Field-induced Single Ion Magnet behaviour in discrete and one-dimensional complexes containing the bis(1-methylimidazol-2-yl)ketone]-containing cobalt(II) building units
Jiménez, Juan-Ramón; Xu, Buqin; El Said, Hasnaa; Li, Yanling; von Bardeleben, Jurgen; Chamoreau, Lise-Marie; Lescouezec, Rodrigue; Shova, Sergiu; Visinescu, Diana; Alexandru, Maria-Gabriela; Cano, Joan; Julve, Miguel; Dalton Transactions  (2021) –; doi:10.1039/D1DT02441H

data_7708550
_publ_section_title
;
 Field-induced Single Ion Magnet behaviour in discrete and one-dimensional
 complexes containing the bis(1-methylimidazol-2-yl)ketone]-containing
 cobalt(II) building units
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02441H
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C33 H28 Co3 N16 O3 S, 1.4(H2 O)'
_chemical_formula_sum            'C33 H30.8 Co3 N16 O4.4 S'
_chemical_formula_weight         930.78
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-03-23
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-03-23 deposited with the CCDC.	2021-10-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.09(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.231(3)
_cell_length_b                   8.1876(11)
_cell_length_c                   21.110(4)
_cell_measurement_reflns_used    1441
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18.6140
_cell_measurement_theta_min      1.9260
_cell_volume                     2102.1(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0797
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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 -37.00   1.00   60.00    --  -15.21-178.00 -60.00   47
  2  \w      4.00  86.00   1.00   60.00    --   17.63  38.00-120.00   82
  3  \w     -3.00  88.00   1.00   60.00    --   17.63  19.00  60.00   91
  4  \w    -52.00  81.00   1.00   60.00    --   17.63   0.00-150.00  133
  5  \w     63.00  89.00   1.00   60.00    --   17.79 178.00  30.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0221015000
_diffrn_orient_matrix_UB_12      0.0543094000
_diffrn_orient_matrix_UB_13      0.0214907000
_diffrn_orient_matrix_UB_21      0.0517085000
_diffrn_orient_matrix_UB_22      0.0033828000
_diffrn_orient_matrix_UB_23      0.0186905000
_diffrn_orient_matrix_UB_31      0.0154153000
_diffrn_orient_matrix_UB_32      0.0674153000
_diffrn_orient_matrix_UB_33      -0.0182059000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1124
_diffrn_reflns_av_unetI/netI     0.2052
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            14566
_diffrn_reflns_point_group_measured_fraction_full 0.926
_diffrn_reflns_point_group_measured_fraction_max 0.926
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.674
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.277
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96153
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
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       prism
_exptl_crystal_F_000             946
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.610
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.105
_refine_ls_abs_structure_details
;
 Flack x determined using 956 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     531
_refine_ls_number_reflns         6888
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.1665
_refine_ls_R_factor_gt           0.0869
_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^)+(0.0399P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1326
_refine_ls_wR_factor_ref         0.1638
_reflns_Friedel_coverage         0.850
_reflns_Friedel_fraction_full    0.852
_reflns_Friedel_fraction_max     0.852
_reflns_number_gt                3766
_reflns_number_total             6888
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02441h2.cif
_cod_data_source_block           shi_4304_gaal
_cod_original_cell_volume        2102.0(7)
_cod_original_formula_sum        'C33 H30.80 Co3 N16 O4.40 S'
_cod_database_code               7708550
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C30H30N8O2Co2
_chemical_oxdiff_usercomment     'C0DPPCobik_ orange'
_shelx_estimated_absorpt_t_max   0.916
_shelx_estimated_absorpt_t_min   0.832
_reflns_odcompleteness_completeness 99.98
_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,H) groups
2. Restrained distances
 S1-C33X \\sim S1-C33 \\sim S1-C32 \\sim S1-C32X
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C33) \\sim Ueq, Uanis(C33X) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C32X) \\sim Ueq, Uanis(C32) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C20) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C32) = Uanis(C32X)
Uanis(C33X) = Uanis(C33)
4. Others
 Sof(C32X)=Sof(H32D)=Sof(H32E)=Sof(H32F)=Sof(C33X)=Sof(H33D)=Sof(H33E)=
 Sof(H33F)=1-FVAR(1)
 Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=
 FVAR(1)
 Fixed Sof: O2W(0.2) H2WA(0.2) H2WB(0.2) O4W(0.5) H4WA(0.5) H4WB(0.5) O1W(0.2)
 H1WA(0.2) H1WB(0.2) O3W(0.5) H3WA(0.5) H3WB(0.5)
5.a Riding coordinates:
 C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C32X(H32D,H32E,H32F), C33X(H33D,
 H33E,H33F), O2W(H2WA,H2WB), O4W(H4WA,H4WB), O1W(H1WA,H1WB), O3W(H3WA,H3WB)
5.b Rotating group:
 O0AA(H0AA,H0AB)
5.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C9(H9), C11(H11), C12(H12), C13(H13),
 C14(H14), C23(H23), C24(H24), C30(H30), C31(H31)
5.d Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C29(H29A,H29B,H29C)
;
_shelx_res_checksum              23380
_shelx_hkl_checksum              62284
_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 1.167
_oxdiff_exptl_absorpt_empirical_full_min 0.855