Hydrogen-bond engineering induced ferroelastic phase transition in copper-based organic-inorganic hybrid thermochromic materials.
Deng, Xin; Zhou, Lin; Yan, Xin; Wang, Yan-Juan; Yang, Wen-Li; Lv, Hui-Peng; Tang, Yuan-Yuan; Chemical communications (Cambridge, England) 60 (2024) 14766–14769; doi:10.1039/d4cc04373a

data_7133906
_publ_section_title
;
 Hydrogen-bond engineering induced ferroelastic phase transition in
 copper-based organic-inorganic hybrid thermochromic materials.
;
_journal_issue                   99
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              14766
_journal_page_last               14769
_journal_paper_doi               10.1039/d4cc04373a
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'Cl4 Cu, 2(C6 H9 N2)'
_chemical_formula_sum            'C12 H18 Cl4 Cu N4'
_chemical_formula_weight         423.659
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_Int_Tables_number      15
_atom_sites_solution_primary     iterative
_audit_block_doi                 10.5517/ccdc.csd.cc2l4d7d
_audit_creation_date             2024-09-28
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-10-19 deposited with the CCDC.	2024-10-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.637(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3440(9)
_cell_length_b                   12.2584(7)
_cell_length_c                   14.3901(13)
_cell_measurement_reflns_used    2974
_cell_measurement_temperature    410.00(10)
_cell_measurement_theta_max      71.6090
_cell_measurement_theta_min      3.3280
_cell_volume                     1846.9(3)
_computing_cell_refinement       'CrysAlisPro 1.171.43.129a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.129a 64-bit (release 29-06-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.129a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      410.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.9600
_diffrn_measured_fraction_theta_max 0.9600
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     25.00  67.00   0.50    0.23    --   60.54-125.00-120.00   84
  2  \w     37.00  79.00   0.50    0.23    --   75.18 -94.00-120.00   84
  3  \w     39.00  69.00   0.50    0.23    --   60.54 -94.00 -90.00   60
  4  \w     36.00  93.00   0.50    0.23    --   75.18-125.00 -30.00  114
  5  \w     38.00  64.00   0.50    0.23    --   60.54 -94.00  90.00   52
  6  \w     43.00  82.00   0.50    0.23    --   75.18 -94.00 120.00   78
  7  \w     13.00  38.00   0.50    0.23    --   60.54 -30.00 120.00   50
  8  \w     11.00  38.00   0.50    0.23    --   60.54 -30.00  90.00   54
  9  \w     12.00  37.00   0.50    0.23    --   60.54 -30.00  30.00   50
 10  \w     12.00  38.00   0.50    0.23    --   60.54 -30.00-150.00   52
 11  \w     12.00  38.00   0.50    0.23    --   60.54 -30.00-180.00   52
 12  \w     40.00 114.00   0.50    0.23    --   75.12   0.00-180.00  148
 13  \w     75.00 101.00   0.50    0.23    --   60.54  30.00 -30.00   52
 14  \w     87.00 119.00   0.50    0.23    --   75.18  30.00  90.00   64
 15  \w     66.00 107.00   0.50    0.23    --   60.54  30.00  60.00   82
 16  \w    -90.00 -52.00   0.50    0.23    --  -60.72   0.00  30.00   76
 17  \w    -48.00 -22.00   0.50    0.23    --  -60.72   0.00  30.00   52
 18  \w    -67.00 -32.00   0.50    0.23    --  -75.50 125.00 -90.00   70
 19  \w    -77.00 -37.00   0.50    0.23    --  -75.50 125.00 150.00   80
 20  \w   -110.00 -35.00   0.50    0.23    --  -74.13   0.00 -60.00  150
 21  \w   -114.00 -76.00   0.50    0.23    --  -75.50 -30.00-150.00   76
 22  \w   -119.00 -94.00   0.50    0.23    --  -75.50-125.00-150.00   50
 23  \w   -114.00 -86.00   0.50    0.23    --  -74.13-125.00 -90.00   56
 24  \w   -117.00 -82.00   0.50    0.23    --  -75.50 -30.00  60.00   70
 25  \w   -123.00 -97.00   0.50    0.23    --  -74.13 -30.00 150.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0628395000
_diffrn_orient_matrix_UB_12      0.0319937000
_diffrn_orient_matrix_UB_13      -0.1118936000
_diffrn_orient_matrix_UB_21      -0.1119949000
_diffrn_orient_matrix_UB_22      -0.0777584000
_diffrn_orient_matrix_UB_23      -0.0133106000
_diffrn_orient_matrix_UB_31      -0.0718020000
_diffrn_orient_matrix_UB_32      0.0934779000
_diffrn_orient_matrix_UB_33      0.0272404000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0608
_diffrn_reflns_av_unetI/netI     0.0393
_diffrn_reflns_Laue_measured_fraction_full 0.9600
_diffrn_reflns_Laue_measured_fraction_max 0.9600
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4407
_diffrn_reflns_point_group_measured_fraction_full 0.9600
_diffrn_reflns_point_group_measured_fraction_max 0.9600
_diffrn_reflns_theta_full        66.5940
_diffrn_reflns_theta_max         66.59
_diffrn_reflns_theta_min         5.56
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.977
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38122
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.129a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic greenish green'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_description       block
_exptl_crystal_F_000             859.715
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.4793
_refine_diff_density_min         -0.8202
_refine_diff_density_rms         0.1298
_refine_ls_d_res_high            0.8400
_refine_ls_d_res_low             7.9614
_refine_ls_goodness_of_fit_ref   1.0162
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    15
_refine_ls_number_parameters     97
_refine_ls_number_reflns         1562
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0162
_refine_ls_R_factor_all          0.0838
_refine_ls_R_factor_gt           0.0690
_refine_ls_shift/su_max          -0.0004
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2029
_refine_ls_wR_factor_ref         0.2557
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -13
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                1159
_reflns_number_total             1562
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4cc04373a2.cif
_cod_data_source_block           LYL_0916_1_410K
_cod_depositor_comments
'Adding full bibliography for 7133906--7133908.cif.'
_cod_database_code               7133906
_chemical_oxdiff_formula         'C H N Cu Cl '
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C5(H5), C1(H1a), C2(H2)
2.b X=CH2 refined with riding coordinates:
 N2(H2a,H2b)
2.c Idealised Me refined as rotating group:
 C4(H4a,H4b,H4c)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 9.304
_oxdiff_exptl_absorpt_empirical_full_min 0.264