Intramolecular transcyclometallation: the exchange of an aryl-Pt bond for an alkyl-Pt bond via an agostic intermediate
Paul A. Shaw; Jessica M. Phillips; Christopher P. Newman; Guy J. Clarkson; Jonathan P. Rourke; Chem.Commun. 51 (2015) 8365–; doi:10.1039/C5cc02355F

data_7117136
_publ_section_title
;
 Intramolecular transcyclometallation: the exchange of an aryl-Pt bond for
 an alkyl-Pt bond via an agostic intermediate
;
_journal_coden_Cambridge         182
_journal_name_full               Chem.Commun.
_journal_page_first              8365
_journal_paper_doi               10.1039/C5cc02355F
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C29 H36 Cl2 F2 N P Pt, 0.5(C H Cl3)'
_chemical_formula_sum            'C29.5 H36.5 Cl3.5 F2 N P Pt'
_chemical_formula_weight         793.23
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-01-15
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2853 for OlexSys, GUI svn.r4736)
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_audit_update_record
;
2015-03-20 deposited with the CCDC.
2015-04-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.9490(14)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   42.5003(7)
_cell_length_b                   8.95573(17)
_cell_length_c                   15.7762(2)
_cell_measurement_reflns_used    19288
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.5250
_cell_measurement_theta_min      3.4550
_cell_volume                     5996.80(17)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.2833
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0156550000
_diffrn_orient_matrix_UB_12      0.0049794000
_diffrn_orient_matrix_UB_13      -0.0176264000
_diffrn_orient_matrix_UB_21      0.0030077000
_diffrn_orient_matrix_UB_22      0.0736949000
_diffrn_orient_matrix_UB_23      -0.0139820000
_diffrn_orient_matrix_UB_31      0.0050131000
_diffrn_orient_matrix_UB_32      -0.0286790000
_diffrn_orient_matrix_UB_33      -0.0389733000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.918
_diffrn_reflns_limit_h_max       55
_diffrn_reflns_limit_h_min       -61
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            39740
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.918
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.815
_diffrn_reflns_theta_min         3.140
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.078
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52013
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.757
_exptl_crystal_description       block
_exptl_crystal_F_000             3128
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.063
_refine_diff_density_min         -1.017
_refine_diff_density_rms         0.124
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.196
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     691
_refine_ls_number_reflns         17255
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.196
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0110P)^2^+10.5150P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0631
_refine_ls_wR_factor_ref         0.0647
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                15822
_reflns_number_total             17255
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc02355f2.cif
_cod_data_source_block           ps1
_cod_depositor_comments
;
2017-03-01
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C59 H73 Cl7 F4 N2 P2 Pt2'
_cod_original_formula_weight         1586.46
_cod_original_formula_moiety         '2(C29 H36 Cl2 F2 N P Pt), C H Cl3'
_cod_original_formula_units_Z            4
_cod_original_cell_volume        5996.83(17)
_cod_database_code               7117136
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C20 H20 N P Cl2 Pt'
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.98
_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.a Ternary CH refined with riding coordinates:
 C30(H30)
2.b Secondary CH2 refined with riding coordinates:
 C118(H11A,H11B), C119(H11C,H11D), C120(H12A,H12B), C122(H12F,H12G), C123(H12H,
 H12I), C124(H12J,H12K), C126(H12O,H12P), C127(H12Q,H12R), C128(H12S,H12T),
 C218(H21A,H21B), C219(H21C,H21D), C220(H22A,H22B), C222(H22F,H22G), C223(H22H,
 H22I), C224(H22J,H22K), C226(H22O,H22P), C227(H22Q,H22R), C228(H22S,H22T)
2.c Aromatic/amide H refined with riding coordinates:
 C102(H102), C104(H104), C105(H105), C108(H108), C109(H109), C110(H110),
 C113(H113), C114(H114), C116(H116), C202(H202), C204(H204), C205(H205),
 C208(H208), C209(H209), C210(H210), C213(H213), C214(H214), C216(H216)
2.d Idealised Me refined as rotating group:
 C121(H12C,H12D,H12E), C125(H12L,H12M,H12N), C129(H12U,H12V,H12W), C221(H22C,
 H22D,H22E), C225(H22L,H22M,H22N), C229(H22U,H22V,H22W)
;