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_1514320
_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 N2 O4 W'
_chemical_formula_sum            'C22 H24 N2 O4 W'
_chemical_formula_weight         564.28
_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                   17.8251(9)
_cell_length_b                   11.6986(6)
_cell_length_c                   21.3193(11)
_cell_measurement_reflns_used    9133
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.337
_cell_measurement_theta_min      2.226
_cell_volume                     4445.7(4)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_collection       'Bruker APEX2 v2012.10-0 (Bruker, 2012)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_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 CCD'
_diffrn_detector_area_resol_mean 8.0
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'Fixed Chi Three-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker D8 APEX'
_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  0.0373
_diffrn_reflns_av_unetI/netI     0.0175
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            49764
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.380
_diffrn_reflns_theta_min         1.910
_diffrn_source                   'sealed tube'
_diffrn_source_type              fine-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.225
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4767
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1127 before and 0.0466 after correction.
The Ratio of minimum to maximum transmission is 0.6395.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            Violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.686
_exptl_crystal_description       Rod
_exptl_crystal_F_000             2208
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.756
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         4560
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0200
_refine_ls_R_factor_gt           0.0159
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0165P)^2^+3.4013P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0364
_refine_ls_wR_factor_ref         0.0387
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4051
_reflns_number_total             4560
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3sc53470g2.cif
_cod_data_source_block           kag4_19_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.

'_exptl_crystal_colour_primary' value 'Violet' changed
to 'violet' 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               1514320
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.421
_shelx_estimated_absorpt_t_min   0.146
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H5(0.023) H6(0.023) H8(0.017) H11(0.017) H13(0.02) H14(0.019)
 H16A(0.034) H16B(0.034) H16C(0.034) H17A(0.038) H17B(0.038) H17C(0.038)
 H18A(0.041) H18B(0.041) H18C(0.041) H20A(0.049) H20B(0.049) H20C(0.049)
 H21A(0.046) H21B(0.046) H21C(0.046) H22A(0.047) H22B(0.047) H22C(0.047)
 Fixed X: H5(0.0301) H6(-0.0308) H8(-0.1587) H11(-0.1855) H13(-0.1308) H14(-
 0.036) H16A(-0.2439) H16B(-0.2294) H16C(-0.1937) H17A(-0.1139) H17B(-0.182)
 H17C(-0.1947) H18A(-0.0643) H18B(-0.0989) H18C(-0.0336) H20A(-0.304) H20B(-
 0.3459) H20C(-0.3172) H21A(-0.1614) H21B(-0.2485) H21C(-0.2124) H22A(-0.2466)
 H22B(-0.2773) H22C(-0.1891)
 Fixed Y: H5(0.8009) H6(0.7923) H8(1.0594) H11(1.1734) H13(1.2747) H14(1.1407)
 H16A(0.9748) H16B(0.9981) H16C(1.0813) H17A(0.7568) H17B(0.8063) H17C(0.7736)
 H18A(1.0514) H18B(0.9737) H18C(0.9244) H20A(1.2306) H20B(1.3314) H20C(1.2212)
 H21A(1.4443) H21B(1.4736) H21C(1.3681) H22A(1.3544) H22B(1.4598) H22C(1.4452)
 Fixed Z: H5(0.2407) H6(0.1461) H8(0.2003) H11(0.2767) H13(0.452) H14(0.452)
 H16A(0.1239) H16B(0.051) H16C(0.1025) H17A(0.0752) H17B(0.0344) H17C(0.1066)
 H18A(0.0616) H18B(0.007) H18C(0.0508) H20A(0.3079) H20B(0.3445) H20C(0.3819)
 H21A(0.3102) H21B(0.3018) H21C(0.2648) H22A(0.4544) H22B(0.414) H22C(0.4254)
;
_shelx_res_checksum              72085
_shelx_hkl_checksum              77697