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_7133907
_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         423.64
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2kwhsr
_audit_creation_date             2024-05-29
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-10-19 deposited with the CCDC.	2024-10-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.345(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3776(3)
_cell_length_b                   8.3515(2)
_cell_length_c                   15.9482(3)
_cell_measurement_reflns_used    4008
_cell_measurement_temperature    299.12(10)
_cell_measurement_theta_max      76.0250
_cell_measurement_theta_min      6.2210
_cell_volume                     1778.75(7)
_computing_cell_refinement       'CrysAlisPro 1.171.42.79a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.79a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.79a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      299.12(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.963
_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     35.00  60.00   0.50    0.14    --  108.36 -61.00 -90.00   50
  2  \w     75.00 100.00   0.50    0.14    --  108.36 -77.00   0.00   50
  3  \w     38.00  67.00   0.50    0.14    --  108.36 -77.00   0.00   58
  4  \w     35.00  60.00   0.50    0.14    --  108.36 -61.00 -30.00   50
  5  \w     42.00  73.00   0.50    0.14    --  108.36 -61.00  60.00   62
  6  \w     35.00 101.00   0.50    0.14    --  108.36 -75.00 133.00  132
  7  \w    -12.00  22.00   0.50    0.05    --   45.20 -75.00 133.00   68
  8  \w    -25.00  25.00   0.50    0.05    --   45.20 -19.00 120.00  100
  9  \w    -29.00  27.00   0.50    0.05    --   45.20 -19.00 -30.00  112
 10  \w    120.00 178.00   0.50    0.14    --  108.36  77.00   0.00  116
 11  \w     85.00 163.00   0.50    0.14    --  108.36  75.00 -98.00  156
 12  \w     90.00 173.00   0.50    0.14    --  108.36  30.00-150.00  166
 13  \w     97.00 178.00   0.50    0.14    --  108.36  30.00-180.00  162
 14  \w     45.00  70.00   0.50    0.05    --   45.20  75.00 -98.00   50
 15  \w    -65.00  28.00   0.50    0.05    --  -45.20  75.00 -98.00  186
 16  \w    -64.00 -28.00   0.50    0.14    -- -102.00  61.00-120.00   72
 17  \w    -58.00 -28.00   0.50    0.14    -- -102.00  75.00 -98.00   60
 18  \w    -84.00 -59.00   0.50    0.14    -- -102.00  75.00 -98.00   50
 19  \w    -69.00 -28.00   0.50    0.14    -- -102.00  61.00 -30.00   82
 20  \w    -60.00 -32.00   0.50    0.14    -- -102.00  61.00  90.00   56
 21  \w    -69.00 -34.00   0.50    0.14    -- -102.00  61.00 120.00   70
 22  \w   -153.00-127.00   0.50    0.14    -- -102.00 -75.00 133.00   52
 23  \w   -100.00 -23.00   0.50    0.05    --  -45.20 -75.00 133.00  154
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0652017000
_diffrn_orient_matrix_UB_12      0.1430202000
_diffrn_orient_matrix_UB_13      0.0304677000
_diffrn_orient_matrix_UB_21      0.0152100000
_diffrn_orient_matrix_UB_22      0.0467873000
_diffrn_orient_matrix_UB_23      -0.0918517000
_diffrn_orient_matrix_UB_31      -0.0938727000
_diffrn_orient_matrix_UB_32      0.1068037000
_diffrn_orient_matrix_UB_33      -0.0006772000
_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  0.0279
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            5781
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.238
_diffrn_reflns_theta_min         5.557
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.244
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47109
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.79a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic orangish orange'
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_description       block
_exptl_crystal_F_000             860
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.522
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       0.00058(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     98
_refine_ls_number_reflns         1790
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0611P)^2^+1.1832P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1043
_refine_ls_wR_factor_ref         0.1069
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1629
_reflns_number_total             1790
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc04373a2.cif
_cod_data_source_block           lyl_240406_5_300k-r
_cod_depositor_comments
'Adding full bibliography for 7133906--7133908.cif.'
_cod_database_code               7133907
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C H  N O Cu Cl '
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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), C3(H3), C6(H6), C2(H2)
2.b X=CH2 refined with riding coordinates:
 N2(H2A,H2B)
2.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C)
;
_shelx_res_checksum              98968
_shelx_hkl_checksum              44493
_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 2.786
_oxdiff_exptl_absorpt_empirical_full_min 0.488