An Efficient Catalytic Method for Hydrophosphination of Heterocumulenes with Diethylzinc as Precatalyst without a Solvent
Zhang, Bingyi; Roesky, Herbert W.; Ma, Xiaoli; Yan, Ben; Ni, Congjian; Yu, Hailong; Yang, Zhi; Dalton Transactions  (2021) –; doi:10.1039/D1DT02706A

data_7708606
_publ_section_title
;
 An Efficient Catalytic Method for Hydrophosphination of Heterocumulenes
 with Diethylzinc as Precatalyst without a Solvent
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02706A
_journal_year                    2021
_chemical_formula_moiety         'C42 H58 N4 P2 Zn2'
_chemical_formula_sum            'C42 H58 N4 P2 Zn2'
_chemical_formula_weight         811.60
_chemical_name_systematic        Zn-C
_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     dual
_audit_creation_date             2021-06-25
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-07-20 deposited with the CCDC.	2021-08-31 downloaded from the CCDC.
;
_cell_angle_alpha                101.438(2)
_cell_angle_beta                 98.239(2)
_cell_angle_gamma                106.0400(10)
_cell_formula_units_Z            2
_cell_length_a                   8.4939(4)
_cell_length_b                   14.3347(7)
_cell_length_c                   18.6216(9)
_cell_measurement_reflns_used    9956
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.41
_cell_measurement_theta_min      2.28
_cell_volume                     2088.01(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0662
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20416
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.141
_diffrn_source_current           35.0
_diffrn_source_power             1.575
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.258
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_description       block
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         7329
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0271
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0334P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0669
_refine_ls_wR_factor_ref         0.0689
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6228
_reflns_number_total             7329
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02706a2.cif
_cod_data_source_block           1
_cod_database_code               7708606
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.884
_shelx_estimated_absorpt_t_min   0.787
_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:
 C27(H27), C36(H36), C34(H34), C30(H30)
2.b Secondary CH2 refined with riding coordinates:
 C42(H42A,H42B), C39(H39A,H39B)
2.c Me refined with riding coordinates:
 C29(H29A,H29B,H29C), C28(H28A,H28B,H28C), C38(H38A,H38B,H38C), C33(H33A,H33B,
 H33C), C35(H35A,H35B,H35C), C37(H37A,H37B,H37C), C32(H32A,H32B,H32C), C31(H31A,
 H31B,H31C), C41(H41A,H41B,H41C), C40(H40A,H40B,H40C)
2.d Aromatic/amide H refined with riding coordinates:
 C20(H20), C16(H16), C22(H22), C18(H18), C2(H2), C8(H8), C15(H15), C9(H9),
 C3(H3), C6(H6), C5(H5), C4(H4), C12(H12), C23(H23), C14(H14), C11(H11),
 C10(H10), C21(H21), C13(H13), C24(H24)
;
_shelx_res_checksum              36993
_olex2_submission_special_instructions 'No special instructions were received'