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_1560368
_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         'C16 H13 Br Mn N3 O4'
_chemical_formula_sum            'C16 H13 Br Mn N3 O4'
_chemical_formula_weight         446.14
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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)
;
_audit_update_record
;
2019-12-06 deposited with the CCDC.	2021-02-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.0480(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5955(4)
_cell_length_b                   10.5011(4)
_cell_length_c                   15.0027(6)
_cell_measurement_reflns_used    9959
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.37
_cell_volume                     1665.10(11)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.03
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_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 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  0.0393
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            26780
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
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_diffrn_source                   'microfocus sealed X-ray tube'
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_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.219
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_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0794 before and 0.0496 after correction. The Ratio of minimum to maximum transmission is 0.8169. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.780
_exptl_crystal_description       block
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
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_refine_diff_density_max         0.381
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       0.0016(3)
_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   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         3848
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0227
_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^)+(0.0190P)^2^+1.4295P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0491
_refine_ls_wR_factor_ref         0.0515
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3407
_reflns_number_total             3848
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc05679k3.cif
_cod_data_source_block           cxy0649_0m
_cod_depositor_comments
'Adding full bibliography for 1560367--1560369.cif.'
_cod_database_code               1560368
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.565
_shelx_estimated_absorpt_t_min   0.466
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C11(H11), C12(H12), C13(H13), C14(H14)
2.b Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              45215
_shelx_hkl_checksum              86374
_olex2_submission_special_instructions 'No special instructions were received'