Electrocatalytic Reduction of Carbon Dioxide by Mn(CN)(2,2'-bipyridine)(CO)3: CN Coordination Alters Mechanism.
Machan, Charles W.; Stanton, 3rd, Charles J; Vandezande, Jonathon E.; Majetich, George F.; Schaefer, 3rd, Henry F; Kubiak, Clifford P.; Agarwal, Jay; Inorganic chemistry 54 (2015) 8849–8856; doi:10.1021/acs.inorgchem.5b01715

data_4344075
_publ_section_title
;
 Electrocatalytic Reduction of Carbon Dioxide by
 Mn(CN)(2,2'-bipyridine)(CO)3: CN Coordination Alters Mechanism.
;
_publ_section_keywords
;
crystal structure
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8849
_journal_page_last               8856
_journal_paper_doi               10.1021/acs.inorgchem.5b01715
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C14 H8 Mn N3 O3, C4 H8 O, 0.5(H2 O)'
_chemical_formula_sum            'C18 H17 Mn N3 O4.5'
_chemical_formula_weight         402.28
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-04-21
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-04-21 # Formatted by publCIF

;
_cell_angle_alpha                80.936(8)
_cell_angle_beta                 79.278(6)
_cell_angle_gamma                89.922(6)
_cell_formula_units_Z            4
_cell_length_a                   6.6349(7)
_cell_length_b                   16.3268(17)
_cell_length_c                   17.535(2)
_cell_measurement_reflns_used    6019
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.388
_cell_measurement_theta_min      2.396
_cell_volume                     1842.3(3)
_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      100.15(2)
_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 0.992
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0308
_diffrn_reflns_av_unetI/netI     0.0509
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13307
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.447
_diffrn_reflns_theta_min         1.263
_diffrn_source                   'sealed tube'
_diffrn_source_type              fine-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.747
_exptl_absorpt_correction_T_max  0.0932
_exptl_absorpt_correction_T_min  0.0592
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0593 before and 0.0410 after correction.
The Ratio of minimum to maximum transmission is 0.6352.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_description       needle
_exptl_crystal_F_000             828
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.425
_refine_diff_density_min         -0.517
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     482
_refine_ls_number_reflns         6809
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0420
_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^)+(0.0477P)^2^+0.9302P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0939
_refine_ls_wR_factor_ref         0.0980
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6065
_reflns_number_total             6809
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01715_si_002.cif
_cod_data_source_block           MnbpyCO_3CN
_cod_depositor_comments          'Adding full bibliography for 4344075.cif.'
_cod_database_code               4344075
_publcif_datablock.id            {95f91ad1-23ba-4d32-9c6c-cca13e3bb863}
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5402(9) 0.4598(9)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
3.a Free rotating group:
 O5(H5A,H5B)
3.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C15A(H15C,
 H15D), C16A(H16C,H16D), C17A(H17C,H17D), C18A(H18C,H18D)
3.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C1A(H1A),
 C2A(H2A), C3A(H3A), C4A(H4A), C7A(H7A), C8A(H8A), C9A(H9A), C10A(H10A)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'