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_1542660
_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            'C21 H16 F2 N O4 P S'
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_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
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_atom_sites_solution_hydrogens   mixed
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_cell_length_b                   11.479(3)
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_cell_measurement_temperature    120(2)
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_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
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_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
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_diffrn_reflns_Laue_measured_fraction_full 1.000
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_diffrn_reflns_limit_k_min       -15
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_diffrn_reflns_point_group_measured_fraction_full 1.000
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_exptl_absorpt_coefficient_mu    0.307
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_exptl_absorpt_correction_T_min  0.912
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
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_exptl_crystal_description       block
_exptl_crystal_F_000             920
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_exptl_crystal_size_mid          0.100
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_refine_ls_extinction_method     none
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_refine_ls_R_factor_all          0.0687
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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^)+(0.0435P)^2^+1.7875P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_reflns_Friedel_coverage         0.000
_reflns_number_gt                3592
_reflns_number_total             4917
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol6b00105_si_002.cif
_cod_data_source_block           cyclemono_a
_cod_original_cell_volume        1882.6(7)
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_shelx_estimated_absorpt_t_min   0.941
_shelx_estimated_absorpt_t_max   0.985
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_shelx_res_checksum              47101
_shelx_hkl_checksum              33454