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_1514318
_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         'C22 H24 Mo N2 O4'
_chemical_formula_sum            'C22 H24 Mo N2 O4'
_chemical_formula_weight         476.37
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-10-14
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.9132(6)
_cell_length_b                   11.6738(4)
_cell_length_c                   21.3034(8)
_cell_measurement_reflns_used    9874
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.387
_cell_measurement_theta_min      2.292
_cell_volume                     4454.9(3)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'Bruker APEX2 v2010-7.0 (Bruker, 2010)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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
'L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard, H. Puschmann, in preparation (2013)'
_computing_structure_solution
'L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard, H. Puschmann, in preparation (2013)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker X8 APEX II'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_unetI/netI     0.0229
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            31065
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.402
_diffrn_reflns_theta_min         2.827
_diffrn_source                   'sealed tube'
_diffrn_source_type              fine-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.617
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6263
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0604 before and 0.0498 after correction.
The Ratio of minimum to maximum transmission is 0.8404.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_description       block
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.664
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         4099
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0240
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0307P)^2^+3.1855P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0601
_refine_ls_wR_factor_ref         0.0647
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3500
_reflns_number_total             4099
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3sc53470g2.cif
_cod_data_source_block           kag_411_0ma
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_database_code               1514318
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.941
_shelx_estimated_absorpt_t_min   0.836
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H5(0.024) H6(0.024) H8(0.018) H14(0.019) H13(0.021) H11(0.017)
 H20A(0.047) H20B(0.047) H20C(0.047) H22A(0.048) H22B(0.048) H22C(0.048)
 H21A(0.051) H21B(0.051) H21C(0.051) H18A(0.038) H18B(0.038) H18C(0.038)
 H17A(0.043) H17B(0.043) H17C(0.043) H16A(0.034) H16B(0.034) H16C(0.034)
 Fixed X: H5(1.0294) H6(0.9689) H8(0.8415) H14(0.962) H13(0.8673) H11(0.8146)
 H20A(0.837) H20B(0.7869) H20C(0.7502) H22A(0.8092) H22B(0.722) H22C(0.7499)
 H21A(0.6541) H21B(0.6966) H21C(0.6825) H18A(0.8189) H18B(0.8856) H18C(0.8046)
 H17A(0.9336) H17B(0.9655) H17C(0.8999) H16A(0.8055) H16B(0.77) H16C(0.7563)
 Fixed Y: H5(1.1969) H6(1.2047) H8(0.938) H14(0.856) H13(0.7226) H11(0.8249)
 H20A(0.5535) H20B(0.6306) H20C(0.5252) H22A(0.5553) H22B(0.5377) H22C(0.6445)
 H21A(0.668) H21B(0.7694) H21C(0.7778) H18A(1.1912) H18B(1.2409) H18C(1.2234)
 H17A(0.9444) H17B(1.071) H17C(1.0239) H16A(0.9162) H16B(1.0009) H16C(1.0232)
 Fixed Z: H5(0.2392) H6(0.1447) H8(0.1998) H14(0.4515) H13(0.451) H11(0.2755)
 H20A(0.309) H20B(0.2634) H20C(0.3002) H22A(0.4249) H22B(0.4117) H22C(0.4526)
 H21A(0.3422) H21B(0.3063) H21C(0.3803) H18A(0.0335) H18B(0.0754) H18C(0.1055)
 H17A(0.0604) H17B(0.0501) H17C(0.0062) H16A(0.1016) H16B(0.0506) H16C(0.1239)
;
_shelx_res_checksum              78189
_shelx_hkl_checksum              872