Thermally responsive morphological change of layered coordination polymer induced by disordering/ordering of flexible alkyl chains
Omoto, Kenichiro; Aoyama, Shota; Galica, Tomasz; Nishibori, Eiji; Katao, Shohei; Yasuhara, Kazuma; Rapenne, Gwenael; Dalton Transactions  (2022) –; doi:10.1039/D2DT03142F

data_7711667
_publ_section_title
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 Thermally responsive morphological change of layered coordination polymer
 induced by disordering/ordering of flexible alkyl chains
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT03142F
_journal_year                    2022
_chemical_formula_moiety         'C24 H36 O5 Zn'
_chemical_formula_sum            'C24 H36 O5 Zn'
_chemical_formula_weight         469.90
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-03-04
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-08-02 deposited with the CCDC.	2022-11-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.95(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.3454(16)
_cell_length_b                   16.8251(13)
_cell_length_c                   23.326(14)
_cell_measurement_reflns_used    942
_cell_measurement_temperature    450(2)
_cell_measurement_theta_max      7.0800
_cell_measurement_theta_min      1.5890
_cell_volume                     2881.1(19)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2008)'
_diffrn_ambient_temperature      450.00
_diffrn_detector_area_resol_mean 5.8410
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'SP-ring8 BL02B1'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.24792
_diffrn_reflns_av_R_equivalents  0.1704
_diffrn_reflns_av_unetI/netI     0.0977
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            19076
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        8.555
_diffrn_reflns_theta_max         8.913
_diffrn_reflns_theta_min         1.587
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.063
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.083
_exptl_crystal_description       block
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.454
_refine_diff_density_min         -0.230
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         3027
_refine_ls_number_restraints     131
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.2526
_refine_ls_R_factor_gt           0.1156
_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^)+(0.1863P)^2^+0.2040P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3147
_refine_ls_wR_factor_ref         0.4144
_reflns_Friedel_coverage         0.000
_reflns_number_gt                913
_reflns_number_total             3027
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03142f3.cif
_cod_data_source_block           450K
_cod_database_code               7711667
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.994
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C16-O1
 1.43 with sigma of 0.02
 C16-C17
 2.4 with sigma of 0.04
 O1-C18
 2.33 with sigma of 0.04
3. Restrained planarity
 C17, C18, C19, C21, O1, C16
 with sigma of 0.1
4. Rigid bond restraints
 C5, C4, C3, C2, C1, C6, C7, C8, C9, C10, C12, C11, C13, C14, C15, C16
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
Uanis(C16) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C13)
\\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C10) \\sim Ueq,
Uanis(C9) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C6) \\sim
Ueq, Uanis(C5) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C2)
\\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms
of 0.2
6. Others
 Fixed Sof: O1(0.5) C16(0.5) H16A(0.5) H16B(0.5) C1(0.5) H1A(0.5) H1B(0.5)
 H1C(0.5) C2(0.5) H2A(0.5) H2B(0.5) C3(0.5) H3A(0.5) H3B(0.5) C4(0.5) H4A(0.5)
 H4B(0.5) C5(0.5) H5A(0.5) H5B(0.5) C6(0.5) H6A(0.5) H6B(0.5) C7(0.5) H7A(0.5)
 H7B(0.5) C8(0.5) H8A(0.5) H8B(0.5) C9(0.5) H9A(0.5) H9B(0.5) C10(0.5)
 H10A(0.5) H10B(0.5) C11(0.5) H11A(0.5) H11B(0.5) C12(0.5) H12A(0.5) H12B(0.5)
 C13(0.5) H13A(0.5) H13B(0.5) C14(0.5) H14A(0.5) H14B(0.5) C15(0.5) H15A(0.5)
 H15B(0.5)
7.a Free rotating group:
 C16(C1,C2,C3,C4,C5,C6,C7,C8,C9,C10,C11,C12,C13,C14,C15)
7.b Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,
 H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B)
7.c Aromatic/amide H refined with riding coordinates:
 C18(H18), C21(H21)
7.d Idealised Me refined with riding coordinates:
 C1(H1A,H1B,H1C)
;
_shelx_res_checksum              37168
_olex2_submission_special_instructions 'No special instructions were received'