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_4518025
_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         'C46 H46 O6 P2'
_chemical_formula_sum            'C46 H46 O6 P2'
_chemical_formula_weight         756.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-05-27
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.235(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.8617(7)
_cell_length_b                   14.6759(8)
_cell_length_c                   11.3999(7)
_cell_measurement_reflns_used    1315
_cell_measurement_temperature    173
_cell_measurement_theta_max      56.1220
_cell_measurement_theta_min      4.8100
_cell_volume                     1972.8(2)
_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 0.999
_diffrn_measured_fraction_theta_max 0.963
_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     44.00  73.00   0.50   30.00    --    0.00  37.00 -30.00   58
  2  \w    -89.00 -58.00   0.50   30.00    --    0.00 -37.00-120.00   62
  3  \w    -88.00  18.00   0.50   30.00    --    0.00 -19.00 120.00  212
  4  \w      2.00  27.00   0.50   30.00    --    0.00  37.00 -30.00   50
  5  \w    -32.00  -6.00   0.50   30.00    --    0.00 -37.00-120.00   52
  6  \w     88.00 121.00   0.50  120.00    --   96.10 -77.00-180.00   66
  7  \w     38.00  79.00   0.50  120.00    --   96.10 -77.00-180.00   82
  8  \w    119.00 180.00   0.50  120.00    --   96.10  61.00 -60.00  122
  9  \w     29.00 125.00   0.50  120.00    --   96.10 -82.00 150.00  192
 10  \w     79.00 144.00   0.50  120.00    --   96.10  45.00 -30.00  130
 11  \w      7.00 119.00   0.50  120.00    --   96.10 -61.00-180.00  224
 12  \w     74.00 106.00   0.50  120.00    --   96.10  61.00 -60.00   64
 13  \w     80.00 184.00   0.50  120.00    --   96.10  30.00  30.00  208
;
_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      -0.0066642000
_diffrn_orient_matrix_UB_12      0.0806066000
_diffrn_orient_matrix_UB_13      0.0855450000
_diffrn_orient_matrix_UB_21      0.0428187000
_diffrn_orient_matrix_UB_22      0.0647810000
_diffrn_orient_matrix_UB_23      -0.0918497000
_diffrn_orient_matrix_UB_31      -0.1232231000
_diffrn_orient_matrix_UB_32      0.0181606000
_diffrn_orient_matrix_UB_33      -0.0522235000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0775
_diffrn_reflns_av_unetI/netI     0.0980
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11152
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.682
_diffrn_reflns_theta_min         3.749
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.394
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72080
_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    1.274
_exptl_crystal_description       prism
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.305
_refine_diff_density_min         -0.271
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.928
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3908
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.928
_refine_ls_R_factor_all          0.1323
_refine_ls_R_factor_gt           0.0608
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1488
_refine_ls_wR_factor_ref         0.1905
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2061
_reflns_number_total             3908
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao0c02177_si_003.cif
_cod_data_source_block           exp_305
_cod_depositor_comments
'Adding full bibliography for 4518025--4518030.cif.'
_cod_database_code               4518025
_chemical_oxdiff_formula         C46H46O6P2
_reflns_odcompleteness_completeness 99.92
_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:
 C19(H19A,H19B), C18(H18A,H18B), C21(H21A,H21B), C20(H20A,H20B), C17(H17A,H17B)
2.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C1AA(H1AA), C0AA(H0AA), C9(H9), C6(H6), C16(H16), C15(H15), C13(H13),
 C12(H12), C5(H5), C2(H2), C3(H3), C4(H4)
;
_shelx_res_checksum              36743
_shelx_hkl_checksum              87861
_shelx_shelxl_version_number     2014/7
_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 1.264
_oxdiff_exptl_absorpt_empirical_full_min 0.702