FDCDU15 - Carbon Dioxide Utilisation: Improving the efficiency of electrochemical CO2 reduction using immobilized manganese complexes
Walsh, James J.; Smith, Charlotte L.; Neri, Gaia; Whitehead, George F. S.; Robertson, Craig M.; Cowan, Alexander J.; Faraday Discuss.  (2015) –; doi:10.1039/C5FD00071H

data_1520532
_publ_section_title
;
 FDCDU15 - Carbon Dioxide Utilisation: Improving the efficiency of
 electrochemical CO2 reduction using immobilized manganese complexes
;
_journal_name_full               'Faraday Discuss.'
_journal_paper_doi               10.1039/C5FD00071H
_journal_year                    2015
_chemical_formula_moiety         'C15 H8 Br Mn N2 O7, 2(C4 H8 O), H2 O'
_chemical_formula_sum            'C23 H26 Br Mn N2 O10'
_chemical_formula_weight         625.31
_chemical_properties_physical    Light-sensitive
_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             2015-04-17
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-04-23 deposited with the CCDC.
2015-06-11 downloaded from the CCDC.
;
_cell_angle_alpha                102.912(3)
_cell_angle_beta                 95.846(2)
_cell_angle_gamma                98.607(2)
_cell_formula_units_Z            2
_cell_length_a                   6.52291(18)
_cell_length_b                   13.1864(4)
_cell_length_c                   16.0537(4)
_cell_measurement_reflns_used    9433
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.3960
_cell_measurement_theta_min      1.8050
_cell_volume                     1317.59(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega -110.00   15.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.0000  -68.0000    0.0000 125

  2 omega -110.00   15.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.0000  -68.0000  120.0000 125

  3 omega -110.00   15.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.0000  -68.0000  240.0000 125

  4 omega -110.00   15.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.0000  -30.0000   90.0000 125
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0003214000
_diffrn_orient_matrix_UB_12      -0.0246563000
_diffrn_orient_matrix_UB_13      0.0350038000
_diffrn_orient_matrix_UB_21      0.0012084000
_diffrn_orient_matrix_UB_22      -0.0492446000
_diffrn_orient_matrix_UB_23      -0.0287525000
_diffrn_orient_matrix_UB_31      0.1110715000
_diffrn_orient_matrix_UB_32      0.0105798000
_diffrn_orient_matrix_UB_33      0.0066395000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_unetI/netI     0.0473
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15112
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         2.313
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.074
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88776
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.576
_exptl_crystal_description       block
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.513
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         5384
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0396
_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^)+(0.0364P)^2^+0.9585P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0810
_refine_ls_wR_factor_ref         0.0863
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4404
_reflns_number_total             5384
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5fd00071h2.cif
_cod_data_source_block           c1_mnpycooh
_cod_original_cell_volume        1317.58(7)
_cod_database_code               1520532
_chemical_oxdiff_formula         'Mn1 Br1 N2 O7 C12 H12'
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.31
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 O4-C1
 1.145 with sigma of 0.001
 C1-Mn02
 1.78 with sigma of 0.001
3. Others
 Sof(Br1)=Sof(C1)=Sof(O4)=1-FVAR(1)
 Sof(Br01)=Sof(O00B)=Sof(C00G)=FVAR(1)
 Fixed Uiso: O4(0.03)
4.a Free rotating group:
 O00E(H00R,H00T)
4.b Secondary CH2 refined with riding coordinates:
 C00T(H00G,H00H), C00U(H00J,H00K), C00V(H00A,H00B), C00W(H00C,H00D), C00Y(H00E,
 H00F), C00Z(H00M,H00N), C011(H01A,H01B)
4.c Aromatic/amide H refined with riding coordinates:
 C00I(H00I), C00L(H00L), C00O(H00O), C00P(H00P), C00Q(H00Q), C00S(H00S)
4.d Idealised tetrahedral OH refined as rotating group:
 O003(H003), O005(H005)
;
_shelx_res_checksum              44815
_shelx_hkl_checksum              28587
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'