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_4518029
_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, C7 H8'
_chemical_formula_sum            'C53 H54 O6 P2'
_chemical_formula_weight         848.90
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                90
_cell_angle_beta                 96.8405(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.58208(11)
_cell_length_b                   14.63153(14)
_cell_length_c                   21.2423(2)
_cell_measurement_reflns_used    10337
_cell_measurement_temperature    173
_cell_measurement_theta_max      74.1130
_cell_measurement_theta_min      4.2240
_cell_volume                     4499.96(7)
_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 0.966
_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     41.00  68.00   0.50    1.74    --    0.00  19.00   0.00   54
  2  \w    -82.00 -55.00   0.50    1.74    --    0.00 -19.00-150.00   54
  3  \w    -51.00   9.00   0.50    1.74    --    0.00 -19.00 120.00  120
  4  \w    -52.00  17.00   0.50    1.74    --    0.00 -37.00 -90.00  138
  5  \w    -89.00  -4.00   0.50    1.74    --    0.00 -37.00  90.00  170
  6  \w    151.00 186.00   0.50    6.96    --   96.10  15.00 -30.00   70
  7  \w    100.00 126.00   0.50    6.96    --   96.10  15.00 -30.00   52
  8  \w      7.00  76.00   0.50    6.96    --   96.10 -30.00-180.00  138
  9  \w     69.00 100.00   0.50    6.96    --   96.10 -45.00-180.00   62
 10  \w     13.00  56.00   0.50    6.96    --   96.10 -45.00-180.00   86
 11  \w      7.00 120.00   0.50    6.96    --   96.10 -82.00 150.00  226
 12  \w     90.00 184.00   0.50    6.96    --   96.10  30.00 -60.00  188
 13  \w     84.00 112.00   0.50    6.96    --   96.10 -30.00-180.00   56
 14  \w     63.00  88.00   0.50    6.96    --   96.10 -61.00 120.00   50
 15  \w     79.00 185.00   0.50    6.96    --   96.10  15.00  30.00  212
;
_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      -0.0429899000
_diffrn_orient_matrix_UB_12      0.0875454000
_diffrn_orient_matrix_UB_13      0.0241311000
_diffrn_orient_matrix_UB_21      0.0968126000
_diffrn_orient_matrix_UB_22      0.0430311000
_diffrn_orient_matrix_UB_23      0.0132163000
_diffrn_orient_matrix_UB_31      -0.0101175000
_diffrn_orient_matrix_UB_32      0.0396471000
_diffrn_orient_matrix_UB_33      -0.0676545000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            27213
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.837
_diffrn_reflns_theta_min         3.904
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.279
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73657
_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    1.253
_exptl_crystal_description       prism
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.426
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     551
_refine_ls_number_reflns         8932
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0462
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0523P)^2^+2.3173P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1172
_refine_ls_wR_factor_ref         0.1235
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7401
_reflns_number_total             8932
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao0c02177_si_004.cif
_cod_data_source_block           exp_300
_cod_depositor_comments
'Adding full bibliography for 4518025--4518030.cif.'
_cod_original_cell_volume        4499.97(7)
_cod_database_code               4518029
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C46H46O6P2
_reflns_odcompleteness_completeness 99.90
_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
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C44(H44A,H44B), C43(H43A,H43B), C45(H45A,H45B), C42(H42A,H42B), C19(H19A,
 H19B), C46(H46A,H46B), C21(H21A,H21B), C23(H23A,H23B), C20(H20A,H20B),
 C22(H22A,H22B)
2.b Aromatic/amide H refined with riding coordinates:
 C37(H37), C31(H31), C29(H29), C25(H25), C8(H8), C12(H12), C38(H38), C35(H35),
 C41(H41), C6(H6), C11(H11), C32(H32), C34(H34), C26(H26), C18(H18), C9(H9),
 C28(H28), C17(H17), C2(H2), C27(H27), C15(H15), C14(H14), C40(H40), C3(H3),
 C48(H48), C52(H52), C5(H5), C4(H4), C49(H49), C51(H51), C50(H50)
2.c Idealised Me refined as rotating group:
 C53(H53A,H53B,H53C)
;
_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 1.529
_oxdiff_exptl_absorpt_empirical_full_min 0.533