Hydrogen-Bonded Cobalt(II)-Organic Framework: Normal and Reverse Spin-Crossover Behaviours
KANETOMO, Takuya; Ni, Zhen; Enomoto, Masaya; Dalton Transactions  (2022) –; doi:10.1039/D2DT00453D

data_7709684
_publ_section_title
;
 Hydrogen-Bonded Cobalt(II)-Organic Framework: Normal and Reverse
 Spin-Crossover Behaviours
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00453D
_journal_year                    2022
_chemical_formula_moiety         'C34 H20 Co N6 O8'
_chemical_formula_sum            'C34 H20 Co N6 O8'
_chemical_formula_weight         699.49
_chemical_melting_point          445
_chemical_name_systematic
'cobalt(II) bis(5H-2.2':6',2"-terpyridine-5,5"-diyl biscarboxylato)'
_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_Hall           '-P 4bc'
_space_group_name_H-M_alt        'P 42/n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-11-25
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-01-19 deposited with the CCDC.	2022-03-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3814(2)
_cell_length_b                   14.3814(2)
_cell_length_c                   18.3531(4)
_cell_measurement_reflns_used    10853
_cell_measurement_temperature    93
_cell_measurement_theta_max      28.9860
_cell_measurement_theta_min      2.2120
_cell_volume                     3795.87(11)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      93
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.891
_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    -61.00  77.00   0.50    2.15    --   -4.70  28.00 -30.00  276
  2  \w     61.00  89.00   0.50    2.15    --    4.70  46.00-180.00   56
  3  \w    -31.00  -5.00   0.50    2.15    --    4.70  46.00-180.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0150559000
_diffrn_orient_matrix_UB_12      -0.0441446000
_diffrn_orient_matrix_UB_13      -0.0125585000
_diffrn_orient_matrix_UB_21      0.0466045000
_diffrn_orient_matrix_UB_22      0.0161091000
_diffrn_orient_matrix_UB_23      -0.0005286000
_diffrn_orient_matrix_UB_31      0.0058224000
_diffrn_orient_matrix_UB_32      -0.0149483000
_diffrn_orient_matrix_UB_33      0.0365529000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_unetI/netI     0.0204
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.891
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            22752
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.891
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.030
_diffrn_reflns_theta_min         2.219
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Mo) X-ray DW Source'
_exptl_absorpt_coefficient_mu    0.505
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.522
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_description       block
_exptl_crystal_F_000             1428
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: N,N-dimethylformamide, water, 1,4-dioxane'
_exptl_crystal_size_max          0.364
_exptl_crystal_size_mid          0.186
_exptl_crystal_size_min          0.128
_refine_diff_density_max         0.270
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         4512
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0311
_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^)+(0.0398P)^2^+1.1864P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0807
_refine_ls_wR_factor_ref         0.0830
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3811
_reflns_number_total             4512
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00453d2.cif
_cod_data_source_block           exp_2621
_cod_original_cell_volume        3795.87(13)
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_database_code               7709684
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C20 H15 O5 N4 Co'
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C15(H15), C1(H1), C4(H4), C9(H9), C3(H3), C8(H8), C12(H12), C13(H13)
2.b Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              85818
_shelx_fab_checksum              65139
_platon_squeeze_void_probe_radius 1.20
_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 1.453
_oxdiff_exptl_absorpt_empirical_full_min 0.730