Improper ferroelastic phase transition in a hydrogen-bonded metallocyanide-based (azetidinium)<sub>2</sub>(H<sub>3</sub>O)[Co(CN)<sub>6</sub>] framework.
Moskwa, Marcin; Sobieszczyk, Paweł; Mikurenda, Julia W.; Zieliński, Piotr; Rok, Magdalena; Chemical communications (Cambridge, England) 59 (2023) 5535–5538; doi:10.1039/d3cc01253k

data_7131513
_publ_section_title
;
 Improper ferroelastic phase transition in a hydrogen-bonded
 metallocyanide-based
 (azetidinium)<sub>2</sub>(H<sub>3</sub>O)[Co(CN)<sub>6</sub>] framework.
;
_journal_issue                   37
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              5535
_journal_page_last               5538
_journal_paper_doi               10.1039/d3cc01253k
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         '2(C3 H8 N 1+), H3 O 1+, C6 Co N6 3-'
_chemical_formula_sum            'C12 H19 Co N8 O'
_chemical_formula_weight         350.28
_space_group_crystal_system      trigonal
_space_group_IT_number           166
_space_group_name_Hall           '-R 3 2"'
_space_group_name_H-M_alt        'R -3 m :H'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   direct
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2023-03-10 deposited with the CCDC.	2023-04-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   8.4901(3)
_cell_length_b                   8.4901(3)
_cell_length_c                   41.463(2)
_cell_measurement_reflns_used    1713
_cell_measurement_temperature    308(2)
_cell_measurement_theta_max      27.7380
_cell_measurement_theta_min      3.6990
_cell_volume                     2588.31(18)
_computing_cell_refinement       'CrysAlisPro 1.171.41.80a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.80a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.80a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Diamond 4.0'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      308(2)
_diffrn_detector_area_resol_mean 10.3456
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0197
_diffrn_reflns_av_unetI/netI     0.0138
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            4115
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         27.495
_diffrn_reflns_theta_min         3.397
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.008
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85607
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.80a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1092
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.140
_refine_diff_density_max         0.458
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     74
_refine_ls_number_reflns         790
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.278
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0401
_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^)+(0.0489P)^2^+6.2353P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1034
_refine_ls_wR_factor_ref         0.1083
_reflns_Friedel_coverage         0.000
_reflns_number_gt                659
_reflns_number_total             790
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc01253k3.cif
_cod_data_source_block           aze308
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7131513--7131514.cif.
;
_cod_original_cell_volume        2588.3(2)
_cod_database_code               7131513
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.839
_shelx_estimated_absorpt_t_max   0.872
_shelx_res_checksum              10387
_shelx_hkl_checksum              3405