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_7706319
_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         'C38 H46 N2 O0.38 P2'
_chemical_formula_sum            'C38 H46 N2 O0.38 P2'
_chemical_formula_weight         598.87
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_block_doi                 10.5517/ccdc.csd.cc26vykl
_audit_creation_date             2020-08-17
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-12-19 deposited with the CCDC.	2021-01-05 downloaded from the CCDC.
;
_cell_angle_alpha                95.100(2)
_cell_angle_beta                 94.213(2)
_cell_angle_gamma                113.203(2)
_cell_formula_units_Z            2
_cell_length_a                   11.6914(5)
_cell_length_b                   12.0731(5)
_cell_length_c                   13.1054(6)
_cell_measurement_reflns_used    4609
_cell_measurement_temperature    100
_cell_measurement_theta_max      68.59
_cell_measurement_theta_min      9.89
_cell_volume                     1681.56(13)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15973
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.328
_diffrn_reflns_theta_min         3.410
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.388
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.6619
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0613 before and 0.0468 after correction.
The Ratio of minimum to maximum transmission is 0.8789.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_description       block
_exptl_crystal_F_000             642
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.433
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         6003
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0370
_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^)+(0.0512P)^2^+0.6308P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.0976
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5452
_reflns_number_total             6003
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01367f3.cif
_cod_data_source_block           cain92_0m_a
_cod_depositor_comments
'Adding full bibliography for 7706316--7706321.cif.'
_cod_database_code               7706319
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.697
_shelx_estimated_absorpt_t_min   0.673
_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:
 C14(H14), C17(H17), C33(H33), C36(H36)
2.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C26(H26A,H26B)
2.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C21(H21), C22(H22), C5(H5), C29(H29), C2(H2), C30(H30), C4(H4),
 C12(H12), C23(H23), C31(H31), C11(H11), C24(H24), C3(H3)
2.d Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C), C19(H19A,H19B,H19C), C16(H16A,H16B,H16C), C15(H15A,H15B,
 H15C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C18(H18A,H18B,H18C), C34(H34A,
 H34B,H34C)
;
_shelx_res_checksum              97718
_olex2_submission_special_instructions 'No special instructions were received'