Phosphine-catalysed reductive coupling of Dihalophosphanes
Siewert, Jan-Erik; Schumann, André; Hering-Junghans, Christian; Dalton Transactions  (2021) –; doi:10.1039/D1DT03095G

data_7708479
_publ_section_title
;
 Phosphine-catalysed reductive coupling of Dihalophosphanes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03095G
_journal_year                    2021
_chemical_formula_moiety         'C30 H46 Br2 P2'
_chemical_formula_sum            'C30 H46 Br2 P2'
_chemical_formula_weight         628.43
_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
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2021-07-23 deposited with the CCDC.	2021-09-28 downloaded from the CCDC.
;
_cell_angle_alpha                90.634(4)
_cell_angle_beta                 102.776(3)
_cell_angle_gamma                96.594(3)
_cell_formula_units_Z            2
_cell_length_a                   9.7477(16)
_cell_length_b                   12.232(2)
_cell_length_c                   13.591(2)
_cell_measurement_reflns_used    9773
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.59
_cell_measurement_theta_min      2.32
_cell_volume                     1568.8(4)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_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  0.0276
_diffrn_reflns_av_unetI/netI     0.0168
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            76651
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.630
_diffrn_reflns_theta_min         1.537
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.702
_exptl_absorpt_correction_T_max  0.67
_exptl_absorpt_correction_T_min  0.59
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_description       prism
_exptl_crystal_F_000             652
_exptl_crystal_size_max          0.322
_exptl_crystal_size_mid          0.242
_exptl_crystal_size_min          0.162
_refine_diff_density_max         1.215
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         9672
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0261
_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^)+(0.0383P)^2^+0.5487P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0674
_refine_ls_wR_factor_ref         0.0713
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8242
_reflns_number_total             9672
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03095g2.cif
_cod_data_source_block           ax1669_Tip2P2Br2_cmpd_RR_1
_cod_database_code               7708479
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.477
_shelx_estimated_absorpt_t_max   0.669
_shelx_res_checksum              71203