Efficient and selective hydroboration of alkenes catalyzed by an air-stable (PP<sup>CF3</sup>P)CoI<sub>2</sub> precatalyst.
Fitzsimmons, Matthew C.; Seith, Maria C.; Moore, Curtis E.; Thomas, Christine M.; Chemical science 16 (2025) 5717–5725; doi:10.1039/d4sc08818b

data_1573994
_publ_section_title
;
 Efficient and selective hydroboration of alkenes catalyzed by an
 air-stable (PP<sup>CF3</sup>P)CoI<sub>2</sub> precatalyst.
;
_journal_issue                   13
_journal_name_full               'Chemical science'
_journal_page_first              5717
_journal_page_last               5725
_journal_paper_doi               10.1039/d4sc08818b
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C47 H41 Co F3 N2 P3, 2[C4H8O]'
_chemical_formula_sum            'C55 H57 Co F3 N2 O2 P3'
_chemical_formula_weight         986.86
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-07-15
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-09-06 deposited with the CCDC.	2025-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.0754(15)
_cell_length_b                   12.3634(8)
_cell_length_c                   34.026(2)
_cell_measurement_reflns_used    9563
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      25.173
_cell_measurement_theta_min      2.205
_cell_volume                     10128.0(11)
_computing_cell_refinement       'SAINT v8.40B (Bruker, 2021)'
_computing_data_collection       'APEX3 v2021.10-0 (Bruker, 2021)'
_computing_data_reduction        'SAINT v8.40B (Bruker, 2021)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker Photon III area detector'
_diffrn_detector_area_resol_mean 10.5
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Double Bounce Multilayer Mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0943
_diffrn_reflns_av_unetI/netI     0.0644
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            148292
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.387
_diffrn_reflns_theta_min         1.794
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_current           50.0
_diffrn_source_power             2.5
_diffrn_source_type              'Bruker TXS'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.487
_exptl_absorpt_correction_T_max  0.0911
_exptl_absorpt_correction_T_min  0.0686
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1222 before and 0.0660 after correction.
The Ratio of minimum to maximum transmission is 0.7530.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_description       plate
_exptl_crystal_F_000             4128
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: pentane'
_exptl_crystal_size_max          0.105
_exptl_crystal_size_mid          0.099
_exptl_crystal_size_min          0.039
_refine_diff_density_max         0.466
_refine_diff_density_min         -0.320
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.420(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1018
_refine_ls_number_reflns         18568
_refine_ls_number_restraints     925
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0451
_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^)+(0.0466P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0911
_refine_ls_wR_factor_ref         0.0986
_reflns_Friedel_coverage         0.962
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                13678
_reflns_number_total             18568
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc08818b2.cif
_cod_data_source_block           Thomas_MCF-4-29
_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 1573992--1573994.cif.
;
_cod_original_cell_volume        10127.9(12)
_cod_database_code               1573994
_shelx_shelxl_version_number     2019/1
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.580(15)
 0.420(15)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Restrained distances
 Co1'-HA = Co1-H
 1.5 with sigma of 0.02
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5.a Ternary CH refined with riding coordinates:
 C2(H2), C2'(H2')
5.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C10(H10A,H10B), C11(H11A,H11B), C1'(H1'A,H1'B), C10'(H10C,H10D),
 C11'(H11C,H11D)
5.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C14(H14), C15(H15), C16(H16),
 C17(H17), C20(H20), C21(H21), C22(H22), C23(H23), C25(H25), C26(H26), C27(H27),
  C28(H28), C29(H29), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35),
 C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C43(H43), C44(H44), C45(H45),
  C46(H46), C47(H47), C4'(H4'), C5'(H5'), C6'(H6'), C7'(H7'), C8'(H8'),
 C14'(H14'), C15'(H15'), C16'(H16'), C17'(H17'), C20'(H20'), C21'(H21'),
 C22'(H22'), C23'(H23'), C25'(H25'), C26'(H26'), C27'(H27'), C28'(H28'),
 C29'(H29'), C31'(H31'), C32'(H32'), C33'(H33'), C34'(H34'), C35'(H35'),
 C37'(H37'), C38'(H38'), C39'(H39'), C40'(H40'), C41'(H41'), C43'(H43'),
 C44'(H44'), C45'(H45'), C46'(H46'), C47'(H47')
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 698 electrons were 
found in a volume of 3084\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 2[C4H8O] per 
formula unit which account for 640 electrons per unit 
cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              38487
_shelx_fab_checksum              8319
_olex2_submission_special_instructions 'No special instructions were received'