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_7243152
_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         'C19 H22 Fe N, C24 H32 O8, 2(F3 P0.5)'
_chemical_formula_sum            'C43 H54 F6 Fe N O8 P'
_chemical_formula_weight         913.72
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_symmetry_Int_Tables_number      13
_audit_creation_date             2015-06-29
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2021-04-06 deposited with the CCDC.	2021-06-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.199(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.497(5)
_cell_length_b                   9.893(2)
_cell_length_c                   22.324(5)
_cell_measurement_reflns_used    4465
_cell_measurement_temperature    93.15
_cell_measurement_theta_max      27.92
_cell_measurement_theta_min      2.19
_cell_volume                     4259.9(16)
_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)'
_diffrn_ambient_temperature      93.15
_diffrn_measured_fraction_theta_full 0.9281
_diffrn_measured_fraction_theta_max 0.9281
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0580
_diffrn_reflns_av_unetI/netI     0.0892
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            22672
_diffrn_reflns_theta_full        28.9537
_diffrn_reflns_theta_max         28.95
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    0.471
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.4247
_exptl_crystal_description       needle
_exptl_crystal_F_000             1915.0325
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.2342
_refine_diff_density_min         -0.9298
_refine_diff_density_rms         0.1932
_refine_ls_d_res_high            0.7341
_refine_ls_d_res_low             11.1205
_refine_ls_goodness_of_fit_ref   1.0920
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    91
_refine_ls_number_parameters     543
_refine_ls_number_reflns         10485
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0920
_refine_ls_R_factor_all          0.1267
_refine_ls_R_factor_gt           0.0762
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0348P)^2^+11.0441P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1466
_refine_ls_wR_factor_ref         0.1637
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              25
_reflns_limit_h_min              -29
_reflns_limit_k_max              13
_reflns_limit_k_min              0
_reflns_limit_l_max              30
_reflns_limit_l_min              0
_reflns_number_gt                6635
_reflns_number_total             10485
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d1ce00457c2.cif
_cod_data_source_block           tdm22203_246_2_0m_a
_cod_depositor_comments
'Adding full bibliography for 7243143--7243153.cif.'
_cod_original_cell_volume        4259.6(15)
_cod_database_code               7243152
_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.a Ternary CH refined with riding coordinates:
 C12(H12), C13(H13), C11(H11), C17(H17), C14(H14), C18(H18), C15(H15),
 C16(H16), C19(H19)
2.b Secondary CH2 refined with riding coordinates:
 N1(H1a,H1b), C9(H9a,H9b), C39(H39a,H39b), C38(H38a,H38b), C26(H26a,H26b),
 C29(H29a,H29b), C27(H27a,H27b), C8(H8a,H8b), C31(H31a,H31b), C30(H30a,H30b),
 C28(H28a,H28b), C40(H40a,H40b), C42(H42a,H42b), C43(H43a,H43b), C41(H41a,H41b)
2.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C36(H36), C33(H33), C7(H7), C24(H24), C4(H4), C21(H21), C35(H35),
 C23(H23), C34(H34), C3(H3), C22(H22)
2.d Idealised Me refined as rotating group:
 C1(H1c,H1d,H1e)
;
_olex2_submission_special_instructions 'No special instructions were received'