Triphosphasumanene Trisulfide: High Out-of-Plane Anisotropy and Janus-Type π-Surfaces.
Furukawa, Shunsuke; Suda, Yuki; Kobayashi, Junji; Kawashima, Takayuki; Tada, Tomofumi; Fujii, Shintaro; Kiguchi, Manabu; Saito, Masaichi; Journal of the American Chemical Society 139 (2017) 5787–5792; doi:10.1021/jacs.6b12119

data_4125924
_publ_section_title
;
 Triphosphasumanene Trisulfide: High Out-of-Plane Anisotropy and
 Janus-Type \p-Surfaces.
;
_journal_issue                   16
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5787
_journal_page_last               5792
_journal_paper_doi               10.1021/jacs.6b12119
_journal_volume                  139
_journal_year                    2017
_chemical_formula_sum            'C42 H42 O6 P2 S2'
_chemical_formula_weight         768.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_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
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 109.818(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.253(3)
_cell_length_b                   22.067(6)
_cell_length_c                   16.144(4)
_cell_measurement_reflns_used    2437
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.23
_cell_measurement_theta_min      2.67
_cell_volume                     3771.4(17)
_computing_cell_refinement       'Bruker SAINT (Bruker 2008)'
_computing_data_collection       'Bruker APEX2 (Bruker 2008)'
_computing_data_reduction        'Bruker SAINT and XPREP (Bruker 2008)'
_computing_molecular_graphics    'XSHEL (Bruker, 2002)'
_computing_publication_material  'XCIF (Bruker, 2001)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0960
_diffrn_reflns_av_unetI/netI     0.1265
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.920
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20809
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.920
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.241
_diffrn_reflns_theta_min         1.628
_diffrn_source                   'Bruker TXS fine-focus rotating anode'
_exptl_absorpt_coefficient_mu    0.274
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.997
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XPREP; Bruker AXS 2008'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_description       needle
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_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.466
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.960
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     475
_refine_ls_number_reflns         8571
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.960
_refine_ls_R_factor_all          0.1267
_refine_ls_R_factor_gt           0.0540
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0452P)^2^+0.0500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1020
_refine_ls_wR_factor_ref         0.1259
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4819
_reflns_number_total             8571
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b12119_si_006.cif
_cod_data_source_block           masa966a
_cod_depositor_comments
'Adding full bibliography for 4125924--4125926.cif.'
_cod_original_cell_volume        3771.7(17)
_cod_database_code               4125924
_shelx_shelxl_version_number     2014/7
_exptl_absorpt_special_details   'SADABS-2008/1 - Bruker AXS 2008'
_shelx_res_checksum              98558
_shelx_hkl_checksum              68151