Manganese(I)-catalyzed dehydrogenative borylation of terminal alkynes.
Ghanwat, Pratiksha B.; Bora, Debashree; Pandya, Rinu; Vanka, Kumar; Saha, Biswajit; Sen, Sakya S.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 10426–10432; doi:10.1039/d5dt00577a

data_7718835
_publ_section_title
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 Manganese(I)-catalyzed dehydrogenative borylation of terminal alkynes.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10426
_journal_page_last               10432
_journal_paper_doi               10.1039/d5dt00577a
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C23 H16 Br Fe Mn N2 O3, C H2 Cl2'
_chemical_formula_sum            'C24 H18 Br Cl2 Fe Mn N2 O3'
_chemical_formula_weight         644.00
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-09-19
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
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2025-02-01 deposited with the CCDC.	2025-05-27 downloaded from the CCDC.
;
_cell_angle_alpha                112.6020(10)
_cell_angle_beta                 91.100(2)
_cell_angle_gamma                109.359(3)
_cell_formula_units_Z            2
_cell_length_a                   9.6556(12)
_cell_length_b                   10.7004(12)
_cell_length_c                   13.2591(16)
_cell_measurement_reflns_used    4205
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      0.687
_cell_measurement_theta_min      0.633
_cell_volume                     1176.2(2)
_computing_cell_refinement       'APEX2 v2010.7-0 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service v2010.7.0.0'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1165
_diffrn_reflns_av_unetI/netI     0.0869
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            43888
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.661
_diffrn_reflns_theta_min         2.159
_exptl_absorpt_coefficient_mu    3.110
_exptl_absorpt_correction_T_max  28.661
_exptl_absorpt_correction_T_min  2.159
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.818
_exptl_crystal_description       block
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.765
_refine_diff_density_min         -1.108
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         5964
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0841
_refine_ls_R_factor_gt           0.0465
_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^)+(0.0382P)^2^+1.1976P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0963
_refine_ls_wR_factor_ref         0.1104
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4205
_reflns_number_total             5964
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00577a2.cif
_cod_data_source_block           ex_db_118_0m_a
_cod_depositor_comments          'Adding full bibliography for 7718835.cif.'
_cod_database_code               7718835
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.707
_shelx_estimated_absorpt_t_min   0.653
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C10(H10), C14(H14), C15(H15),
 C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23)
;
_shelx_res_checksum              79064
_shelx_hkl_checksum              13407
_olex2_submission_special_instructions 'No special instructions were received'