A five- and six-coordinated two-dimensional metal halide organic-inorganic phase transition material.
Chen, Hui-Ping; Wang, Zhen-Yu; Qi, Jun-Chao; Peng, Hang; Yang, Tian-En; Zhang, Xiao-Xuan; Luo, Xin-Yu; Liao, Wei-Qiang; Chemical communications (Cambridge, England) 61 (2025) 16636–16639; doi:10.1039/d5cc04326c

data_7135041
_publ_section_title
;
 A five- and six-coordinated two-dimensional metal halide
 organic-inorganic phase transition material.
;
_journal_issue                   85
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              16636
_journal_page_last               16639
_journal_paper_doi               10.1039/d5cc04326c
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'Cd3 Cl7, C8 H20 N'
_chemical_formula_sum            'C8 H20 Cd3 Cl7 N'
_chemical_formula_weight         715.60
_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
_audit_creation_date             2025-09-17
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-09-17 deposited with the CCDC.	2025-09-22 downloaded from the CCDC.
;
_cell_angle_alpha                66.714(2)
_cell_angle_beta                 82.325(2)
_cell_angle_gamma                70.712(3)
_cell_formula_units_Z            2
_cell_length_a                   7.8180(3)
_cell_length_b                   11.1147(3)
_cell_length_c                   13.4404(2)
_cell_measurement_reflns_used    7840
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      73.2080
_cell_measurement_theta_min      3.5090
_cell_volume                     1012.55(6)
_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  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      93.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11103
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        66.576
_diffrn_reflns_theta_max         66.576
_diffrn_reflns_theta_min         3.580
_diffrn_source                   'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    33.398
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38696
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.347
_exptl_crystal_description       needle
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.199
_refine_diff_density_min         -1.339
_refine_diff_density_rms         0.189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         3541
_refine_ls_number_restraints     188
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0314
_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^)+(0.0670P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0874
_refine_ls_wR_factor_ref         0.0891
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3270
_reflns_number_total             3541
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc04326c2.cif
_cod_data_source_block           1_93K
_cod_depositor_comments
'Adding full bibliography for 7135041--7135042.cif.'
_cod_original_cell_volume        1012.54(5)
_cod_database_code               7135041
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.076
_shelx_estimated_absorpt_t_min   0.034
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C8-C6 = C8A-C6A
 1.53 with sigma of 0.01
 C7A-C6A = C7-C6
 1.53 with sigma of 0.01
 C2A-C1A = C2-C1
 1.53 with sigma of 0.01
 C4A-C3A = C4-C3
 1.53 with sigma of 0.01
 N1-C6 = N1-C6A
 1.52 with sigma of 0.01
 C2A-C1A \\sim C2-C1
 with sigma of 0.02
 N1-C1A \\sim N1-C1
 with sigma of 0.02
 C4-C3 \\sim C4A-C3A
 with sigma of 0.02
 C5-C3 \\sim C5A-C3A
 with sigma of 0.02
 N1-C3A \\sim N1-C3
 with sigma of 0.02
 C7-C6 \\sim C7A-C6A
 with sigma of 0.02
 C8-C6 \\sim C8A-C6A
 with sigma of 0.02
 N1-C6 \\sim N1-C6A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1 \\sim C1A \\sim C2 \\sim C2A: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C3 \\sim C3A \\sim C4 \\sim C4A \\sim C5 \\sim C5A: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
C6 \\sim C6A \\sim C7 \\sim C7A \\sim C8 \\sim C8A: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
4. Same fragment restrains
{C6, C7, C8} sigma for 1-2: 0.02, 1-3: 0.02
as in
{C6A, C7A, C8A}
{C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.02
as in
{C3A, C4A, C5A}
{C1, C2} sigma for 1-2: 0.02, 1-3: 0.02
as in
{C1A, C2A}
5. Others
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C3)=Sof(H3)=
 Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=Sof(C6)=
 Sof(H6)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=
 1-FVAR(1)
 Sof(C1A)=Sof(H1C)=Sof(H1D)=Sof(C2A)=Sof(H2D)=Sof(H2E)=Sof(H2F)=Sof(C3A)=
 Sof(H3A)=Sof(C4A)=Sof(H4D)=Sof(H4E)=Sof(H4F)=Sof(C5A)=Sof(H5D)=Sof(H5E)=
 Sof(H5F)=Sof(C6A)=Sof(H6A)=Sof(C7A)=Sof(H7D)=Sof(H7E)=Sof(H7F)=Sof(C8A)=
 Sof(H8D)=Sof(H8E)=Sof(H8F)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 N1(H1), C3(H3), C3A(H3A), C6(H6), C6A(H6A)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C1A(H1C,H1D)
6.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C2A(H2D,H2E,H2F), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C4A(H4D,
 H4E,H4F), C5A(H5D,H5E,H5F), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C7A(H7D,H7E,H7F),
  C8A(H8D,H8E,H8F)
;
_shelx_res_checksum              68332
_olex2_submission_special_instructions 'No special instructions were received'