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_7715150
_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         984.696
_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'
_symmetry_Int_Tables_number      14
_audit_creation_date             2023-12-11
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2023.11.24 svn.r209d9fb2 for OlexSys, GUI svn.r6697)
;
_audit_update_record
;
2023-12-19 deposited with the CCDC.	2024-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.196(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.5673(4)
_cell_length_b                   14.9013(3)
_cell_length_c                   16.1628(3)
_cell_measurement_reflns_used    13517
_cell_measurement_temperature    110
_cell_measurement_theta_max      30.7360
_cell_measurement_theta_min      2.6710
_cell_volume                     4335.31(16)
_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 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-dev (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      110.00
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9991
_diffrn_measured_fraction_theta_max 0.9991
_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    -55.00  -7.00   0.50   10.89    --   -7.90 -57.00 -30.00   96
  2  \w    -41.00   1.00   0.50   10.89    --   -7.90 -57.00  90.00   84
  3  \w     21.00  86.00   0.50   10.89    --    8.68  19.00-120.00  130
  4  \w      3.00  55.00   0.50   10.89    --    8.68  57.00 -60.00  104
  5  \w    -15.00  30.00   0.50   10.89    --    8.68 -77.00 120.00   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_unetI/netI     0.0416
_diffrn_reflns_Laue_measured_fraction_full 0.9991
_diffrn_reflns_Laue_measured_fraction_max 0.9991
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            30148
_diffrn_reflns_point_group_measured_fraction_full 0.9991
_diffrn_reflns_point_group_measured_fraction_max 0.9991
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.57
_exptl_absorpt_coefficient_mu    0.591
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44614
_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            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_description       block
_exptl_crystal_F_000             2036.007
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.9246
_refine_diff_density_min         -0.6024
_refine_diff_density_rms         0.0940
_refine_ls_d_res_high            0.8000
_refine_ls_d_res_low             7.9305
_refine_ls_goodness_of_fit_ref   1.0230
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    83
_refine_ls_number_parameters     656
_refine_ls_number_reflns         8866
_refine_ls_number_restraints     136
_refine_ls_restrained_S_all      1.0140
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0433
_refine_ls_shift/su_max          -0.0010
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0662P)^2^+3.7235P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1163
_refine_ls_wR_factor_ref         0.1225
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              22
_reflns_limit_h_min              -23
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                7196
_reflns_number_total             8866
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3dt03936f2.cif
_cod_data_source_block           220719_phometerpycoclo4_drumeoh_110k
_cod_depositor_comments
'Adding full bibliography for 7715150--7715153.cif.'
_cod_database_code               7715150
_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
 Cl1-O8 \\sim Cl1a-O8a
 with sigma of 0.02
 Cl1-O10 \\sim Cl1a-O10a
 with sigma of 0.02
 Cl1-O7 \\sim Cl1a-O7a
 with sigma of 0.02
 Cl1-O9 \\sim Cl1a-O9a
 with sigma of 0.02
 O8-O10 \\sim O8a-O10a
 with sigma of 0.04
 O8-O7 \\sim O8a-O7a
 with sigma of 0.04
 O8-O9 \\sim O8a-O9a
 with sigma of 0.04
 O10-O7 \\sim O10a-O7a
 with sigma of 0.04
 O10-O9 \\sim O10a-O9a
 with sigma of 0.04
 O7-O9 \\sim O7a-O9a
 with sigma of 0.04
 O8a-O10a \\sim O8a-O7a \\sim O8a-O9a \\sim O10a-O7a \\sim O10a-O9a \\sim
O7a-O9a
 with sigma of 0.002
 Cl1a-O8a \\sim Cl1a-O10a \\sim Cl1a-O7a \\sim Cl1a-O9a
 with sigma of 0.001
 O8-O10 \\sim O8-O7 \\sim O8-O9 \\sim O10-O7 \\sim O10-O9 \\sim O7-O9
 with sigma of 0.002
 Cl1-O8 \\sim Cl1-O10 \\sim Cl1-O7 \\sim Cl1-O9
 with sigma of 0.001
 O45-C12 \\sim O45a-C12a
 with sigma of 0.02
 O45a-C12a \\sim O45-C12
 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
O45a \\sim C12a: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C12 \\sim O45: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
4. Rigid body (RIGU) restrains
 O45, C12
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O8, Cl1, O10, O7, O9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl1a, O8a, O10a, O7a, O9a
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O8a, Cl1a, O10a, O7a, O9a
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(O8a)=Sof(Cl1a)=Sof(O10a)=Sof(O7a)=Sof(O9a)=1-FVAR(1)
 Sof(Cl1)=Sof(O8)=Sof(O10)=Sof(O7)=Sof(O9)=FVAR(1)
 Fixed Sof: O45(0.32) H45(0.32) C12(0.32) H12a(0.32) H12b(0.32) H12c(0.32)
 O45a(0.18) H45a(0.18) C12a(0.18) H12d(0.18) H12e(0.18) H12f(0.18)
6.a Aromatic/amide H refined with riding coordinates:
 C29(H29), C9(H9), C31(H31), C4(H4), C13(H13), C36(H36), C7(H7), C37(H37),
 C34(H34), C23(H23), C43(H43), C24(H24), C40(H40), C15(H15), C47(H47), C20(H20),
  C42(H42), C39(H39), C2(H2), C3(H3), C25(H25), C21(H21), C14(H14), C1(H1),
 C35(H35), C26(H26), C18(H18), C17(H17)
6.b Idealised Me refined as rotating group:
 C44(H44a,H44b,H44c), C22(H22a,H22b,H22c), C46(H46a,H46b,H46c), C12(H12a,H12b,
 H12c), C12a(H12d,H12e,H12f)
6.c Idealised tetrahedral OH refined as rotating group:
 O11(H11), O45(H45), O45a(H45a)
;
_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
;