Further investigations of the crystal-to-crystal phase transition of a [2]pseudorotaxane composed of ferrocene-terminated dialkylammonium and dibenzo[24]crown-8-ether
Suzaki, Yuji; Fukuchi, Yugo; Tadami, Hiroko; Koizumi, Take-aki; Osakada, Kohtaro; Ide, Tomohito; Horie, Masaki; Hoshino, Norihisa; Akutagawa, Tomoyuki; CrystEngComm 23 (2021) 5944–5952; doi:10.1039/D1CE00457C

data_7243153
_publ_section_title
;
 Further investigations of the crystal-to-crystal phase transition of a
 [2]pseudorotaxane composed of ferrocene-terminated dialkylammonium and
 dibenzo[24]crown-8-ether
;
_journal_issue                   34
_journal_name_full               CrystEngComm
_journal_page_first              5944
_journal_page_last               5952
_journal_paper_doi               10.1039/D1CE00457C
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'F6 P0.48 Sb0.52, C19 H22 Fe N, C24 H32 O8'
_chemical_formula_sum            'C43 H54 F6 Fe N O8 P0.484 Sb0.516'
_chemical_formula_weight         960.53
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-04-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-04-03 deposited with the CCDC.	2021-06-21 downloaded from the CCDC.
;
_cell_angle_alpha                85.655(4)
_cell_angle_beta                 87.434(4)
_cell_angle_gamma                88.542(5)
_cell_formula_units_Z            2
_cell_length_a                   10.1390(18)
_cell_length_b                   11.679(2)
_cell_length_c                   17.971(3)
_cell_measurement_reflns_used    6509
_cell_measurement_temperature    113.35
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.34
_cell_volume                     2119.2(6)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      113.35
_diffrn_measured_fraction_theta_full 0.9323
_diffrn_measured_fraction_theta_max 0.9323
_diffrn_measurement_device_type  Saturn70
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            16069
_diffrn_reflns_theta_full        27.4836
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.34
_exptl_absorpt_coefficient_mu    0.776
_exptl_crystal_density_diffrn    1.5051
_exptl_crystal_description       prism
_exptl_crystal_F_000             993.9121
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.1382
_refine_diff_density_min         -0.9917
_refine_diff_density_rms         0.1009
_refine_ls_d_res_high            0.7700
_refine_ls_d_res_low             6.1026
_refine_ls_goodness_of_fit_ref   1.0287
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    92
_refine_ls_number_parameters     546
_refine_ls_number_reflns         9054
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.0279
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0548
_refine_ls_shift/su_max          0.0024
_refine_ls_shift/su_mean         0.0002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0852P)^2^+3.3567P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1452
_refine_ls_wR_factor_ref         0.1637
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              15
_reflns_limit_k_min              -15
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                7718
_reflns_number_total             9054
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d1ce00457c2.cif
_cod_data_source_block           256b-1
_cod_depositor_comments
'Adding full bibliography for 7243143--7243153.cif.'
_cod_original_cell_volume        2119.3(7)
_cod_database_code               7243153
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Sb1-F1 \\sim Sb1-F2 \\sim Sb1-F3 \\sim Sb1-F4 \\sim Sb1-F5 \\sim Sb1-F6
 with sigma of 0.02
 P1-F1 \\sim P1-F2 \\sim P1-F3 \\sim P1-F4 \\sim P1-F5 \\sim P1-F6
 with sigma of 0.02
3. Others
 Sof(P1)=1-FVAR(1)
 Sof(Sb1)=FVAR(1)
 U11(P1)=2.69983*FVAR(2)
 Fixed U22: P1(0.999918)
4.a Secondary CH2 refined with riding coordinates:
 N1(H1a,H1b), C8(H8a,H8b), C9(H9a,H9b), C26(H26a,H26b), C27(H27a,H27b),
 C28(H28a,H28b), C29(H29a,H29b), C30(H30a,H30b), C31(H31a,H31b), C38(H38a,H38b),
  C39(H39a,H39b), C40(H40a,H40b), C41(H41a,H41b), C42(H42a,H42b), C43(H43a,H43b)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C11(H11), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22), C23(H23),
  C24(H24), C33(H33), C34(H34), C35(H35), C36(H36)
4.c Idealised Me refined as rotating group:
 C1(H1c,H1d,H1e)
;
_olex2_submission_special_instructions 'No special instructions were received'