A Molecular Ruthenium Electrocatalyst for the Reduction of Carbon Dioxide to CO and Formate.
Machan, Charles W.; Sampson, Matthew D.; Kubiak, Clifford P.; Journal of the American Chemical Society 137 (2015) 8564–8571; doi:10.1021/jacs.5b03913

data_4123879
_publ_section_title
;
 A Molecular Ruthenium Electrocatalyst for the Reduction of Carbon Dioxide
 to CO and Formate.
;
_journal_issue                   26
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8564
_journal_page_last               8571
_journal_paper_doi               10.1021/jacs.5b03913
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C30 H28 Cl2 N2 O2 Ru'
_chemical_formula_sum            'C54 H76 Cl2 N2 O8 Ru'
_chemical_formula_weight         1053.13
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-03-04
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-03-16 # Formatted by publCIF
;
_cell_angle_alpha                90
_cell_angle_beta                 91.104(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4514(15)
_cell_length_b                   26.119(4)
_cell_length_c                   17.888(3)
_cell_measurement_reflns_used    9820
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.405
_cell_measurement_theta_min      2.292
_cell_volume                     4415.0(12)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2013.6-2 (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2008)'
_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 0.993
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker X8 APEX Mo'
_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_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_laue_measured_fraction_full 0.993
_diffrn_reflns_laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            64108
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.480
_diffrn_reflns_theta_min         1.931
_diffrn_source                   'sealed tube'
_diffrn_source_type              fine-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.540
_exptl_absorpt_correction_T_max  0.0452
_exptl_absorpt_correction_T_min  0.0225
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0779 before and 0.0587 after correction.
The Ratio of minimum to maximum transmission is 0.4978.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_description       plate
_exptl_crystal_F_000             2224
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.929
_refine_diff_density_min         -0.698
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         9034
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0476
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0579P)^2^+7.5712P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1222
_refine_ls_wR_factor_ref         0.1284
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7347
_reflns_number_total             9034
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b03913_si_002.cif
_cod_data_source_block           RumesbpyCO2Cl2
_cod_depositor_comments          'Adding full bibliography for 4123879.cif.'
_cod_original_cell_volume        4415.1(12)
_cod_database_code               4123879
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.948
_shelx_estimated_absorpt_t_min   0.855
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2AA(H2AA), C6AA(H6AA), C7AA(H7AA), C8AA(H8AA), C21(H21), C24(H24), C29(H29),
 C30(H30), C32(H32), C34(H34)
2.b Idealised Me refined as rotating group:
 C0BA(H0BA,H0BB,H0BC), C4AA(H4AA,H4AB,H4AC), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C), C33(H33A,H33B,H33C), C35(H35A,H35B,H35C)
;
_shelx_res_checksum              37982
_shelx_hkl_checksum              2632
_shelx_fab_checksum              73785
_olex2_submission_special_instructions 'No special instructions were received'