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_4518028
_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'
_chemical_formula_sum            'C48 H50 O6 P2'
_chemical_formula_weight         784.82
_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             2017-05-16
_audit_creation_method
;
Olex2 1.2
(compiled Mar 28 2017 19:26:29 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                78.793(2)
_cell_angle_beta                 71.385(2)
_cell_angle_gamma                77.940(2)
_cell_formula_units_Z            2
_cell_length_a                   11.6696(3)
_cell_length_b                   12.2099(3)
_cell_length_c                   16.0856(4)
_cell_measurement_reflns_used    9064
_cell_measurement_temperature    173
_cell_measurement_theta_max      73.6240
_cell_measurement_theta_min      4.2910
_cell_volume                     2103.86(10)
_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 0.996
_diffrn_measured_fraction_theta_max 0.965
_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    -20.00  29.00   0.50    5.00    --    0.00  57.00 -90.00   98
  2  \w     27.00  86.00   0.50    5.00    --    0.00  82.00 -60.00  118
  3  \w    -36.00  16.00   0.50    5.00    --    0.00 -38.00  60.00  104
  4  \w     -4.00  89.00   0.50    5.00    --    0.00  38.00  30.00  186
  5  \w    -87.00 -39.00   0.50    5.00    --    0.00 -38.00  60.00   96
  6  \w      9.00  63.00   0.50   20.00    --   95.80 -15.00  90.00  108
  7  \w     28.00 120.00   0.50   20.00    --   95.80 -61.00 -90.00  184
  8  \w     27.00  99.00   0.50   20.00    --   95.80 -61.00-150.00  144
  9  \w     30.00 124.00   0.50   20.00    --   95.80 -82.00-150.00  188
 10  \w      7.00 123.00   0.50   20.00    --   95.80 -82.00 -60.00  232
 11  \w      7.00 119.00   0.50   20.00    --   95.80 -61.00  60.00  224
 12  \w    118.00 144.00   0.50   20.00    --   95.80  30.00  30.00   52
 13  \w     69.00 106.00   0.50   20.00    --   95.80  15.00 150.00   74
 14  \w    137.00 170.00   0.50   20.00    --   95.80  15.00 150.00   66
 15  \w     67.00 109.00   0.50   20.00    --   95.80 -82.00   0.00   84
 16  \w     59.00 100.00   0.50   20.00    --   95.80 -82.00 150.00   82
 17  \w     68.00 122.00   0.50   20.00    --   95.80 -15.00  90.00  108
 18  \w      9.00 109.00   0.50   20.00    --   95.80 -30.00 150.00  200
 19  \w      6.00 127.00   0.50   20.00    --   95.80 -82.00  60.00  242
 20  \w     84.00 109.00   0.50   20.00    --   95.80 -82.00 120.00   50
 21  \w     72.00  97.00   0.50   20.00    --   95.80 -82.00-180.00   50
 22  \w      8.00 122.00   0.50   20.00    --   95.80 -15.00-120.00  228
;
_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      0.1208741000
_diffrn_orient_matrix_UB_12      0.0198124000
_diffrn_orient_matrix_UB_13      0.0098451000
_diffrn_orient_matrix_UB_21      -0.0311328000
_diffrn_orient_matrix_UB_22      -0.0647718000
_diffrn_orient_matrix_UB_23      0.0946247000
_diffrn_orient_matrix_UB_31      0.0657456000
_diffrn_orient_matrix_UB_32      -0.1112676000
_diffrn_orient_matrix_UB_33      -0.0368756000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_unetI/netI     0.0393
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            23876
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.213
_diffrn_reflns_theta_min         4.048
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.324
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86145
_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    1.239
_exptl_crystal_description       prism
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.376
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         8278
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0478
_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^)+(0.0905P)^2^+0.2897P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1382
_refine_ls_wR_factor_ref         0.1466
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6731
_reflns_number_total             8278
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao0c02177_si_006.cif
_cod_data_source_block           exp_295
_cod_depositor_comments
'Adding full bibliography for 4518025--4518030.cif.'
_cod_original_cell_volume        2103.85(10)
_cod_database_code               4518028
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C48H50O4P2
_reflns_odcompleteness_completeness 99.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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:
 C45(H45A,H45B), C46(H46A,H46B), C48(H48A,H48B), C42(H42A,H42B), C43(H43A,
 H43B), C44(H44A,H44B), C47(H47A,H47B), C40(H40A,H40B), C41(H41A,H41B),
 C39(H39A,H39B), C37(H37A,H37B), C38(H38A,H38B)
2.b Aromatic/amide H refined with riding coordinates:
 C30(H30), C32(H32), C29(H29), C20(H20), C33(H33), C15(H15), C27(H27),
 C14(H14), C26(H26), C12(H12), C24(H24), C11(H11), C17(H17), C18(H18), C36(H36),
  C6(H6), C35(H35), C2(H2), C23(H23), C21(H21), C4(H4), C8(H8), C9(H9),
 C22(H22), C3(H3), C5(H5)
;
_olex2_exptl_crystal_mounting_method loop
_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 1.514
_oxdiff_exptl_absorpt_empirical_full_min 0.735