Sequential Addition of Phosphine to Alkynes for the Selective Synthesis of 1,2-Diphosphinoethanes under Catalysis. Well-Defined NHC-Copper Phosphides vs in Situ CuCl2/NHC Catalyst
Yuan, Jia; Zhu, Lizhao; Zhang, Jianying; Li, Jianfeng; Cui, Chunming; Organometallics 36 (2017) 455–; doi:10.1021/acs.organomet.6b00854

data_4086907
_publ_section_title
;
 Sequential Addition of Phosphine to Alkynes for the Selective Synthesis
 of 1,2-Diphosphinoethanes under Catalysis. Well-Defined NHC-Copper
 Phosphides vs in Situ CuCl2/NHC Catalyst
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              455
_journal_paper_doi               10.1021/acs.organomet.6b00854
_journal_volume                  36
_journal_year                    2017
_chemical_formula_sum            'C69 H90 Cu3 N6 P3'
_chemical_formula_weight         1287.04
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_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
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_atom_sites_solution_secondary   difmap
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_cell_angle_beta                 116.826(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.862(3)
_cell_length_b                   22.2816(19)
_cell_length_c                   27.235(3)
_cell_measurement_reflns_used    33752
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     14547(3)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r2'
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_diffrn_ambient_temperature      113(2)
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_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rigaku Saturn 724CCD camera'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  Multilayer
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_limit_h_max       34
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_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            152347
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.530
_diffrn_reflns_theta_min         3.018
_exptl_absorpt_coefficient_mu    0.975
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_exptl_absorpt_correction_T_min  0.917
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_exptl_crystal_colour            red
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_exptl_crystal_density_method    'not measured'
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_refine_ls_number_reflns         33185
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      0.683
_refine_ls_R_factor_all          0.0716
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_refine_ls_shift/su_max          0.052
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1484P)^2^+95.1709P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_reflns_number_gt                28015
_reflns_number_total             33185
_reflns_threshold_expression     'I > 2\s(I)'
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_cod_depositor_comments          'Adding full bibliography for 4086907.cif.'
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