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_4125925
_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_moiety         'C50 H47 Cl6 O6 P3 S3'
_chemical_formula_sum            'C50 H47 Cl6 O6 P3 S3'
_chemical_formula_weight         1145.66
_space_group_crystal_system      monoclinic
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_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
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_cell_angle_alpha                90
_cell_angle_beta                 91.9110(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1387(10)
_cell_length_b                   20.645(2)
_cell_length_c                   28.401(3)
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_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.11
_cell_measurement_theta_min      2.37
_cell_volume                     5355.4(10)
_computing_cell_refinement       'Bruker SAINT (Bruker 2008)'
_computing_data_collection       'Bruker APEX2 (Bruker 2008)'
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_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.930
_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  0.0369
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.930
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_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            60727
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.930
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.564
_diffrn_reflns_theta_min         1.220
_diffrn_source                   'Bruker TXS fine-focus rotating anode'
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_exptl_absorpt_correction_type   multi-scan
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_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_description       needle
_exptl_crystal_F_000             2360
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
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_exptl_transmission_factor_min   0.986
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_refine_diff_density_min         -1.209
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     621
_refine_ls_number_reflns         12708
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0748
_refine_ls_R_factor_gt           0.0574
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0706P)^2^+13.3116P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1475
_refine_ls_wR_factor_ref         0.1572
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10082
_reflns_number_total             12708
_reflns_threshold_expression     'I > 2\s(I)'
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_cod_data_source_block           masa1002
_cod_depositor_comments
'Adding full bibliography for 4125924--4125926.cif.'
_cod_database_code               4125925
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_exptl_absorpt_special_details   'SADABS-2008/1 - Bruker AXS 2008'
_shelx_res_checksum              48973
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