P-Alkynyl functionalized benzazaphospholes as transmetalating agents.
Zhou, Daniel Y.; Miura-Akagi, Preston M; McCarty, Sierra M.; Guiles, Celeste H.; O'Donnell, Timothy J; Yoshida, Wesley Y.; Krause, Colleen E.; Rheingold, Arnold L.; Hughes, Russell P.; Cain, Matthew F.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 599–611; doi:10.1039/d0dt01367f

data_7706317
_publ_section_title
;
 P-Alkynyl functionalized benzazaphospholes as transmetalating agents.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              599
_journal_page_last               611
_journal_paper_doi               10.1039/d0dt01367f
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C43 H77 I N P3 Pd2'
_chemical_formula_sum            'C43 H77 I N P3 Pd2'
_chemical_formula_weight         1040.66
_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     direct
_audit_block_doi                 10.5517/ccdc.csd.cc26vyjk
_audit_creation_date             2020-09-03
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2020-12-19 deposited with the CCDC.	2021-01-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.8940(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6610(2)
_cell_length_b                   23.3921(3)
_cell_length_c                   15.1918(2)
_cell_measurement_reflns_used    9945
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.23
_cell_volume                     4645.18(11)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_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  0.0594
_diffrn_reflns_av_unetI/netI     0.0579
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            38348
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.312
_diffrn_reflns_theta_min         1.649
_diffrn_source_current           50.0
_diffrn_source_power             2.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.571
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6555
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0797 before and 0.0684 after correction.
The Ratio of minimum to maximum transmission is 0.8790.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_description       plate
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.831
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.120
_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     472
_refine_ls_number_reflns         11515
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0313
_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^)+(0.0166P)^2^+2.6677P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0712
_refine_ls_wR_factor_ref         0.0769
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9880
_reflns_number_total             11515
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01367f3.cif
_cod_data_source_block           cain94_0m_a
_cod_depositor_comments
'Adding full bibliography for 7706316--7706321.cif.'
_cod_original_cell_volume        4645.17(11)
_cod_database_code               7706317
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.776
_shelx_estimated_absorpt_t_min   0.659
_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:
 C17(H17), C14(H14)
2.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B)
2.c Me refined with riding coordinates:
 C31(H31A,H31B,H31C)
2.d Aromatic/amide H refined with riding coordinates:
 C10(H10), C12(H12), C11(H11), C2(H2), C4(H4), C3(H3), C5(H5)
2.e Idealised Me refined as rotating group:
 C43(H43A,H43B,H43C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C35(H35A,H35B,
 H35C), C33(H33A,H33B,H33C), C38(H38A,H38B,H38C), C21(H21A,H21B,H21C), C19(H19A,
 H19B,H19C), C29(H29A,H29B,H29C), C39(H39A,H39B,H39C), C37(H37A,H37B,H37C),
 C15(H15A,H15B,H15C), C34(H34A,H34B,H34C), C30(H30A,H30B,H30C), C18(H18A,H18B,
 H18C), C25(H25A,H25B,H25C), C16(H16A,H16B,H16C), C23(H23A,H23B,H23C), C26(H26A,
 H26B,H26C), C27(H27A,H27B,H27C), C22(H22A,H22B,H22C)
;
_shelx_res_checksum              45857
_olex2_submission_special_instructions 'No special instructions were received'