Oxaphosphacyclophanes Constructed from a Bis(triphenylphosphine oxide) Moiety Linked by Dioxyalkyl Chains: Synthesis and Crystal Structures.
Katagiri, Kosuke; Ohara, Masahiro; Ikehara, Masahiro; Higashimura, Ikkei; Isono, Koshiro; ACS omega 5 (2020) 23621–23630; doi:10.1021/acsomega.0c02177

data_4518026
_publ_section_title
;
 Oxaphosphacyclophanes Constructed from a Bis(triphenylphosphine oxide)
 Moiety Linked by Dioxyalkyl Chains: Synthesis and Crystal Structures.
;
_journal_issue                   37
_journal_name_full               'ACS omega'
_journal_page_first              23621
_journal_page_last               23630
_journal_paper_doi               10.1021/acsomega.0c02177
_journal_volume                  5
_journal_year                    2020
_chemical_formula_moiety         'C48 H50 O6 P2, 2(C6 H12)'
_chemical_formula_sum            'C60 H74 O6 P2'
_chemical_formula_weight         953.13
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-06-17
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                70.567(3)
_cell_angle_beta                 81.108(2)
_cell_angle_gamma                85.4235(18)
_cell_formula_units_Z            1
_cell_length_a                   6.07681(12)
_cell_length_b                   12.5823(3)
_cell_length_c                   18.8446(6)
_cell_measurement_reflns_used    4513
_cell_measurement_temperature    173
_cell_measurement_theta_max      76.3550
_cell_measurement_theta_min      5.0230
_cell_volume                     1341.83(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w     -3.00  23.00   0.50   12.80    --    0.00  37.00-150.00   52
  2  \w    -54.00 -28.00   0.50   12.80    --    0.00 -37.00  60.00   52
  3  \w    -82.00   9.00   0.50   12.80    --    0.00 -19.00 -30.00  182
  4  \w    -21.00  83.00   0.50   12.80    --    0.00  57.00 -60.00  208
  5  \w     43.00  69.00   0.50   12.80    --    0.00  37.00-150.00   52
  6  \w    -16.00  10.00   0.50   12.80    --    0.00 -37.00  60.00   52
  7  \w     76.00 185.00   0.50   30.00    --   99.70  15.00 -60.00  218
  8  \w    152.00 178.00   0.50   30.00    --   99.70  15.00-150.00   52
  9  \w     11.00 116.00   0.50   30.00    --   99.70 -30.00  90.00  210
 10  \w     89.00 143.00   0.50   30.00    --   99.70  15.00-150.00  108
 11  \w     90.00 127.00   0.50   30.00    --   99.70 -82.00  60.00   74
 12  \w     10.00 123.00   0.50   30.00    --   99.70 -61.00 -30.00  226
 13  \w     59.00  85.00   0.50   30.00    --   99.70 -45.00   0.00   52
 14  \w     24.00 128.00   0.50   30.00    --   99.70 -82.00 -30.00  208
 15  \w     99.00 124.00   0.50   30.00    --   99.70 -77.00 120.00   50
 16  \w     11.00  45.00   0.50   30.00    --   99.70 -77.00 120.00   68
 17  \w    104.00 129.00   0.50   30.00    --   99.70 -82.00-150.00   50
 18  \w     44.00 129.00   0.50   30.00    --   99.70 -77.00-180.00  170
 19  \w     94.00 119.00   0.50   30.00    --   99.70 -77.00   0.00   50
 20  \w     17.00  43.00   0.50   30.00    --   99.70 -77.00  30.00   52
 21  \w     88.00 129.00   0.50   30.00    --   99.70 -77.00  30.00   82
 22  \w     77.00 102.00   0.50   30.00    --   99.70 -82.00-120.00   50
 23  \w     22.00 107.00   0.50   30.00    --   99.70 -30.00-180.00  170
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa dual home/near'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0693219000
_diffrn_orient_matrix_UB_12      0.0551034000
_diffrn_orient_matrix_UB_13      -0.0797663000
_diffrn_orient_matrix_UB_21      -0.1625143000
_diffrn_orient_matrix_UB_22      -0.0956775000
_diffrn_orient_matrix_UB_23      0.0158172000
_diffrn_orient_matrix_UB_31      -0.1862462000
_diffrn_orient_matrix_UB_32      0.0684269000
_diffrn_orient_matrix_UB_33      0.0323148000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0790
_diffrn_reflns_av_unetI/netI     0.0881
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12782
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.641
_diffrn_reflns_theta_min         3.727
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.120
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75426
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.20a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.180
_exptl_crystal_description       prism
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.558
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         5388
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_gt           0.0675
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1008P)^2^+0.1461P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1785
_refine_ls_wR_factor_ref         0.1921
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3896
_reflns_number_total             5388
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao0c02177_si_005.cif
_cod_data_source_block           exp_844
_cod_depositor_comments
'Adding full bibliography for 4518025--4518030.cif.'
_cod_database_code               4518026
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C48H50O6P2
_reflns_odcompleteness_completeness 99.49
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C23(H23A,
 H23B), C22(H22A,H22B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B),
 C26(H26A,H26B), C25(H25A,H25B), C27(H27A,H27B)
2.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C8(H8), C12(H12), C17(H17), C9(H9), C2(H2), C6(H6), C3(H3),
 C14(H14), C15(H15), C11(H11), C4(H4), C5(H5)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.816
_oxdiff_exptl_absorpt_empirical_full_min 0.426