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_1520531
_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         'C13 H8 Br Mn N2 O5'
_chemical_formula_sum            'C13 H8 Br Mn N2 O5'
_chemical_formula_weight         407.06
_chemical_properties_physical    Light-sensitive
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-04-16
_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                90
_cell_angle_beta                 98.591(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1341(2)
_cell_length_b                   13.1528(2)
_cell_length_c                   7.05370(10)
_cell_measurement_temperature    293(2)
_cell_volume                     1388.33(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega -110.00   15.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.0000  -68.0000    0.0000 125

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

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

  4 omega -110.00   15.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.0000  -30.0000   90.0000 125
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_orient_matrix_UB_11      -0.0182223000
_diffrn_orient_matrix_UB_12      0.0494488000
_diffrn_orient_matrix_UB_13      0.0049290000
_diffrn_orient_matrix_UB_21      -0.0411009000
_diffrn_orient_matrix_UB_22      -0.0171755000
_diffrn_orient_matrix_UB_23      -0.0516713000
_diffrn_orient_matrix_UB_31      -0.0150597000
_diffrn_orient_matrix_UB_32      -0.0129608000
_diffrn_orient_matrix_UB_33      0.0874083000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            20916
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.994
_diffrn_reflns_theta_min         2.061
_exptl_absorpt_coefficient_mu    3.854
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.948
_exptl_crystal_description       block
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.700
_refine_diff_density_min         -0.990
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         4417
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0359
_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^)+(0.0504P)^2^+1.3888P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0921
_refine_ls_wR_factor_ref         0.0962
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3815
_reflns_number_total             4417
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5fd00071h3.cif
_cod_data_source_block           test_a
_cod_database_code               1520531
_cell_oxdiff_angle_alpha         89.982(2)
_cell_oxdiff_angle_beta          98.561(2)
_cell_oxdiff_angle_gamma         90.004(3)
_cell_oxdiff_length_a            15.1282(5)
_cell_oxdiff_length_b            13.1529(4)
_cell_oxdiff_length_c            7.05592(19)
_cell_oxdiff_measurement_reflns_used 12996
_cell_oxdiff_volume              1388.33(7)
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.93
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C00C(H00C), C00D(H00D), C00G(H00G), C00H(H00H), C00I(H00I), C00M(H00M)
2.b Idealised tetrahedral OH refined as rotating group:
 O003(H003), O006(H006)
;
_shelx_res_checksum              9655
_shelx_hkl_checksum              80805
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'