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_1559727
_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 H48 B N4 O2 Pt, C32 H12 B F24'
_chemical_formula_sum            'C58 H60 B2 F24 N4 O2 Pt'
_chemical_formula_weight         1517.81
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                90
_cell_angle_beta                 109.711(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9627(11)
_cell_length_b                   24.4797(19)
_cell_length_c                   20.1924(16)
_cell_measurement_reflns_used    9786
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      21.959
_cell_measurement_theta_min      2.322
_cell_volume                     6497.4(9)
_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    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.990
_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  0.0699
_diffrn_reflns_av_unetI/netI     0.0450
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            134022
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         22.540
_diffrn_reflns_theta_min         1.814
_diffrn_source_current           0.6
_diffrn_source_power             0.03
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.239
_exptl_absorpt_correction_T_max  0.7448
_exptl_absorpt_correction_T_min  0.6170
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1001 before and 0.0641 after correction.
The Ratio of minimum to maximum transmission is 0.8284.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_description       block
_exptl_crystal_F_000             3024
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2CL2, pentane'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.536
_refine_diff_density_min         -1.106
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1092
_refine_ls_number_reflns         17211
_refine_ls_number_restraints     960
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0245P)^2^+11.4852P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0730
_refine_ls_wR_factor_ref         0.0813
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13211
_reflns_number_total             17211
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc05522k2.cif
_cod_data_source_block           4
_cod_depositor_comments
;Adding full bibliography for 1559727--1559730.cif.

 Adding full bibliography for 1559727--1559730.cif.
;
_cod_database_code               1559727
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.708
_shelx_estimated_absorpt_t_min   0.637
_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
 C21A-C23A \\sim C21A-C24A \\sim C21B-C23B \\sim C21B-C24B
 with sigma of 0.02
 C22A-C25A \\sim C22A-C26A \\sim C22B-C25B \\sim C22B-C26B
 with sigma of 0.02
 C23A-C24A \\sim C23B-C24B \\sim C25A-C26A \\sim C25B-C26B
 with sigma of 0.04
 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
 C34-F4A \\sim C34-F5A \\sim C34-F6A \\sim C34-F4B \\sim C34-F5B \\sim C34-F6B
 with sigma of 0.02
 F4A-F5A \\sim F4A-F6A \\sim F5A-F6A \\sim F4B-F5B \\sim F4B-F6B \\sim F5B-F6B
 with sigma of 0.02
 C42-F10A \\sim C42-F11A \\sim C42-F12A \\sim C42-F10B \\sim C42-F11B \\sim
C42-F12B
 with sigma of 0.02
 F10A-F11A \\sim F10A-F12A \\sim F11A-F12A \\sim F10B-F11B \\sim F10B-F12B
\\sim F11B-F12B
 with sigma of 0.02
 C49-F13A \\sim C49-F14A \\sim C49-F15A \\sim C49-F13B \\sim C49-F14B \\sim
C49-F15B
 with sigma of 0.02
 F13A-F14A \\sim F13A-F15A \\sim F14A-F15A \\sim F13B-F14B \\sim F13B-F15B
\\sim F14B-F15B
 with sigma of 0.02
 C50-F16A \\sim C50-F17A \\sim C50-F18A \\sim C50-F16B \\sim C50-F17B \\sim
C50-F18B
 with sigma of 0.02
 F16A-F17A \\sim F16A-F18A \\sim F17A-F18A \\sim F16B-F17B \\sim F16B-F18B
\\sim F17B-F18B
 with sigma of 0.02
 C57-F19A \\sim C57-F20A \\sim C57-F21A \\sim C57-F19B \\sim C57-F20B \\sim
C57-F21B
 with sigma of 0.02
