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_1559728
_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   geom
_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                77.056(3)
_cell_angle_beta                 83.793(3)
_cell_angle_gamma                71.134(3)
_cell_formula_units_Z            4
_cell_length_a                   17.7840(10)
_cell_length_b                   19.3314(12)
_cell_length_c                   19.4985(12)
_cell_measurement_reflns_used    9983
_cell_measurement_temperature    99.99
_cell_measurement_theta_max      24.05
_cell_measurement_theta_min      2.49
_cell_volume                     6177.4(7)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      99.99
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56086
_diffrn_reflns_av_R_equivalents  0.0671
_diffrn_reflns_av_unetI/netI     0.0875
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            140866
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         24.105
_diffrn_reflns_theta_min         1.649
_diffrn_source_current           0.6
_diffrn_source_power             0.03
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.302
_exptl_absorpt_correction_T_max  0.7450
_exptl_absorpt_correction_T_min  0.6256
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1128 before and 0.0597 after correction.
The Ratio of minimum to maximum transmission is 0.8397.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_description       prism
_exptl_crystal_F_000             2992
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2CL2, pentane'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         7.006
_refine_diff_density_min         -4.131
_refine_diff_density_rms         0.189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1799
_refine_ls_number_reflns         39747
_refine_ls_number_restraints     486
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.1031
_refine_ls_R_factor_gt           0.0600
_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^)+(0.0731P)^2^+16.4641P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1401
_refine_ls_wR_factor_ref         0.1624
_reflns_Friedel_coverage         0.000
_reflns_number_gt                26520
_reflns_number_total             39747
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc05522k2.cif
_cod_data_source_block           2
_cod_depositor_comments
;Adding full bibliography for 1559727--1559730.cif.

 Adding full bibliography for 1559727--1559730.cif.
;
_cod_database_code               1559728
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.870
_shelx_estimated_absorpt_t_min   0.696
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C75-F13
 1.27 with sigma of 0.02
 C75-F14
 1.29 with sigma of 0.02
 C75-F15
 1.36 with sigma of 0.02
 C116-F48
 1.36 with sigma of 0.02
 C116-F46
 1.29 with sigma of 0.02
 C116-F47
 1.27 with sigma of 0.02
 C59-F3 \\sim C59-F2 \\sim C59-F1
 with sigma of 0.02
 F3-F2 \\sim F2-F1 \\sim F1-F3
 with sigma of 0.03
 C75-F14 \\sim C75-F15 \\sim C75-F13
 with sigma of 0.02
 F14-F15 \\sim F15-F13 \\sim F13-F14
 with sigma of 0.03
 F46-F48 \\sim F48-F47 \\sim F47-F46
 with sigma of 0.03
 C116-F46 \\sim C116-F48 \\sim C116-F47
 with sigma of 0.02
3. Rigid bond restraints
 C59, F2, F3A, F1, F2A, F3, F1A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C75, F13A, F15, F14A, F13, F15A, F14
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C68, F11, F10A, F12, F11A, F10, F12A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C67, F9, F7A, F8, F9A, F7, F8A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C116, F48A, F46, F47A, F48, F46A, F47
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C84, F23, F22, F24
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C107, F41, F42, F40
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C59 \\sim F2 \\sim F3A \\sim F1 \\sim F2A \\sim F3 \\sim F1A: within 1.7A with
sigma of 0.001 and sigma for terminal atoms of 0.002 within 1.7A
C75 \\sim F13A \\sim F15 \\sim F14A \\sim F13 \\sim F15A \\sim F14: within 1.7A
with sigma of 0.005 and sigma for terminal atoms of 0.01 within 1.7A
C68 \\sim F11 \\sim F10A \\sim F12 \\sim F11A \\sim F10 \\sim F12A: within 1.7A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
C67 \\sim F7 \\sim F9A \\sim F8 \\sim F7A \\sim F9 \\sim F8A: within 1.7A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
C116 \\sim F48A \\sim F46 \\sim F47A \\sim F48 \\sim F46A \\sim F47: within
1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
C107 \\sim F41 \\sim F42 \\sim F40: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.7A
C84 \\sim F23 \\sim F22 \\sim F24: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.7A
5. Others
 Sof(F11A)=Sof(F12A)=Sof(F10A)=1-FVAR(1)
 Sof(F10)=Sof(F12)=Sof(F11)=FVAR(1)
 Sof(F3A)=Sof(F2A)=Sof(F1A)=1-FVAR(2)
 Sof(F3)=Sof(F2)=Sof(F1)=FVAR(2)
 Sof(F13A)=Sof(F14A)=Sof(F15A)=1-FVAR(3)
 Sof(F14)=Sof(F15)=Sof(F13)=FVAR(3)
 Sof(F7A)=Sof(F8A)=Sof(F9A)=1-FVAR(4)
 Sof(F9)=Sof(F7)=Sof(F8)=FVAR(4)
 Sof(F46A)=Sof(F48A)=Sof(F47A)=1-FVAR(5)
 Sof(F46)=Sof(F48)=Sof(F47)=FVAR(5)
6.a Ternary CH refined with riding coordinates:
 C14(H14), C30(H30), C4(H4), C40(H40)
6.b Aromatic/amide H refined with riding coordinates:
 N5(H5), N12(H12A), N11(H11), C78(H78), N6(H6), C102(H102), C98(H98), C86(H86),
  C82(H82), C94(H94), C110(H110), C28(H28), C13(H13), C90(H90), C104(H104),
 C58(H58), C80(H80), C114(H114), C88(H88), C66(H66), C12(H12), C106(H106),
 C26(H26), C96(H96), C112(H112), C49(H49), C74(H74), C29(H29), C70(H70),
 C38(H38), C62(H62), C3(H3), C64(H64), C50(H50), C2(H2), C25(H25), C56(H56),
 C72(H72), C52(H52), C39(H39), C54(H54), C23(H23), C24(H24), C51(H51)
6.c Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C32(H32A,H32B,H32C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C),
 C34(H34A,H34B,H34C), C44(H44A,H44B,H44C), C16(H16A,H16B,H16C), C35(H35A,H35B,
 H35C), C19(H19A,H19B,H19C), C18(H18A,H18B,H18C), C10(H10A,H10B,H10C), C15(H15A,
 H15B,H15C), C31(H31A,H31B,H31C), C41(H41A,H41B,H41C), C5(H5A,H5B,H5C),
 C20(H20A,H20B,H20C), C45(H45A,H45B,H45C), C6(H6A,H6B,H6C), C42(H42A,H42B,H42C),
  C46(H46A,H46B,H46C)
;
_shelx_res_checksum              56395
_olex2_submission_special_instructions 'No special instructions were received'