Oxidative addition of Bi-C bonds to Pt(0): reaction of Pt(PEt<sub>3</sub>)<sub>3</sub> with cyclic organobismuth compounds.
Shimada, Shigeru; Wang, Xiang-Bo; Tanaka, Masato; Chemical communications (Cambridge, England) 56 (2020) 15216–15219; doi:10.1039/d0cc07408j

data_7127501
_publ_section_title
;
 Oxidative addition of Bi-C bonds to Pt(0): reaction of
 Pt(PEt<sub>3</sub>)<sub>3</sub> with cyclic organobismuth compounds.
;
_journal_issue                   96
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              15216
_journal_page_last               15219
_journal_paper_doi               10.1039/d0cc07408j
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C30 H51 Bi Cl N P2 Pt'
_chemical_formula_sum            'C30 H51 Bi Cl N P2 Pt'
_chemical_formula_weight         927.17
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-11-02
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2020-11-10 deposited with the CCDC.	2020-11-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.378(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.278(2)
_cell_length_b                   14.7178(6)
_cell_length_c                   18.1372(7)
_cell_measurement_reflns_used    8909
_cell_measurement_temperature    93
_cell_measurement_theta_max      30.0390
_cell_measurement_theta_min      3.7260
_cell_volume                     3276.5(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      93
_diffrn_detector                 'PLATUS 200K area detector'
_diffrn_detector_area_resol_mean 5.811
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

 # Type Start End Width t~exp~ \w \q \k \f Frames
 1 \w -105.00 75.00 0.50 40.00 -- -15.00 45.00 0.00 360
 2 \w -105.00 75.00 0.50 40.00 -- -15.00 45.00 90.00 360
 3 \w -105.00 75.00 0.50 40.00 -- -15.00 45.00 180.00 360
 4 \w -105.00 75.00 0.50 40.00 -- -15.00 45.00 270.00 360
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0403550000
_diffrn_orient_matrix_UB_12      -0.0187686000
_diffrn_orient_matrix_UB_13      0.0241787000
_diffrn_orient_matrix_UB_21      -0.0205084000
_diffrn_orient_matrix_UB_22      0.0261421000
_diffrn_orient_matrix_UB_23      0.0294495000
_diffrn_orient_matrix_UB_31      -0.0359470000
_diffrn_orient_matrix_UB_32      -0.0358701000
_diffrn_orient_matrix_UB_33      0.0088126000
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2983
_diffrn_reflns_av_unetI/netI     0.3548
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.918
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            56399
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.918
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.723
_diffrn_reflns_theta_min         1.981
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              micromax007
_exptl_absorpt_coefficient_mu    9.827
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.20878
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.880
_exptl_crystal_description       prism
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.342
_refine_diff_density_min         -2.537
_refine_diff_density_rms         0.374
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.901
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         9364
_refine_ls_number_restraints     139
_refine_ls_restrained_S_all      0.898
_refine_ls_R_factor_all          0.1784
_refine_ls_R_factor_gt           0.0755
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0444P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1419
_refine_ls_wR_factor_ref         0.1577
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3993
_reflns_number_total             9364
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 2.6119\% 
 around [-0.54 -0.05 -0.84] (reciprocal) or [-0.82 -0.05 -0.57] (direct)
;
_cod_data_source_file            d0cc07408j2.cif
_cod_data_source_block           Complex-6a
_cod_original_cell_volume        3276.6(6)
_cod_database_code               7127501
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C30H51BiClNP2Pt
_chemical_oxdiff_usercomment     tBuBismocine-PtCl(PEt3)2
_shelx_estimated_absorpt_t_max   0.828
_shelx_estimated_absorpt_t_min   0.546
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C27-C28A = C29-C30A
 1.53 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8)
\\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15) \\sim Ueq,
Uanis(C16) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C22)
\\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C27) \\sim Ueq,
Uanis(C29) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.1
Uanis(C21) = Uanis(C22)
Uanis(C23) = Uanis(C24)
Uanis(C25) = Uanis(C26)
Uanis(C27) = Uanis(C28A) = Uanis(C28B)
Uanis(C29) = Uanis(C30A) = Uanis(C30B)
4. Same fragment restrains
{P2, C27, C28A} sigma for 1-2: 0.02, 1-3: 0.04
{P2, C27, C28B} sigma for 1-2: 0.02, 1-3: 0.04
{P2, C29, C30A} sigma for 1-2: 0.02, 1-3: 0.04
{P2, C29, C30B} sigma for 1-2: 0.02, 1-3: 0.04
as in
{P2, C25, C26}
5. Others
 Sof(H27C)=Sof(H27D)=Sof(C28B)=Sof(H28D)=Sof(H28E)=Sof(H28F)=1-FVAR(1)
 Sof(H27A)=Sof(H27B)=Sof(C28A)=Sof(H28A)=Sof(H28B)=Sof(H28C)=FVAR(1)
 Sof(H29C)=Sof(H29D)=Sof(C30B)=Sof(H30D)=Sof(H30E)=Sof(H30F)=1-FVAR(2)
 Sof(H29A)=Sof(H29B)=Sof(C30A)=Sof(H30A)=Sof(H30B)=Sof(H30C)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C27(H27A,H27B), C27(H27C,H27D), C29(H29A,H29B), C29(H29C,
 H29D), C7(H7A,H7B), C8(H8A,H8B), C19(H19A,H19B), C21(H21A,H21B), C23(H23A,H23B)
6.b Me refined with riding coordinates:
 C26(H26A,H26B,H26C), C28B(H28D,H28E,H28F), C28A(H28A,H28B,H28C), C30B(H30D,
 H30E,H30F), C30A(H30A,H30B,H30C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C),
 C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C24(H24A,H24B,
 H24C)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C10(H10), C11(H11), C12(H12), C13(H13)
;
_shelx_res_checksum              28036
_shelx_hkl_checksum              82812
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.719
_oxdiff_exptl_absorpt_empirical_full_min 0.442
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2