Electrocatalytic reduction of carbon dioxide with Mn(terpyridine) carbonyl complexes.
Machan, Charles W.; Kubiak, Clifford P.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 17179–17186; doi:10.1039/c6dt03243e

data_7040768
_publ_section_title
;
 Electrocatalytic reduction of carbon dioxide with Mn(terpyridine)
 carbonyl complexes.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17179
_journal_page_last               17186
_journal_paper_doi               10.1039/c6dt03243e
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety
'C17 H11 Mn N3 O2, 2(C10 H20 K0.5 O4), C4 H8 O'
_chemical_formula_sum            'C41 H59 K Mn N3 O11'
_chemical_formula_weight         863.98
_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_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   direct
_audit_creation_date             2016-07-25
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-08-04 deposited with the CCDC.
2016-09-28 downloaded from the CCDC.
;
_cell_angle_alpha                78.713(4)
_cell_angle_beta                 86.471(4)
_cell_angle_gamma                85.761(4)
_cell_formula_units_Z            2
_cell_length_a                   9.3458(8)
_cell_length_b                   9.7583(9)
_cell_length_c                   23.585(2)
_cell_measurement_reflns_used    7901
_cell_measurement_temperature    100
_cell_measurement_theta_max      24.436
_cell_measurement_theta_min      2.318
_cell_volume                     2101.1(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX2'
_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  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.9965
_diffrn_measured_fraction_theta_max 0.9965
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0708
_diffrn_reflns_av_unetI/netI     0.0715
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            41885
_diffrn_reflns_theta_full        26.0000
_diffrn_reflns_theta_max         25.72
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    0.475
_exptl_absorpt_correction_T_max  0.5621
_exptl_absorpt_correction_T_min  0.5193
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0630 before and 0.0534 after correction.
The Ratio of minimum to maximum transmission is 0.9239.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.3655
_exptl_crystal_description       intense
_exptl_crystal_F_000             917.5658
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.3546
_refine_diff_density_min         -1.3055
_refine_diff_density_rms         0.1546
_refine_ls_d_res_high            0.8188
_refine_ls_d_res_low             11.5510
_refine_ls_goodness_of_fit_ref   1.0532
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    100
_refine_ls_number_parameters     525
_refine_ls_number_reflns         7983
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0532
_refine_ls_R_factor_all          0.1099
_refine_ls_R_factor_gt           0.0705
_refine_ls_shift/su_max          7.4509
_refine_ls_shift/su_mean         0.1666
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0967P)^2^+5.0577P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1735
_refine_ls_wR_factor_ref         0.2036
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              11
_reflns_limit_k_min              -11
_reflns_limit_l_max              28
_reflns_limit_l_min              0
_reflns_number_gt                5521
_reflns_number_total             7983
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c6dt03243e2.cif
_cod_data_source_block           Mnk3tpyCO2_K18Crown6_a
_cod_depositor_comments          'Adding full bibliography for 7040768.cif.'
_cod_database_code               7040768
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Others
 Fixed Sof: O14(0.5) O15(0.5) H30b(0.5) H30c(0.5) H30a(0.5) H30d(0.5)
 H31b(0.5) H31a(0.5) H31c(0.5) H31d(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C22(H22a,H22b), C23(H23a,H23b), C24(H24a,H24b), C25(H25a,H25b), C26(H26a,
 H26b), C27(H27a,H27b), C41(H41a,H41b), C42(H42a,H42b), C43(H43a,H43b),
 C44(H44a,H44b), C32(H32a,H32b), C33(H33a,H33b), C34(H34a,H34b), C35(H35a,H35b),
  C36(H36a,H36b), C37(H37a,H37b), C38(H38a,H38b), C39(H39a,H39b), C40(H40a,
 H40b), C45(H45a,H45b), C28(H28a,H28b), C29(H29a,H29b), C30(H30c,H30d),
 C30(H30a,H30b), C31(H31a,H31b), C31(H31c,H31d)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13),
 C14(H14), C15(H15)
;
_olex2_submission_special_instructions 'No special instructions were received'