An organometallic half-sandwich supramolecular complex {K(18-Crown-6)(η<sup>n</sup>-C<sub>6</sub>H<sub>5</sub>B(C<sub>6</sub>H<sub>5</sub>)<sub>3</sub>)} (n = 1-6) exhibiting a reversible breaking-symmetry phase transition and switchable dielectric behaviour.
Yuan, Guo-Jun; Shao, Dong-Sheng; Yao, Zhi-Yuan; Liu, Wen-Long; Ren, Xiao-Ming; Dalton transactions (Cambridge, England : 2003) 47 (2018) 16835–16839; doi:10.1039/c8dt04060e

data_7047950
_publ_section_title
;
 An organometallic half-sandwich supramolecular complex
 {K(18-Crown-6)(\h<sup>n</sup>-C<sub>6</sub>H<sub>5</sub>B(C<sub>6</sub>H<sub>5</sub>)<sub>3</sub>)}
 (n = 1-6) exhibiting a reversible breaking-symmetry phase transition and
 switchable dielectric behaviour.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16835
_journal_page_last               16839
_journal_paper_doi               10.1039/c8dt04060e
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C34.1 H40.2 B K0.84 O5.05, 0.16(C12 H24 K O6)'
_chemical_formula_sum            'C36 H44 B K O6'
_chemical_formula_weight         622.62
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-08-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-08-22 deposited with the CCDC.
2018-10-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.078(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.6855(10)
_cell_length_b                   14.1873(12)
_cell_length_c                   17.7565(15)
_cell_measurement_reflns_used    5498
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.412
_cell_measurement_theta_min      2.458
_cell_volume                     3452.0(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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0510
_diffrn_reflns_av_unetI/netI     0.0519
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            27080
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         1.890
_exptl_absorpt_coefficient_mu    0.196
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6181
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1146 before and 0.0491 after correction.
The Ratio of minimum to maximum transmission is 0.8290.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_description       block
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.226
_refine_diff_density_min         -0.182
_refine_diff_density_rms         0.033
_refine_ls_extinction_coef       0.0069(15)
_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   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     558
_refine_ls_number_reflns         6034
_refine_ls_number_restraints     784
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.1501
_refine_ls_R_factor_gt           0.0698
_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^)+(0.0997P)^2^+1.4368P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1807
_refine_ls_wR_factor_ref         0.2259
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2990
_reflns_number_total             6034
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04060e2.cif
_cod_data_source_block           11
_cod_depositor_comments
'Adding full bibliography for 7047949--7047951.cif.'
_cod_database_code               7047950
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.967
_shelx_estimated_absorpt_t_min   0.964
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 O5A-C33A
 1.43 with sigma of 0.02
 C34A-C33A
 1.5 with sigma of 0.02
 C34A-O6A
 1.45 with sigma of 0.02
 O6A-C35A
 1.45 with sigma of 0.02
 C35A-C36A
 1.5 with sigma of 0.02
 C36A-O1A
 1.45 with sigma of 0.02
 O1A-C25A
 1.45 with sigma of 0.02
 C25A-C26A
 1.45 with sigma of 0.02
 C26A-O2A
 1.45 with sigma of 0.02
 O2A-C27A
 1.45 with sigma of 0.02
 C27A-C28A
