Reactions of a persistent phosphinyl radical/diphosphine with heteroallenes.
Giffin, Nick A.; Hendsbee, Arthur D.; Masuda, Jason D.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 12636–12638; doi:10.1039/c6dt02790c

data_7040034
_publ_section_title
;
 Reactions of a persistent phosphinyl radical/diphosphine with
 heteroallenes.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12636
_journal_page_last               12638
_journal_paper_doi               10.1039/c6dt02790c
_journal_volume                  45
_journal_year                    2016
_chemical_formula_sum            'C59 H81 N5 O P2'
_chemical_formula_weight         938.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-07-14 deposited with the CCDC.
2016-07-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.239(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   29.594(7)
_cell_length_b                   19.280(5)
_cell_length_c                   22.869(6)
_cell_measurement_reflns_used    7123
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      26.04
_cell_measurement_theta_min      2.32
_cell_volume                     12078(5)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Siemens/Bruker APEXII'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0809
_diffrn_reflns_av_unetI/netI     0.0904
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            39221
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         1.936
_exptl_absorpt_coefficient_mu    0.111
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6802
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Bruker, 2008)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.032
_exptl_crystal_description       plate
_exptl_crystal_F_000             4064
_exptl_crystal_size_max          0.237
_exptl_crystal_size_mid          0.154
_exptl_crystal_size_min          0.094
_platon_squeeze_details
;
The unit cell contains 6 toluene molecules which have been treated as a diffuse contribution to the overall scattering without specific atom positions by SQUEEZE/PLATON.A.L.Spek, J.Appl.Cryst. 2003, 36, 7-13. 
;
_refine_diff_density_max         0.226
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_refine_ls_extinction_method     none
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_refine_ls_number_reflns         10618
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.921
_refine_ls_R_factor_all          0.1020
_refine_ls_R_factor_gt           0.0560
_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^)+(0.0664P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1218
_refine_ls_wR_factor_ref         0.1368
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6304
_reflns_number_total             10618
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02790c2.cif
_cod_data_source_block           NG122_0m
_cod_depositor_comments
'Adding full bibliography for 7040032--7040034.cif.'
_cod_database_code               7040034
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.974
_shelx_estimated_absorpt_t_max   0.990
_shelx_res_checksum              77966