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_7715153
_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)'
_chemical_formula_sum            'C44 H34 Cl2 Co N6 O10'
_chemical_formula_weight         936.60
_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             2023-07-13
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-10-21 deposited with the CCDC.	2024-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.289(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.9555(15)
_cell_length_b                   15.5934(11)
_cell_length_c                   16.1013(13)
_cell_measurement_reflns_used    3249
_cell_measurement_temperature    300
_cell_measurement_theta_max      30.5330
_cell_measurement_theta_min      2.5560
_cell_volume                     4228.5(6)
_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      300
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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    -82.00 -17.00   0.50   10.00    --   -8.15 -19.00 -60.00  130
  2  \w    -47.00 -13.00   0.50   10.00    --   -8.15 -57.00  90.00   68
  3  \w    -29.00  -1.00   0.50   10.00    --   -8.15  77.00  60.00   56
  4  \w     -3.00  52.00   0.50   10.00    --    8.47  57.00  90.00  110
  5  \w    -13.00  19.00   0.50   10.00    --    8.47 -77.00-150.00   64
  6  \w     21.00  50.00   0.50   10.00    --    8.47  57.00 -30.00   58
;
_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      0.0326920000
_diffrn_orient_matrix_UB_12      -0.0288130000
_diffrn_orient_matrix_UB_13      0.0125152000
_diffrn_orient_matrix_UB_21      -0.0263231000
_diffrn_orient_matrix_UB_22      -0.0349537000
_diffrn_orient_matrix_UB_23      -0.0153656000
_diffrn_orient_matrix_UB_31      0.0030651000
_diffrn_orient_matrix_UB_32      0.0042833000
_diffrn_orient_matrix_UB_33      -0.0425820000
_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  0.0971
_diffrn_reflns_av_unetI/netI     0.1132
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26132
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.419
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.599
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64252
_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    1.471
_exptl_crystal_description       plate
_exptl_crystal_F_000             1924
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.091
_refine_diff_density_min         -0.458
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     570
_refine_ls_number_reflns         8628
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1723
_refine_ls_R_factor_gt           0.0849
_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^)+(0.1296P)^2^+0.5128P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2106
_refine_ls_wR_factor_ref         0.2540
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4281
_reflns_number_total             8628
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03936f2.cif
_cod_data_source_block           220719_phometerpycoclo4_300k_110k_1_300_00
_cod_depositor_comments
'Adding full bibliography for 7715150--7715153.cif.'
_cod_database_code               7715153
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H N O Co Cl'
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.971
_reflns_odcompleteness_completeness 99.77
_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
2.a Aromatic/amide H refined with riding coordinates:
 C29(H29), C26(H26), C40(H40), C9(H9), C25(H25), C23(H23), C39(H39), C31(H31),
 C7(H7), C12(H12), C42(H42), C24(H24), C43(H43), C15(H15), C1(H1), C4(H4),
 C3(H3), C21(H21), C2(H2), C13(H13), C37(H37), C34(H34), C14(H14), C20(H20),
 C36(H36), C17(H17), C18(H18), C35(H35)
2.b Idealised Me refined as rotating group:
 C44(H44A,H44B,H44C), C22(H22A,H22B,H22C)
;
_shelx_res_checksum              26610
_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 2.261
_oxdiff_exptl_absorpt_empirical_full_min 0.578