Negative to positive axial thermal expansion switching of an organic crystal: contribution to multistep photoactuation.
Hasebe, Shodai; Hagiwara, Yuki; Ueno, Takashi; Asahi, Toru; Koshima, Hideko; Chemical science 15 (2024) 1088–1097; doi:10.1039/d3sc04796b

data_1570542
_publ_section_title
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 Negative to positive axial thermal expansion switching of an organic
 crystal: contribution to multistep photoactuation.
;
_journal_issue                   3
_journal_name_full               'Chemical science'
_journal_page_first              1088
_journal_page_last               1097
_journal_paper_doi               10.1039/d3sc04796b
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C21 H26 N2 O3'
_chemical_formula_sum            'C21 H26 N2 O3'
_chemical_formula_weight         354.44
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-06-06
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-08-31 deposited with the CCDC.	2023-12-11 downloaded from the CCDC.
;
_cell_angle_alpha                101.333(7)
_cell_angle_beta                 92.155(6)
_cell_angle_gamma                101.650(7)
_cell_formula_units_Z            2
_cell_length_a                   6.0455(6)
_cell_length_b                   10.3195(10)
_cell_length_c                   16.7114(17)
_cell_measurement_reflns_used    7964
_cell_measurement_temperature    279.95
_cell_measurement_theta_max      68
_cell_measurement_theta_min      4
_cell_volume                     997.93(18)
_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    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      279.95
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  RAPID
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0644
_diffrn_reflns_av_unetI/netI     0.0642
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11113
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.249
_diffrn_reflns_theta_min         4.473
_exptl_absorpt_coefficient_mu    0.634
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.6222
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ABSCOR(Rigaku,1995)
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.180
_exptl_crystal_description       prism
_exptl_crystal_F_000             380
_exptl_crystal_size_max          1
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.167
_refine_diff_density_min         -0.246
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         3562
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.1131
_refine_ls_R_factor_gt           0.0738
_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^)+(0.0755P)^2^+0.1630P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1741
_refine_ls_wR_factor_ref         0.1973
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2124
_reflns_number_total             3562
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc04796b3.cif
_cod_data_source_block           6point8degC
_cod_depositor_comments
'Adding full bibliography for 1570536--1570543.cif.'
_cod_database_code               1570542
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Uiso/Uaniso restraints and constraints
C00I \\sim C00R \\sim C2 \\sim C1: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C00I \\sim C00Q \\sim C00P \\sim C00O: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
3. Rigid body (RIGU) restrains
 C00I, C00R, C2, C1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C00I, C00Q, C00P, C00O
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C00R)=Sof(H00Y)=Sof(H)=Sof(HA)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C2)=
 Sof(H2A)=Sof(H2B)=Sof(H2C)=1-FVAR(1)
 Sof(C00O)=Sof(H00P)=Sof(H00Q)=Sof(H00R)=Sof(C00P)=Sof(H00S)=Sof(H00T)=
 Sof(H00U)=Sof(C00Q)=Sof(H00V)=Sof(H00W)=Sof(H00X)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C009(H009), C00B(H00B), C00C(H00C), C00D(H00D), C00G(H00G), C00J(H00J),
 C00K(H00K)
5.b Idealised Me refined as rotating group:
 C00L(H00A,H00E,H00F), C00M(H00H,H00I,H00L), C00N(H00M,H00N,H00O), C00O(H00P,
 H00Q,H00R), C00P(H00S,H00T,H00U), C00Q(H00V,H00W,H00X), C00R(H00Y,H,HA),
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C)
5.c Idealised tetrahedral OH refined as rotating group:
 O001(H001)
;
_shelx_res_checksum              68253
_shelx_hkl_checksum              55188
_olex2_submission_special_instructions 'No special instructions were received'