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_4135390
_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         'C32 H34 Cl N2 Ni P2, 0.25(C7 H8)'
_chemical_formula_sum            'C33.75 H36 Cl N2 Ni P2'
_chemical_formula_weight         625.74
_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             2019-07-30
_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            8
_cell_length_a                   15.4791(13)
_cell_length_b                   15.4791(13)
_cell_length_c                   26.403(2)
_cell_measurement_reflns_used    9666
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.33
_cell_measurement_theta_min      2.42
_cell_volume                     6326.2(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XLMP (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      99.99
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0601
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            178189
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.023
_diffrn_reflns_theta_min         1.525
_exptl_absorpt_coefficient_mu    0.824
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6820
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.1248 before and 0.0636 after correction. 
The Ratio of minimum to maximum transmission is 0.9140. 
The \l/2 correction factor is Not present. 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_description       plate
_exptl_crystal_F_000             2620
_exptl_crystal_size_max          0.285
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.015
_refine_diff_density_max         2.207
_refine_diff_density_min         -0.607
_refine_diff_density_rms         0.132
_refine_ls_abs_structure_details
; 
 Flack x determined using 3733 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.017(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         10098
_refine_ls_number_restraints     277
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0523
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0922P)^2^+4.8497P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1476
_refine_ls_wR_factor_ref         0.1547
_reflns_Friedel_coverage         0.840
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                9000
_reflns_number_total             10098
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c11161_si_005.cif
_cod_data_source_block           final
_cod_depositor_comments
'Adding full bibliography for 4135390--4135393.cif.'
_cod_original_cell_volume        6326.3(12)
_cod_database_code               4135390
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.988
_shelx_estimated_absorpt_t_min   0.799
_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 
 C1S-C2S = C1T-C2T 
 1.52 with sigma of 0.01 
 C1S-C3S \\sim C1S-C7S \\sim C1T-C3T \\sim C1T-C7T 
 with sigma of 0.02 
3. Restrained planarity 
 C1S, C2S, C3S, C4S, C5S, C6S, C7S 
 with sigma of 0.1 
 C1T, C2T, C3T, C4T, C5T, C6T, C7T 
 with sigma of 0.1 
4. Uiso/Uaniso restraints and constraints 
C1S \\sim C2S \\sim C3S \\sim C4S \\sim C5S \\sim C6S \\sim C7S \\sim C1T \\sim 
C2T \\sim C3T \\sim C4T \\sim C5T \\sim C6T \\sim C7T: within 2A with sigma of 
0.04 and sigma for terminal atoms of 0.08 
Uanis(C1S) = Uanis(C1T) 
Uanis(C2S) = Uanis(C2T) 
Uanis(C3S) = Uanis(C3T) 
Uanis(C4S) = Uanis(C4T) 
Uanis(C5S) = Uanis(C5T) 
Uanis(C6S) = Uanis(C6T) 
Uanis(C7S) = Uanis(C7T) 
5. Rigid body (RIGU) restrains 
 C1S, C2S, C3S, C4S, C5S, C6S, C7S 
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 
6. Others 
 Sof(C1T)=Sof(H1TA)=Sof(H1TB)=Sof(H1TC)=Sof(C2T)=Sof(C3T)=Sof(H3T)=Sof(C4T)= 
 Sof(H4T)=Sof(C5T)=Sof(H5T)=Sof(C6T)=Sof(H6T)=Sof(C7T)=Sof(H7T)=0.25*(1-FVAR(2)) 
 Sof(C1S)=Sof(H1SA)=Sof(H1SB)=Sof(H1SC)=Sof(C2S)=Sof(C3S)=Sof(H3S)=Sof(C4S)= 
 Sof(H4S)=Sof(C5S)=Sof(H5S)=Sof(C6S)=Sof(H6S)=Sof(C7S)=Sof(H7S)=0.25*FVAR(2) 
7.a Ternary CH refined with riding coordinates: 
 C26(H26), C29(H29) 
7.b Me refined with riding coordinates: 
 C1T(H1TA,H1TB,H1TC), C1S(H1SA,H1SB,H1SC) 
7.c Aromatic/amide H refined with riding coordinates: 
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11), 
 C15(H15), C16(H16), C17(H17), C18(H18), C21(H21), C22(H22), C23(H23), C24(H24), 
  C3T(H3T), C4T(H4T), C5T(H5T), C6T(H6T), C7T(H7T), C3S(H3S), C4S(H4S), 
 C5S(H5S), C6S(H6S), C7S(H7S) 
7.d Fitted hexagon refined as free rotating group: 
 C2T(C3T,C4T,C5T,C6T,C7T), C2S(C3S,C4S,C5S,C6S,C7S) 
7.e Idealised Me refined as rotating group: 
 C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C31(H31A,H31B, 
 H31C), C32(H32A,H32B,H32C) 
;
_shelx_res_checksum              59213
_shelx_hkl_checksum              97962
_olex2_submission_special_instructions 'No special instructions were received'