Photoreduction of Carbon Dioxide to Carbon Monoxide with Hydrogen Catalyzed by a Rhenium(I) Phenanthroline-Polyoxometalate Hybrid Complex
Jessica Ettedgui; Yael Diskin-Posner; Lev Weiner; Ronny Neumann; Journal of the American Chemical Society 133 (2011) 188–190; doi:10.1021/ja1078199

data_4105522
_publ_section_title
;
 Photoreduction of Carbon Dioxide to Carbon Monoxide with Hydrogen
 Catalyzed by a Rhenium(I) Phenanthroline-Polyoxometalate Hybrid Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              188
_journal_page_last               190
_journal_paper_doi               10.1021/ja1078199
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety
'C27 H26 N4 Na O48 P Re W12, 3(C2 H3 N), 3.5(H2 O)'
_chemical_formula_sum            'C33 H43.5 N7 Na O51.5 P Re W12'
_chemical_formula_weight         3808.61
_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                92.9650(10)
_cell_angle_beta                 97.4110(10)
_cell_angle_gamma                106.9480(10)
_cell_formula_units_Z            2
_cell_length_a                   12.3808(3)
_cell_length_b                   12.7008(3)
_cell_length_c                   23.8421(5)
_cell_measurement_reflns_used    51494
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.4335
_cell_measurement_theta_min      2.595
_cell_volume                     3540.49(14)
_computing_cell_refinement       'APEX 2'
_computing_data_collection       'APEX 2'
_computing_data_reduction        'APEX 2'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II Kappa CCD'
_diffrn_measurement_method       'Omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0432
_diffrn_reflns_av_sigmaI/netI    0.0506
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            51391
_diffrn_reflns_theta_full        28.49
_diffrn_reflns_theta_max         28.49
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    21.242
_exptl_absorpt_correction_T_max  0.4165
_exptl_absorpt_correction_T_min  0.2252
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker APEX-2'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.573
_exptl_crystal_description       prism
_exptl_crystal_F_000             3383
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.083
_refine_diff_density_min         -2.204
_refine_diff_density_rms         0.334
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     932
_refine_ls_number_reflns         17690
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0395
_refine_ls_shift/su_max          0.041
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0260P)^2^+57.5597P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0806
_refine_ls_wR_factor_ref         0.0880
_reflns_number_gt                13696
_reflns_number_total             17690
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1078199_si_002.cif
_cod_data_source_block           n304
_cod_depositor_comments
;

2023-09-06
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C66 H87 N14 Na2 O103 P2 Re2 W24'
_cod_original_formula_weight         7617.22
_cod_original_formula_moiety
'2(C27 H26 N4 Na O48 P Re W12), 6(C2 H3 N), 7(H2 O)'
_cod_original_formula_units_Z            1
_cod_original_sg_symbol_Hall     -P1
_cod_database_code               4105522