Electrocatalytic CO2 reduction by M(bpy-R)(CO)4 (M = Mo, W; R = H, tBu) complexes. Electrochemical, spectroscopic, and computational studies and comparison with group 7 catalysts
Clark, Melissa L.; Grice, Kyle A.; Moore, Curtis E.; Rheingold, Arnold L.; Kubiak, Clifford P.; Chemical Science 5 (2014) 1894–; doi:10.1039/c3sc53470g

data_1514321
_publ_section_title
;
 Electrocatalytic CO2 reduction by M(bpy-R)(CO)4 (M = Mo, W; R = H, tBu)
 complexes. Electrochemical, spectroscopic, and computational studies and
 comparison with group 7 catalysts
;
_journal_issue                   5
_journal_name_full               'Chemical Science'
_journal_page_first              1894
_journal_paper_doi               10.1039/c3sc53470g
_journal_volume                  5
_journal_year                    2014
_chemical_formula_moiety         'C30 H40 K N2 O11 W'
_chemical_formula_sum            'C30 H40 K N2 O11 W'
_chemical_formula_weight         827.60
_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'
_audit_creation_date             2013-09-13
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                90
_cell_angle_beta                 107.674(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2130(3)
_cell_length_b                   18.7469(5)
_cell_length_c                   15.4880(4)
_cell_measurement_temperature    100
_cell_volume                     3378.69(15)
_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.
;
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.9969
_diffrn_measured_fraction_theta_max 0.9969
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            31036
_diffrn_reflns_theta_full        25.4121
_diffrn_reflns_theta_max         25.41
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    3.601
_exptl_crystal_density_diffrn    1.6269
_exptl_crystal_F_000             1659.0286
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.0803
_refine_diff_density_min         -0.5909
_refine_diff_density_rms         0.1721
_refine_ls_d_res_high            0.8281
_refine_ls_d_res_low             11.6365
_refine_ls_goodness_of_fit_ref   0.7312
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    64
_refine_ls_number_parameters     405
_refine_ls_number_reflns         6209
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.7312
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0226
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0898
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              22
_reflns_limit_k_min              0
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                5323
_reflns_number_total             6209
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c3sc53470g2.cif
_cod_data_source_block           MC_Wbipy_anion
_cod_database_code               1514321
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C30(H30a,H30b), C29(H29a,H29b), C28(H28a,H28b), C27(H27a,H27b), C20(H20a,
 H20b), C19(H19a,H19b), C18(H18a,H18b), C17(H17a,H17b), C16(H16a,H16b),
 C15(H15a,H15b), C26(H26a,H26b), C25(H25a,H25b), C24(H24a,H24b), C23(H23a,H23b),
  C22(H22a,H22b), C21(H21a,H21b)
2.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C13(H13), C12(H12), C11(H11), C5(H5), C6(H6), C7(H7), C8(H8)
;