Synthesis of Phosphorus-Centered and Chalcogen-Bridged Concave Molecules: Modulation of Bowl Geometries and Packing Structures by Changing Bridging Atoms.
Yamamura, Masaki; Hasegawa, Toru; Nabeshima, Tatsuya; Organic letters 18 (2016) 816–819; doi:10.1021/acs.orglett.6b00105

data_1542659
_publ_section_title
;
 Synthesis of Phosphorus-Centered and Chalcogen-Bridged Concave Molecules:
 Modulation of Bowl Geometries and Packing Structures by Changing Bridging
 Atoms.
;
_journal_issue                   4
_journal_name_full               'Organic letters'
_journal_page_first              816
_journal_page_last               819
_journal_paper_doi               10.1021/acs.orglett.6b00105
_journal_volume                  18
_journal_year                    2016
_chemical_formula_sum            'C18 H9 O2 P S'
_chemical_formula_weight         320.28
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.762(2)
_cell_length_b                   22.071(3)
_cell_length_c                   7.4782(10)
_cell_measurement_reflns_used    3951
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.10
_cell_measurement_theta_min      2.94
_cell_volume                     2766.6(6)
_computing_cell_refinement       'Bruker SAINT'
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_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
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_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
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_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_unetI/netI     0.0139
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.936
_diffrn_reflns_limit_h_max       18
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_diffrn_reflns_limit_k_min       -19
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_diffrn_reflns_limit_l_min       -9
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_diffrn_reflns_point_group_measured_fraction_full 1.000
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_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.005
_diffrn_reflns_theta_min         1.525
_exptl_absorpt_coefficient_mu    0.353
_exptl_absorpt_correction_T_max  0.931
_exptl_absorpt_correction_T_min  0.867
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
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_exptl_crystal_description       "'block"
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_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
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_refine_ls_number_reflns         3441
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0342
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+3.8000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol6b00105_si_006.cif
_cod_data_source_block           PO2Stry2_0ma_a
_cod_database_code               1542659
_shelx_estimated_absorpt_t_min   0.933
_shelx_estimated_absorpt_t_max   0.989
_shelxl_version_number           2014-3
_shelx_res_checksum              29004
_shelx_hkl_checksum              26951