Spin-state crossover in photo-catalyzed nitrile dihydroboration via Mn-thiolate cooperation
Elsby, Matthew R.; Oh, Changjin; Son, Mina; Kim, Scott Y. H.; Baik, Mu-Hyun; Baker, R. Tom; Chemical Science 13 (2022) 12550–12559; doi:10.1039/D2SC04339D

data_1567819
_publ_section_title
;
 Spin-state crossover in photo-catalyzed nitrile dihydroboration via
 Mn-thiolate cooperation
;
_journal_issue                   42
_journal_name_full               'Chemical Science'
_journal_page_first              12550
_journal_page_last               12559
_journal_paper_doi               10.1039/D2SC04339D
_journal_volume                  13
_journal_year                    2022
_chemical_formula_moiety         'C40 H40 Mn N4 S4, C4 H7 O'
_chemical_formula_sum            'C44 H47 Mn N4 O S4'
_chemical_formula_weight         831.03
_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     iterative
_audit_block_doi                 10.5517/ccdc.csd.cc2756h4
_audit_creation_date             2021-01-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-02-02 deposited with the CCDC.	2022-09-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.000(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8594(10)
_cell_length_b                   19.0914(13)
_cell_length_c                   16.2268(11)
_cell_measurement_reflns_used    9652
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      30.57
_cell_measurement_theta_min      2.58
_cell_volume                     4183.5(5)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      200.05
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0565
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            117743
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.684
_diffrn_reflns_theta_min         1.672
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.554
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5490
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1237 before and 0.0700 after correction. The Ratio of minimum to maximum transmission is 0.7358. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_description       block
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.37
_refine_diff_density_max         0.570
_refine_diff_density_min         -1.023
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         12917
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0468
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0740P)^2^+1.6834P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1225
_refine_ls_wR_factor_ref         0.1375
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10176
_reflns_number_total             12917
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc04339d2.cif
_cod_data_source_block           s0526_0m_a
_cod_depositor_comments
'Adding full bibliography for 1567818--1567819.cif.'
_cod_database_code               1567819
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.821
_shelx_estimated_absorpt_t_min   0.781
_olex2_refinement_description
;
1. 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
2.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C23(H23A,H23B), C42(H42A,H42B), C41(H41A,H41B), C43(H43A,H43B)
2.b Aromatic/amide H refined with riding coordinates:
 C20(H20), C40(H40), C17(H17), C19(H19), C5(H5), C18(H18), C25(H25), C39(H39),
 C2(H2), C10(H10), C4(H4), C37(H37), C3(H3), C13(H13), C31(H31), C38(H38),
 C26(H26), C28(H28), C12(H12), C27(H27), C11(H11), C34(H34), C33(H33), C32(H32),
  C44(H44)
2.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C22(H22A,H22B,H22C), C15(H15A,H15B,H15C), C30(H30A,H30B,H30C)
;
_shelx_res_checksum              98770
_olex2_submission_original_sample_id Mn(bis-amido)bpy
_olex2_submission_special_instructions 'No special instructions were received'