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_4518030
_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         '2(C22 H21 O3 P)'
_chemical_formula_sum            'C44 H42 O6 P2'
_chemical_formula_weight         728.71
_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     dual
_audit_creation_date             2019-11-26
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 95.31(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.019(5)
_cell_length_b                   9.0240(18)
_cell_length_c                   17.562(4)
_cell_measurement_reflns_used    17001
_cell_measurement_temperature    100
_cell_measurement_theta_max      32.045
_cell_measurement_theta_min      1.000
_cell_volume                     3632.4(14)
_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      100
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  MX225HE
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.800
_diffrn_reflns_av_R_equivalents  0.0683
_diffrn_reflns_av_unetI/netI     0.0627
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            17001
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        28.685
_diffrn_reflns_theta_max         32.045
_diffrn_reflns_theta_min         1.000
_diffrn_source                   'Spring-8 BL38B1'
_exptl_absorpt_coefficient_mu    0.233
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_description       prism
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.575
_refine_diff_density_min         -0.885
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       0.024(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     596
_refine_ls_number_reflns         8776
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.0656
_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^)+(0.1177P)^2^+1.3173P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1907
_refine_ls_wR_factor_ref         0.2064
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7146
_reflns_number_total             8776
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao0c02177_si_002.cif
_cod_data_source_block           p21c
_cod_depositor_comments
'Adding full bibliography for 4518025--4518030.cif.'
_cod_original_cell_volume        3632.4(13)
_cod_database_code               4518030
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.977
_shelx_estimated_absorpt_t_min   0.977
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Others
 Fixed Sof: H13A(0.75) H13B(0.75) H13C(0.25) H13D(0.25) H18(0.75) H18A(0.25)
 O3(0.75) C14(0.75) H14A(0.75) H14B(0.75) C15(0.75) H15A(0.75) H15B(0.75)
 C16(0.75) H16A(0.75) H16B(0.75) C17(0.75) C21(0.75) H21(0.75) C22(0.75)
 H22(0.75) O0AA(0.25) C0AA(0.25) H0AA(0.25) H0AB(0.25) C1AA(0.25) H1AA(0.25)
 H1AB(0.25) C2AA(0.25) H2AA(0.25) H2AB(0.25) C6AA(0.25) C7AA(0.25) H7AA(0.25)
 C8AA(0.25) H8AA(0.25) H35A(0.75) H35B(0.75) H35C(0.25) H35D(0.25) H40(0.75)
 H40A(0.25) O6(0.75) C36(0.75) H36A(0.75) H36B(0.75) C37(0.75) H37A(0.75)
 H37B(0.75) C38(0.75) H38A(0.75) H38B(0.75) C39(0.75) C43(0.75) H43(0.75)
 C44(0.75) H44(0.75) O1AA(0.25) C0BA(0.25) H0BA(0.25) C1BA(0.25) H1BA(0.25)
 C3AA(0.25) H3AA(0.25) H3AB(0.25) C4AA(0.25) H4AA(0.25) H4AB(0.25) C5AA(0.25)
 H5AA(0.25) H5AB(0.25) C9AA(0.25)
3.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C13(H13C,H13D), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,
 H16B), C0AA(H0AA,H0AB), C1AA(H1AA,H1AB), C2AA(H2AA,H2AB), C35(H35A,H35B),
 C35(H35C,H35D), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C3AA(H3AA,
 H3AB), C4AA(H4AA,H4AB), C5AA(H5AA,H5AB)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C11(H11), C12(H12),
 C18(H18), C18(H18A), C19(H19), C21(H21), C22(H22), C7AA(H7AA), C8AA(H8AA),
 C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C30(H30), C31(H31), C33(H33),
  C34(H34), C40(H40), C40(H40A), C41(H41), C43(H43), C44(H44), C0BA(H0BA),
 C1BA(H1BA)
;
_olex2_exptl_crystal_mounting_method loop
_olex2_submission_special_instructions 'No special instructions were received'