Reversible carbon-boron bond formation at platinum centers through σ-BH complexes.
Ríos, Pablo; Martín-de la Calle, Rocío; Vidossich, Pietro; Fernández-de-Córdova, Francisco José; Lledós, Agustí; Conejero, Salvador; Chemical science 12 (2020) 1647–1655; doi:10.1039/d0sc05522k

data_1559729
_publ_section_title
;
 Reversible carbon-boron bond formation at platinum centers through \s-BH
 complexes.
;
_journal_issue                   5
_journal_name_full               'Chemical science'
_journal_page_first              1647
_journal_page_last               1655
_journal_paper_doi               10.1039/d0sc05522k
_journal_volume                  12
_journal_year                    2020
_chemical_formula_moiety         'C26 H42 B N6 Pt, C32 H12 B F24'
_chemical_formula_sum            'C58 H54 B2 F24 N6 Pt'
_chemical_formula_weight         1507.78
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-09-08
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2020-09-25 deposited with the CCDC.	2020-11-10 downloaded from the CCDC.
;
_cell_angle_alpha                96.145(3)
_cell_angle_beta                 98.035(3)
_cell_angle_gamma                91.631(3)
_cell_formula_units_Z            2
_cell_length_a                   12.8046(7)
_cell_length_b                   13.6804(7)
_cell_length_c                   18.4265(10)
_cell_measurement_reflns_used    9928
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.99
_cell_measurement_theta_min      2.37
_cell_volume                     3174.7(3)
_computing_cell_refinement       'SAINT V8.18C (?, 2016)'
_computing_data_reduction        'SAINT V8.18C (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56086
_diffrn_reflns_av_R_equivalents  0.0653
_diffrn_reflns_av_unetI/netI     0.0827
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            89536
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         25.801
_diffrn_reflns_theta_min         1.696
_diffrn_source_current           0.6
_diffrn_source_power             0.03
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.267
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6748
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0863 before and 0.0604 after correction.
The Ratio of minimum to maximum transmission is 0.9054.
The \l/2 correction factor is 0.0000.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_description       block
_exptl_crystal_F_000             1496
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2CL2, pentane'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.246
_refine_diff_density_min         -1.562
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     897
_refine_ls_number_reflns         24625
_refine_ls_number_restraints     324
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0438
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0341P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0819
_refine_ls_wR_factor_ref         0.0888
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19247
_reflns_number_total             24625
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc05522k2.cif
_cod_data_source_block           3
_cod_depositor_comments
;Adding full bibliography for 1559727--1559730.cif.

 Adding full bibliography for 1559727--1559730.cif.
;
_cod_database_code               1559729
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.813
_shelx_estimated_absorpt_t_min   0.742
_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. Restrained distances
 C33-F1A \\sim C33-F2A \\sim C33-F3A \\sim C33-F1B \\sim C33-F2B \\sim C33-F3B
 with sigma of 0.02
 F1A-F2A \\sim F1A-F3A \\sim F2A-F3A \\sim F1B-F2B \\sim F1B-F3B \\sim F2B-F3B
 with sigma of 0.02
 C41-F7A \\sim C41-F8A \\sim C41-F9A \\sim C41-F7B \\sim C41-F8B \\sim C41-F9B
 with sigma of 0.02
 F7A-F8A \\sim F7A-F9A \\sim F8A-F9A \\sim F7B-F8B \\sim F7B-F9B \\sim F8B-F9B
 with sigma of 0.02
3. Rigid bond restraints
 C57, F21, F20, F19
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C33, F3B, F2A, F1B, F3A, F2B, F1A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C41, F7A, F8A, F9A, F7B, F8B, F9B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C58, F22, F23, F24
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C57 \\sim F20 \\sim F19 \\sim F21: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.7A
C33 \\sim F3B \\sim F2A \\sim F1B \\sim F3A \\sim F2B \\sim F1A: within 1.7A
with sigma of 0.005 and sigma for terminal atoms of 0.01 within 1.7A
C41 \\sim F7A \\sim F8A \\sim F9A \\sim F7B \\sim F8B \\sim F9B: within 2A with
sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
C58 \\sim F22 \\sim F23 \\sim F24: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
Uanis(F21) \\sim Ueq, Uanis(F20) \\sim Ueq, Uanis(F19) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.005
Uanis(F3B) \\sim Ueq, Uanis(F2A) \\sim Ueq, Uanis(F1B) \\sim Ueq, Uanis(F3A)
\\sim Ueq, Uanis(F2B) \\sim Ueq, Uanis(F1A) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.02
5. Others
 Sof(F1B)=Sof(F2B)=Sof(F3B)=1-FVAR(1)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=FVAR(1)
 Sof(F7B)=Sof(F8B)=Sof(F9B)=1-FVAR(2)
 Sof(F7A)=Sof(F8A)=Sof(F9A)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C14(H14), C24(H24)
6.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C18(H18), C19(H19), C28(H28),
 C30(H30), C32(H32), C36(H36), C38(H38), C40(H40), C44(H44), C46(H46), C48(H48),
  C52(H52), C54(H54), C56(H56)
6.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C25(H25A,
 H25B,H25C), C26(H26A,H26B,H26C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              44557
_shelx_fab_checksum              85132
_olex2_submission_special_instructions 'No special instructions were received'