Interrogating heterobimetallic co-catalytic responses for the electrocatalytic reduction of CO2 using supramolecular assembly.
Machan, Charles W.; Kubiak, Clifford P.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 15942–15950; doi:10.1039/c6dt01956k

data_7039764
_publ_section_title
;
 Interrogating heterobimetallic co-catalytic responses for the
 electrocatalytic reduction of CO2 using supramolecular assembly.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15942
_journal_page_last               15950
_journal_paper_doi               10.1039/c6dt01956k
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C19 H18 Br Mn N4 O5, C2 H3 N'
_chemical_formula_sum            'C21 H21 Br Mn N5 O5'
_chemical_formula_weight         558.27
_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     direct
_audit_creation_date             2015-01-06
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.06 svn.r3119 for OlexSys, GUI svn.r4979)
;
_audit_update_record
;
2016-05-16 deposited with the CCDC.
2016-07-04 downloaded from the CCDC.
;
_cell_angle_alpha                101.163(6)
_cell_angle_beta                 95.668(5)
_cell_angle_gamma                112.647(5)
_cell_formula_units_Z            2
_cell_length_a                   8.4602(13)
_cell_length_b                   8.6080(15)
_cell_length_c                   17.623(3)
_cell_measurement_reflns_used    4953
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.339
_cell_measurement_theta_min      2.401
_cell_volume                     1140.5(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
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.9908
_diffrn_measured_fraction_theta_max 0.9908
_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  0.0685
_diffrn_reflns_av_unetI/netI     0.0667
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18832
_diffrn_reflns_theta_full        26.4107
_diffrn_reflns_theta_max         26.41
_diffrn_reflns_theta_min         2.40
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.373
_exptl_absorpt_correction_T_max  0.0932
_exptl_absorpt_correction_T_min  0.0565
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.1581 before and 0.0710 after correction.
The Ratio of minimum to maximum transmission is 0.6062.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_density_diffrn    1.6255
_exptl_crystal_description       plate
_exptl_crystal_F_000             564.3709
_exptl_crystal_preparation       'vapor diffusion of pentane into'
_exptl_crystal_recrystallization_method
'vapor diffusion of diethyl ether into acetonitrile solution'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.5595
_refine_diff_density_min         -0.6397
_refine_diff_density_rms         0.1431
_refine_ls_d_res_high            0.7989
_refine_ls_d_res_low             8.4848
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0295
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    34
_refine_ls_number_parameters     300
_refine_ls_number_reflns         4653
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0295
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0297P)^2^+0.2964P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0784
_refine_ls_wR_factor_ref         0.0856
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              10
_reflns_limit_k_min              -10
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                3660
_reflns_number_total             4653
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c6dt01956k2.cif
_cod_data_source_block           kub_CM33_0m
_cod_depositor_comments          'Adding full bibliography for 7039764.cif.'
_cod_database_code               7039764
_publcif_datablock.id            {84b85df4-16ec-4872-b1fd-0fe057f3ff67}
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C27(H27a,H27b), C30(H30a,H30b)
2.b Aromatic/amide H refined with riding coordinates:
 N12(H12), N8(H8), C19(H19), C14(H14), C18(H18), C23(H23), C24(H24), C17(H17)
2.c Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c), C32(H32a,H32b,H32c), C33(H33a,H33b,H33c)
;
_olex2_submission_special_instructions 'No special instructions were received'