Anthracene as a Launchpad for a Phosphinidene Sulfide and for Generation of a Phosphorus-Sulfur Material Having the Composition P<sub>2</sub>S, a Vulcanized Red Phosphorus That Is Yellow.
Transue, Wesley J.; Nava, Matthew; Terban, Maxwell W.; Yang, Jing; Greenberg, Matthew W.; Wu, Gang; Foreman, Elizabeth S.; Mustoe, Chantal L.; Kennepohl, Pierre; Owen, Jonathan S.; Billinge, Simon J. L.; Kulik, Heather J.; Cummins, Christopher C.; Journal of the American Chemical Society 141 (2019) 431–440; doi:10.1021/jacs.8b10775

data_4133528
_publ_section_title
;
 Anthracene as a Launchpad for a Phosphinidene Sulfide and for Generation
 of a Phosphorus-Sulfur Material Having the Composition P<sub>2</sub>S, a
 Vulcanized Red Phosphorus That Is Yellow.
;
_journal_issue                   1
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              431
_journal_page_last               440
_journal_paper_doi               10.1021/jacs.8b10775
_journal_volume                  141
_journal_year                    2019
_chemical_formula_sum            'C14 H11 P S'
_chemical_formula_weight         242.26
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.3118(5)
_cell_length_b                   22.2656(12)
_cell_length_c                   6.2032(3)
_cell_measurement_reflns_used    8201
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.96
_cell_measurement_theta_min      2.62
_cell_volume                     1148.01(11)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2011)'
_computing_data_collection       'APEX2 v2011.4.0 (Bruker-AXS, 2011)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2011)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Smart APEX2 CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            16752
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.989
_diffrn_reflns_theta_min         1.829
_diffrn_source
'I\mS micro-focus sealed tube, multilayer optics'
_exptl_absorpt_coefficient_mu    0.387
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6668
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.440
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.309
_refine_diff_density_min         -0.241
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details
; 
 Flack x determined using 1409 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         3523
_refine_ls_number_restraints     115
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0274
_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^)+(0.0344P)^2^+0.3068P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0666
_refine_ls_wR_factor_ref         0.0673
_reflns_Friedel_coverage         0.796
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.937
_reflns_number_gt                3393
_reflns_number_total             3523
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b10775_si_002.cif
_cod_data_source_block           main
_cod_database_code               4133528
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.848
_shelx_estimated_absorpt_t_max   0.962
_shelx_res_checksum              32094
_shelx_hkl_checksum              72284