Synergistic Effects of Imidazolium-Functionalization on fac-Mn(CO)<sub>3</sub> Bipyridine Catalyst Platforms for Electrocatalytic Carbon Dioxide Reduction.
Sung, Siyoung; Li, Xiaohui; Wolf, Lucienna M.; Meeder, Jeremy R.; Bhuvanesh, Nattamai S.; Grice, Kyle A.; Panetier, Julien A.; Nippe, Michael; Journal of the American Chemical Society 141 (2019) 6569–6582; doi:10.1021/jacs.8b13657

data_4128258
_publ_section_title
;
 Synergistic Effects of Imidazolium-Functionalization on
 fac-Mn(CO)<sub>3</sub> Bipyridine Catalyst Platforms for Electrocatalytic
 Carbon Dioxide Reduction.
;
_journal_issue                   16
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6569
_journal_page_last               6582
_journal_paper_doi               10.1021/jacs.8b13657
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C22 H23 Br Mn N4 O3, F6 P'
_chemical_formula_sum            'C22 H23 Br F6 Mn N4 O3 P'
_chemical_formula_weight         671.26
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-06-11
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_cell_angle_alpha                80.848(4)
_cell_angle_beta                 87.913(4)
_cell_angle_gamma                83.603(4)
_cell_formula_units_Z            4
_cell_length_a                   7.1504(6)
_cell_length_b                   13.4353(11)
_cell_length_c                   27.972(2)
_cell_measurement_reflns_used    9252
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      63.947
_cell_measurement_theta_min      3.201
_cell_volume                     2636.0(4)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.2074
_diffrn_reflns_av_unetI/netI     0.0980
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            41953
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        64.601
_diffrn_reflns_theta_max         64.601
_diffrn_reflns_theta_min         3.201
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.112
_exptl_absorpt_correction_T_max  0.4402
_exptl_absorpt_correction_T_min  0.2725
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1349 before and 0.0956 after correction. The Ratio of minimum to maximum transmission is 0.6190. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.691
_exptl_crystal_description       plate
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.204
_exptl_crystal_size_mid          0.182
_exptl_crystal_size_min          0.037
_refine_diff_density_max         2.848
_refine_diff_density_min         -2.188
_refine_diff_density_rms         0.276
_refine_ls_extinction_coef       0.0037(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.474
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     683
_refine_ls_number_reflns         8571
_refine_ls_number_restraints     1086
_refine_ls_restrained_S_all      1.400
_refine_ls_R_factor_all          0.1243
_refine_ls_R_factor_gt           0.1186
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3174
_refine_ls_wR_factor_ref         0.3350
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7989
_reflns_number_total             8571
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b13657_si_004.cif
_cod_data_source_block           sy04003
_cod_database_code               4128258
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.779
_shelx_estimated_absorpt_t_min   0.325
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.582(3)
 0.418(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(C8) = Uanis(C7)
Uanis(C20B) = Uanis(C22B)
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C12B(H12C,H12D)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C8(H8), C9(H9), C10(H10), C13(H13), C14(H14),
 C15(H15), C2B(H2B), C3B(H3B), C4B(H4B), C8B(H8B), C9B(H9B), C10B(H10B),
 C13B(H13B), C14B(H14B), C15B(H15B)
5.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,
 H19C), C6B(H6BA,H6BB,H6BC), C17B(H17D,H17E,H17F), C18B(H18D,H18E,H18F),
 C19B(H19D,H19E,H19F)
;
_shelx_res_checksum              86431
_shelx_hkl_checksum              33386
_olex2_submission_special_instructions 'No special instructions were received'