Solvation/desolvation induced reversible distortion change and switching between spin crossover and single molecular magnet behaviour in a cobalt(II) complex.
Zenno, Hikaru; Sekine, Yoshihiro; Zhang, Zhongyue; Hayami, Shinya; Dalton transactions (Cambridge, England : 2003) 53 (2024) 5861–5870; doi:10.1039/d3dt03936f

data_7715151
_publ_section_title
;
 Solvation/desolvation induced reversible distortion change and switching
 between spin crossover and single molecular magnet behaviour in a
 cobalt(II) complex.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5861
_journal_page_last               5870
_journal_paper_doi               10.1039/d3dt03936f
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C44 H34 Co N6 O2, 2(Cl O4), 1.5(C H4 O)'
_chemical_formula_sum            'C45.5 H40 Cl2 Co N6 O11.5'
_chemical_formula_weight         984.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-12-13
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-12-19 deposited with the CCDC.	2024-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.515(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.8486(9)
_cell_length_b                   15.2034(7)
_cell_length_c                   16.2749(8)
_cell_measurement_reflns_used    6193
_cell_measurement_temperature    273
_cell_measurement_theta_max      30.4360
_cell_measurement_theta_min      2.5570
_cell_volume                     4514.9(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.15 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.15 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.15 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      273
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -84.00 -17.00   0.50   10.00    --   -7.82 -19.00 -60.00  134
  2  \w    -29.00   3.00   0.50   10.00    --   -7.82  77.00  60.00   64
  3  \w      4.00  58.00   0.50   10.00    --    8.68  57.00  60.00  108
  4  \w    -15.00  21.00   0.50   10.00    --    8.68 -77.00-150.00   72
  5  \w     29.00  54.00   0.50   10.00    --    8.68  57.00  90.00   50
  6  \w    -49.00 -17.00   0.50   10.00    --    8.68 -19.00 -60.00   64
;
_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      0.0284903000
_diffrn_orient_matrix_UB_12      -0.0298834000
_diffrn_orient_matrix_UB_13      -0.0018455000
_diffrn_orient_matrix_UB_21      -0.0260942000
_diffrn_orient_matrix_UB_22      -0.0341900000
_diffrn_orient_matrix_UB_23      -0.0118928000
_diffrn_orient_matrix_UB_31      -0.0041808000
_diffrn_orient_matrix_UB_32      0.0107270000
_diffrn_orient_matrix_UB_33      -0.0433957000
_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  0.0747
_diffrn_reflns_av_unetI/netI     0.0903
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            30143
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.546
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.568
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46645
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.15 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic light orange'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_description       block
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.493
_refine_diff_density_min         -0.695
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     651
_refine_ls_number_reflns         9216
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.1218
_refine_ls_R_factor_gt           0.0611
_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^)+(0.0834P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1469
_refine_ls_wR_factor_ref         0.1678
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5425
_reflns_number_total             9216
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03936f2.cif
_cod_data_source_block           220905_phometerpycoclo4_273k
_cod_depositor_comments
'Adding full bibliography for 7715150--7715153.cif.'
_cod_original_formula_sum        'C45.50 H40 Cl2 Co N6 O11.50'
_cod_database_code               7715151
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H N O Co Cl'
_chemical_oxdiff_usercomment     273K
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.972
_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 C(H,H,H) groups, All O(H) groups
2. Restrained distances
 H11-O11 = O11-C45
 1.25 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O8A) \\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(O9A)
\\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(O7A) \\sim Ueq, Uanis(O7) \\sim Ueq,
Uanis(O10A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Others
 Sof(O10A)=Sof(O7A)=Sof(O9A)=Sof(O8A)=Sof(Cl2A)=1-FVAR(1)
 Sof(Cl2)=Sof(O7)=Sof(O8)=Sof(O9)=Sof(O10)=FVAR(1)
 Fixed Sof: C45A(0.32) H45A(0.32) H45B(0.32) H45C(0.32) O11A(0.32) H11A(0.32)
 O11(0.18) H11(0.18) C45(0.18) H45D(0.18) H45E(0.18) H45F(0.18)
 Fixed Uiso: C45A(0.08) O11A(0.08) O11(0.08) C45(0.08)
5.a Aromatic/amide H refined with riding coordinates:
 C31(H31), C9(H9), C20(H20), C29(H29), C7(H7), C40(H40), C21(H21), C43(H43),
 C23(H23), C39(H39), C42(H42), C4(H4), C24(H24), C15(H15), C1(H1), C34(H34),
 C26(H26), C12(H12), C13(H13), C3(H3), C14(H14), C2(H2), C37(H37), C25(H25),
 C36(H36), C18(H18), C35(H35), C17(H17)
5.b Tetrahedral OH refined with riding coordinates:
 O11(H11)
5.c Idealised Me refined as rotating group:
 C44(H44A,H44B,H44C), C22(H22A,H22B,H22C), C47(H47A,H47B,H47C), C45A(H45A,H45B,
 H45C), C45(H45D,H45E,H45F)
5.d Idealised tetrahedral OH refined as rotating group:
 O12(H12A), O11A(H11A)
;
_shelx_res_checksum              36149
_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 3.372
_oxdiff_exptl_absorpt_empirical_full_min 0.586