 F19A-F20A \\sim F19A-F21A \\sim F20A-F21A \\sim F19B-F20B \\sim F19B-F21B
\\sim F20B-F21B
 with sigma of 0.02
 C58-F22A \\sim C58-F23A \\sim C58-F24A \\sim C58-F22B \\sim C58-F23B \\sim
C58-F24B
 with sigma of 0.02
 F22A-F23A \\sim F22A-F24A \\sim F23A-F24A \\sim F22B-F23B \\sim F22B-F24B
\\sim F23B-F24B
 with sigma of 0.02
3. Rigid bond restraints
 C21A, C23A, C24A, C21B, C23B, C24B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C22A, C25A, C26A, C22B, C25B, C26B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C33, F1A, F2A, F3A, F1B, F2B, F3B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C34, F4A, F5A, F6A, F4B, F5B, F6B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C42, F10A, F11A, F12A, F10B, F11B, F12B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C49, F13A, F14A, F15A, F13B, F14B, F15B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C50, F16A, F17A, F18A, F16B, F17B, F18B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C57, F19A, F20A, F21A, F19B, F20B, F21B
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C58, F22A, F23A, F24A, F22B, F23B, F24B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C21A \\sim C23A \\sim C24A \\sim C21B \\sim C23B \\sim C24B: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C22A \\sim C25A \\sim C26A \\sim C22B \\sim C25B \\sim C26B: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C33 \\sim F1A \\sim F2A \\sim F3A \\sim F1B \\sim F2B \\sim F3B: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C34 \\sim F4A \\sim F5A \\sim F6A \\sim F4B \\sim F5B \\sim F6B: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C42 \\sim F10A \\sim F11A \\sim F12A \\sim F10B \\sim F11B \\sim F12B: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C49 \\sim F13A \\sim F14A \\sim F15A \\sim F13B \\sim F14B \\sim F15B: within
2A with sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
C50 \\sim F16A \\sim F17A \\sim F18A \\sim F16B \\sim F17B \\sim F18B: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C57 \\sim F19A \\sim F20A \\sim F21A \\sim F19B \\sim F20B \\sim F21B: within
2A with sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
C58 \\sim F22A \\sim F23A \\sim F24A \\sim F22B \\sim F23B \\sim F24B: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
5. Others
 Sof(C21B)=Sof(C22B)=Sof(C23B)=Sof(H23D)=Sof(H23E)=Sof(H23F)=Sof(C24B)=
 Sof(H24D)=Sof(H24E)=Sof(H24F)=Sof(C25B)=Sof(H25D)=Sof(H25E)=Sof(H25F)=
 Sof(C26B)=Sof(H26D)=Sof(H26E)=Sof(H26F)=1-FVAR(1)
 Sof(C21A)=Sof(C22A)=Sof(C23A)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C24A)=
 Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C25A)=Sof(H25A)=Sof(H25B)=Sof(H25C)=
 Sof(C26A)=Sof(H26A)=Sof(H26B)=Sof(H26C)=FVAR(1)
 Sof(F1B)=Sof(F2B)=Sof(F3B)=1-FVAR(2)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=FVAR(2)
 Sof(F4B)=Sof(F5B)=Sof(F6B)=1-FVAR(3)
 Sof(F4A)=Sof(F5A)=Sof(F6A)=FVAR(3)
 Sof(F10B)=Sof(F11B)=Sof(F12B)=1-FVAR(4)
 Sof(F10A)=Sof(F11A)=Sof(F12A)=FVAR(4)
 Sof(F13B)=Sof(F14B)=Sof(F15B)=1-FVAR(5)
 Sof(F13A)=Sof(F14A)=Sof(F15A)=FVAR(5)
 Sof(F16B)=Sof(F17B)=Sof(F18B)=1-FVAR(6)
 Sof(F16A)=Sof(F17A)=Sof(F18A)=FVAR(6)
 Sof(F19B)=Sof(F20B)=Sof(F21B)=1-FVAR(7)
 Sof(F19A)=Sof(F20A)=Sof(F21A)=FVAR(7)
 Sof(F22A)=Sof(F23A)=Sof(F24A)=1-FVAR(8)
 Sof(F22B)=Sof(F23B)=Sof(F24B)=FVAR(8)
6.a Ternary CH refined with riding coordinates:
 C4(H4), C14(H14)
6.b Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C12(H12), C13(H13), 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:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C),
 C19(H19A,H19B,H19C), C23A(H23A,H23B,H23C), C24A(H24A,H24B,H24C), C25A(H25A,
 H25B,H25C), C26A(H26A,H26B,H26C), C23B(H23D,H23E,H23F), C24B(H24D,H24E,H24F),
 C25B(H25D,H25E,H25F), C26B(H26D,H26E,H26F)
;
_shelx_res_checksum              92192
_olex2_submission_special_instructions 'No special instructions were received'