An amide-based second coordination sphere promotes the dimer pathway of Mn-catalyzed CO2-to-CO reduction at low overpotential
Yang, Yong; Ertem, Mehmed Z.; Duan, Lele; Chemical Science 12 (2021) 4779–4788; doi:10.1039/D0SC05679K

data_1560369
_publ_section_title
;
 An amide-based second coordination sphere promotes the dimer pathway of
 Mn-catalyzed CO2-to-CO reduction at low overpotential
;
_journal_issue                   13
_journal_name_full               'Chemical Science'
_journal_page_first              4779
_journal_page_last               4788
_journal_paper_doi               10.1039/D0SC05679K
_journal_volume                  12
_journal_year                    2021
_chemical_formula_moiety         'C15 H11 Br Mn N3 O4'
_chemical_formula_sum            'C15 H11 Br Mn N3 O4'
_chemical_formula_weight         432.12
_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
_atom_sites_solution_primary     dual
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;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
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_audit_update_record
;
2019-10-08 deposited with the CCDC.	2021-02-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.266(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.650(4)
_cell_length_b                   9.121(4)
_cell_length_c                   16.456(6)
_cell_measurement_reflns_used    9847
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.507
_cell_measurement_theta_min      2.516
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_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
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_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker PHOTO 100 area detector'
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_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker PHOTO 100 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0835
_diffrn_reflns_av_unetI/netI     0.0455
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
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_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            27967
_diffrn_reflns_point_group_measured_fraction_full 0.999
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_diffrn_reflns_theta_full        25.242
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_diffrn_source                   'microfocus sealed X-ray tube'
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_exptl_crystal_colour_primary    orange
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_exptl_crystal_size_max          0.36
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_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         3618
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0287
_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^)+(0.0229P)^2^+1.2808P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0682
_refine_ls_wR_factor_ref         0.0709
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3185
_reflns_number_total             3618
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc05679k3.cif
_cod_data_source_block           cxy0701_0m
_cod_depositor_comments
'Adding full bibliography for 1560367--1560369.cif.'
_cod_database_code               1560369
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.772
_shelx_estimated_absorpt_t_min   0.374
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N3(H3), C1(H1), C2(H2), C3(H3A), C4(H4), C7(H7), C8(H8), C9(H9)
2.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C)
;
_olex2_submission_special_instructions 'No special instructions were received'