_c                   11.6878(10)
_cell_measurement_reflns_used    6690
_cell_measurement_temperature    145
_cell_measurement_theta_max      31.23
_cell_measurement_theta_min      2.35
_cell_volume                     958.49(14)
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      145
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22542
_diffrn_reflns_theta_full        31.52
_diffrn_reflns_theta_max         31.52
_diffrn_reflns_theta_min         2.35
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.158
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9370
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0693 before and 0.0421 after correction.
The Ratio of minimum to maximum transmission is 0.9370.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             380
_exptl_crystal_preparation       'slow evaporation'
_exptl_crystal_recrystallization_method 'grown by slow evaporation'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.457
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         6295
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0448
_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^)+(0.0566P)^2^+0.2782P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1109
_refine_ls_wR_factor_ref         0.1222
_reflns_number_gt                4824
_reflns_number_total             6295
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cs5009927_si_004.cif
_cod_data_source_block           helm110_0m
_cod_depositor_comments
'Adding full bibliography for 4511995--4511996.cif.'
_cod_database_code               4511996
_refinement_special_details
'Hydrogen atoms on the formate carbon and phosphorus atoms work located and allowed to refine freely.'