Enthalpy-Controlled Insertion of a "Nonspectator" Tricoordinate Phosphorus Ligand into Group 10 Transition Metal-Carbon Bonds.
Hwang, Seung Jun; Tanushi, Akira; Radosevich, Alexander T.; Journal of the American Chemical Society 142 (2020) 21285–21291; doi:10.1021/jacs.0c11161

data_4135393
_publ_section_title
;
 Enthalpy-Controlled Insertion of a &quot;Nonspectator&quot; Tricoordinate
 Phosphorus Ligand into Group 10 Transition Metal-Carbon Bonds.
;
_journal_issue                   51
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              21285
_journal_page_last               21291
_journal_paper_doi               10.1021/jacs.0c11161
_journal_volume                  142
_journal_year                    2020
_chemical_formula_moiety         '4(C31 H34 Cl N3 P2 Pd), C7 H5 F3'
_chemical_formula_sum            'C131 H141 Cl4 F3 N12 P8 Pd4'
_chemical_formula_weight         2755.71
_space_group_crystal_system      tetragonal
_space_group_IT_number           114
_space_group_name_Hall           'P -4 2n'
_space_group_name_H-M_alt        'P -4 21 c'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-07-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.426(3)
_cell_length_b                   15.426(3)
_cell_length_c                   26.835(6)
_cell_measurement_reflns_used    2698
_cell_measurement_temperature    15(2)
_cell_measurement_theta_max      7.61
_cell_measurement_theta_min      2.315
_cell_volume                     6386(2)
_computing_cell_refinement       'SAINT 8.35A (Bruker-AXS,2015)'
_computing_data_collection       'APEX3 v2016.1.0 (Bruker-AXS,2016)'
_computing_data_reduction        'SAINT 8.35A (Bruker-AXS,2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XLMP (Sheldrick, 2008)'
_diffrn_ambient_temperature      15.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
;
Huber three-circle goniometer with free kappa with Pilatus 1M CdTe Pixel Array Detector
;
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.24797
_diffrn_reflns_av_R_equivalents  0.1382
_diffrn_reflns_av_unetI/netI     0.0455
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            131592
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        8.485
_diffrn_reflns_theta_max         8.485
_diffrn_reflns_theta_min         0.839
_exptl_absorpt_coefficient_mu    0.227
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2820
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.221
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.124
_refine_ls_abs_structure_details
;
 Flack x determined using 2190 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.004(17)
_refine_ls_extinction_coef       0.063(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         5631
_refine_ls_number_restraints     139
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0371
_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^)+(0.0563P)^2^+5.0929P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0970
_refine_ls_wR_factor_ref         0.1018
_reflns_Friedel_coverage         0.812
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                5168
_reflns_number_total             5631
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c11161_si_004.cif
_cod_data_source_block           final
_cod_depositor_comments
'Adding full bibliography for 4135390--4135393.cif.'
_cod_original_cell_volume        6386(3)
_cod_database_code               4135393
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.995
_shelx_estimated_absorpt_t_min   0.991
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C7S-F1S = C7S-F2S = C7S-F3S
 1.32 with sigma of 0.02
 C5S-C7S \\sim C1S-C7S
 with sigma of 0.02
 F1S-F2S \\sim F2S-F3S \\sim F3S-F1S
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1S \\sim C2S \\sim C3S \\sim C4S \\sim C5S \\sim C6S \\sim C7S \\sim F1S \\sim
F2S \\sim F3S: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C1S) = Uanis(C5S)
Uanis(C2S) = Uanis(C4S)
Uanis(C3S) = Uanis(C6S)
Uanis(F1S) = Uanis(F2S) = Uanis(F3S)
4. Rigid body (RIGU) restrains
 C1S, C2S, C3S, C4S, C5S, C6S, C7S, F1S, F2S, F3S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C1S(0.25) H1S(0.25) C2S(0.25) H2S(0.25) C3S(0.25) H3S(0.25)
 C4S(0.25) H4S(0.25) C5S(0.25) H5S(0.25) C6S(0.25) C7S(0.25) F1S(0.25)
 F2S(0.25) F3S(0.25)
6.a Ternary CH refined with riding coordinates:
 C25(H25), C28(H28)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C11(H11), C12(H12),
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C21(H21), C22(H22), C23(H23),
  C24(H24), C1S(H1S), C2S(H2S), C3S(H3S), C4S(H4S), C5S(H5S)
6.c Fitted hexagon refined as free rotating group:
 C1S(C2S,C3S,C4S,C5S,C6S)
6.d Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C), C31(H31A,H31B,H31C)
;
_shelx_res_checksum              52824
_shelx_hkl_checksum              8739
_olex2_submission_special_instructions 'No special instructions were received'