A selective route to aryl-triphosphiranes and their titanocene-induced fragmentation
Schumann, André; Reiß, Fabian; Jiao, Haijun; Rabeah, Jabor; Siewert, Jan-Erik; Krummenacher, Ivo; Braunschweig, Holger; Hering-Junghans, Christian; Chemical Science  (2019) –; doi:10.1039/C9SC02322D

data_1552160
_publ_section_title
;
 A selective route to aryl-triphosphiranes and their titanocene-induced
 fragmentation
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC02322D
_journal_year                    2019
_chemical_formula_moiety         'C30 H46 P2'
_chemical_formula_sum            'C30 H46 P2'
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_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-05-09 deposited with the CCDC.    2019-08-06 downloaded from the CCDC.
;
_cell_angle_alpha                91.2410(10)
_cell_angle_beta                 100.0930(10)
_cell_angle_gamma                91.1460(10)
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_cell_length_b                   8.5877(7)
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_cell_measurement_reflns_used    9972
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.52
_cell_measurement_theta_min      2.37
_cell_volume                     709.40(10)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
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_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 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_unetI/netI     0.0165
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
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_diffrn_reflns_limit_k_min       -12
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_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            35520
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
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_diffrn_reflns_theta_min         1.465
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.168
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.88
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.097
_exptl_crystal_description       prism
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_refine_diff_density_max         0.460
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_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         4338
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0368
_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^)+(0.0523P)^2^+0.2282P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_reflns_Friedel_coverage         0.000
_reflns_number_gt                3816
_reflns_number_total             4338
_reflns_threshold_expression     'I > 2\s(I)'
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_cod_data_source_block           ax1494_Tipp2P2_cmp_2
_cod_database_code               1552160
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.954
_shelx_estimated_absorpt_t_max   0.979
_shelx_res_checksum              20950