A high temperature reversible phase transition in a supramolecular complex of 15-crown-5 with tetraphenylboron sodium
Yuan, Guo-Jun; Liu, Shao-Xian; Tian, Zheng-Fang; Ren, Xiao-Ming; New Journal of Chemistry 42 (2018) 14943–; doi:10.1039/C8NJ02754D

data_7057606
_publ_section_title
;
 A high temperature reversible phase transition in a supramolecular
 complex of 15-crown-5 with tetraphenylboron sodium
;
_journal_issue                   18
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              14943
_journal_paper_doi               10.1039/C8NJ02754D
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety         'C20 H40 Na2 O10, 2(C24 H20 B)'
_chemical_formula_sum            'C68 H80 B2 Na2 O10'
_chemical_formula_weight         1124.92
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-07-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-07-23 deposited with the CCDC.
2018-07-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.885(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.0154(13)
_cell_length_b                   12.3870(13)
_cell_length_c                   20.7837(18)
_cell_measurement_reflns_used    9825
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.396
_cell_measurement_theta_min      3.192
_cell_volume                     3087.0(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 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      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_unetI/netI     0.0136
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            35262
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.007
_diffrn_reflns_theta_max         25.007
_diffrn_reflns_theta_min         3.198
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.623
_refine_diff_density_min         -0.458
_refine_diff_density_rms         0.041
_refine_ls_extinction_coef       0.0175(14)
_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   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         5440
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0550
_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^)+(0.0753P)^2^+1.7868P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1493
_refine_ls_wR_factor_ref         0.1629
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4431
_reflns_number_total             5440
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj02754d2.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 7057606.cif.'
_cod_database_code               7057606
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.985
_shelx_estimated_absorpt_t_min   0.983
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C25-Na1
 3.2 with sigma of 0.02
 C25-C26
 1.5 with sigma of 0.01
3. Rigid bond restraints
 O1, C26, O5, C25
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4.a Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C30(H30A,H30B), C34(H34A,
 H34B), C28(H28A,H28B), C29(H29A,H29B), C27(H27A,H27B), C26(H26A,H26B),
 C25(H25A,H25B)
4.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C6(H6), C8(H8), C5(H5), C18(H18), C15(H15), C24(H24), C12(H12),
 C2(H2), C22(H22), C4(H4), C17(H17), C20(H20), C16(H16), C10(H10), C9(H9),
 C11(H11), C3(H3), C21(H21), C23(H23)
;
_shelx_res_checksum              86581
_olex2_submission_special_instructions 'No special instructions were received'