Two active species from a single metal halide precursor: a case study of highly productive Mn-catalyzed dehydrogenation of amine-boranes <i>via</i> intermolecular bimetallic cooperation.
Gulyaeva, Ekaterina S.; Osipova, Elena S.; Kovalenko, Sergey A.; Filippov, Oleg A.; Belkova, Natalia V.; Vendier, Laure; Canac, Yves; Shubina, Elena S.; Valyaev, Dmitry A.; Chemical science 15 (2024) 1409–1417; doi:10.1039/d3sc05356c

data_1570527
_publ_section_title
;
 Two active species from a single metal halide precursor: a case study of
 highly productive Mn-catalyzed dehydrogenation of amine-boranes
 <i>via</i> intermolecular bimetallic cooperation.
;
_journal_issue                   4
_journal_name_full               'Chemical science'
_journal_page_first              1409
_journal_page_last               1417
_journal_paper_doi               10.1039/d3sc05356c
_journal_volume                  15
_journal_year                    2024
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C30 H31 Mn N5 O3, B F4'
_chemical_formula_sum            'C30 H31 B F4 Mn N5 O3'
_chemical_formula_weight         651.35
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-03-13T14:45:19-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2023-05-11 deposited with the CCDC.	2023-12-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.9120(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.6994(2)
_cell_length_b                   8.04650(10)
_cell_length_c                   33.4683(2)
_cell_measurement_reflns_used    26413
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      71.3890
_cell_measurement_theta_min      3.7830
_cell_measurement_wavelength     1.54184
_cell_volume                     6287.04(10)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SIR2014 (Burla et al., 1994)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_unetI/netI     0.0176
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            59479
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.493
_diffrn_reflns_theta_min         5.005
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.961
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70919
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2688
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: MeCN/Et2O'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.651
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         6105
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0589P)^2^+5.1309P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1003
_refine_ls_wR_factor_ref         0.1023
_reflns_Friedel_coverage         0
_reflns_number_gt                5757
_reflns_number_total             6105
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc05356c3.cif
_cod_data_source_block           complex_[3MeCN](BF4)
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 1570527--1570528.cif.
;
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               1570527
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              4355
_shelx_hkl_checksum              99034