 1.5 with sigma of 0.02
 C28A-O3A
 1.45 with sigma of 0.02
 C29A-O3A
 1.45 with sigma of 0.02
 C29A-C30A
 0.5 with sigma of 0.02
 C30A-O4A
 1.45 with sigma of 0.02
 O4A-C31A
 1.45 with sigma of 0.02
 C31A-C32A
 1.45 with sigma of 0.02
 C32A-O5A
 1.45 with sigma of 0.02
 O6-C34
 1.45 with sigma of 0.02
 C36A-K1A
 3.65 with sigma of 0.02
 K1A-C34A
 3.65 with sigma of 0.02
 O6A-K1A
 2.86 with sigma of 0.02
 K1A-O1A
 2.86 with sigma of 0.02
 K1A-O2A
 2.86 with sigma of 0.02
 K1A-O3A
 2.86 with sigma of 0.02
 O4A-K1A
 2.86 with sigma of 0.02
 C32A-K1A
 3.65 with sigma of 0.02
 K1A-C31A
 3.65 with sigma of 0.02
 K1A-C25A
 3.65 with sigma of 0.02
 O3A-C30A
 2.45 with sigma of 0.02
 C29A-O4A
 2.45 with sigma of 0.02
 C27A-K1A
 3.65 with sigma of 0.02
 O2A-C25A
 2.38 with sigma of 0.02
 O1A-C35A
 2.36 with sigma of 0.02
 O6A-C36A
 2.36 with sigma of 0.02
 C36A-C35A
 1.5 with sigma of 0.02
 O1A-C36A
 1.45 with sigma of 0.02
 C35A-O6A
 1.45 with sigma of 0.02
 K1A-C33A
 3.65 with sigma of 0.02
 K1A-C29A
 3.65 with sigma of 0.02
 C30A-K1A
 3.65 with sigma of 0.02
 C28A-K1A
 3.65 with sigma of 0.02
 C26A-K1A
 3.65 with sigma of 0.02
 C30A-C29A
 1.55 with sigma of 0.02
3. Rigid bond restraints
 K1, O2, O5, O4, O6, O1, O3, C26, C34, C33, C25, C27, C32, C30, C36, C31, C29,
 C35, C28, K1A, O2A, O5A, O4A, O6A, O1A, O3A, C26A, C34A, C33A, C25A, C27A,
 C32A, C30A, C36A, C31A, C29A, C35A, C28A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
K1 \\sim O2 \\sim O5 \\sim O4 \\sim O6 \\sim O1 \\sim O3 \\sim C26 \\sim C34
\\sim C33 \\sim C25 \\sim C27 \\sim C32 \\sim C30 \\sim C36 \\sim C31 \\sim C29
\\sim C35 \\sim C28 \\sim K1A \\sim O2A \\sim O5A \\sim O4A \\sim O6A \\sim O1A
\\sim O3A \\sim C26A \\sim C34A \\sim C33A \\sim C25A \\sim C27A \\sim C32A
\\sim C30A \\sim C36A \\sim C31A \\sim C29A \\sim C35A \\sim C28A: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C26A) \\sim Ueq, Uanis(C25A) \\sim Ueq, Uanis(C30A) \\sim Ueq,
Uanis(C29A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C30) = Uanis(C30A)
Uanis(C29) = Uanis(C29A)
5. Others
 Sof(K1A)=Sof(O2A)=Sof(O5A)=Sof(O4A)=Sof(O6A)=Sof(O1A)=Sof(O3A)=Sof(C26A)=
 Sof(H26C)=Sof(H26D)=Sof(C34A)=Sof(H34C)=Sof(H34D)=Sof(C33A)=Sof(H33C)=
 Sof(H33D)=Sof(C25A)=Sof(H25C)=Sof(H25D)=Sof(C27A)=Sof(H27C)=Sof(H27D)=
 Sof(C32A)=Sof(H32C)=Sof(H32D)=Sof(C30A)=Sof(H30C)=Sof(H30D)=Sof(C36A)=
 Sof(H36C)=Sof(H36D)=Sof(C31A)=Sof(H31C)=Sof(H31D)=Sof(C29A)=Sof(H29C)=
 Sof(H29D)=Sof(C35A)=Sof(H35C)=Sof(H35D)=Sof(C28A)=Sof(H28C)=Sof(H28D)=1-FVAR(1)
 Sof(K1)=Sof(O2)=Sof(O5)=Sof(O4)=Sof(O6)=Sof(O1)=Sof(O3)=Sof(C26)=Sof(H26A)=
 Sof(H26B)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(C25)=
 Sof(H25A)=Sof(H25B)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(C32)=Sof(H32A)=Sof(H32B)=
 Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(C31)=Sof(H31A)=
 Sof(H31B)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(C28)=
 Sof(H28A)=Sof(H28B)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C34(H34A,H34B), C33(H33A,H33B), C25(H25A,H25B), C27(H27A,
 H27B), C32(H32A,H32B), C30(H30A,H30B), C36(H36A,H36B), C31(H31A,H31B),
 C29(H29A,H29B), C35(H35A,H35B), C28(H28A,H28B), C26A(H26C,H26D), C34A(H34C,
 H34D), C33A(H33C,H33D), C25A(H25C,H25D), C27A(H27C,H27D), C32A(H32C,H32D),
 C30A(H30C,H30D), C36A(H36C,H36D), C31A(H31C,H31D), C29A(H29C,H29D), C35A(H35C,
 H35D), C28A(H28C,H28D)
6.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C6(H6), C14(H14), C9(H9), C18(H18), C20(H20), C5(H5), C22(H22),
 C11(H11), C2(H2), C4(H4), C24(H24), C15(H15), C16(H16), C8(H8), C10(H10),
 C3(H3), C17(H17), C23(H23), C21(H21)
;
_shelx_res_checksum              89141
_olex2_submission_special_instructions 'No special instructions were received'