Synthesis, X-ray structure and magnetic properties of the apically functionalized monocapped cobalt(II) tris-pyridineoximates possessing SMM behaviour.
Belov, Alexander S.; Belova, Svetlana A.; Efimov, Nikolay N.; Zlobina, Veronika V.; Novikov, Valentin V.; Nelyubina, Yulya V.; Zubavichus, Yan V.; Voloshin, Yan Z.; Pavlov, Alexander A.; Dalton transactions (Cambridge, England : 2003)  (2023) –; doi:10.1039/d2dt04073e

data_7712372
_publ_section_title
;
 Synthesis, X-ray structure and magnetic properties of the apically
 functionalized monocapped cobalt(II) tris-pyridineoximates possessing SMM
 behaviour.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d2dt04073e
_journal_year                    2023
_chemical_formula_moiety         'C29 H30 B Co N6 O5 S2, Cl O4'
_chemical_formula_sum            'C29 H30 B Cl Co N6 O9 S2'
_chemical_formula_weight         775.90
_chemical_properties_physical
'Either radiation damage under the beam or desolvation'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-11-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-12-16 deposited with the CCDC.	2023-02-07 downloaded from the CCDC.
;
_cell_angle_alpha                104.71(3)
_cell_angle_beta                 112.39(3)
_cell_angle_gamma                95.43(3)
_cell_formula_units_Z            2
_cell_length_a                   10.939(2)
_cell_length_b                   13.525(3)
_cell_length_c                   14.224(3)
_cell_measurement_reflns_used    660
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      3.6
_cell_measurement_theta_min      32.0
_cell_volume                     1838.4(9)
_computing_cell_refinement       'iMosflm (Battye et al., 2011)'
_computing_data_collection       'Marccd (Doyle, 2011)'
_computing_data_reduction        iMosflm
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.941
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_device_type  'Rayonix SX165 CCD'
_diffrn_measurement_method       '/f scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.9699
_diffrn_reflns_av_R_equivalents  0.1228
_diffrn_reflns_av_unetI/netI     0.2146
_diffrn_reflns_Laue_measured_fraction_full 0.941
_diffrn_reflns_Laue_measured_fraction_max 0.941
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10450
_diffrn_reflns_point_group_measured_fraction_full 0.941
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        32.495
_diffrn_reflns_theta_max         32.495
_diffrn_reflns_theta_min         3.571
_exptl_absorpt_coefficient_mu    1.718
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Scala (Evans, 2006)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_description       prism
_exptl_crystal_F_000             798
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane -- hexane'
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.348
_refine_diff_density_min         -0.976
_refine_diff_density_rms         0.116
_refine_ls_extinction_coef       0.0057(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         4910
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1147
_refine_ls_R_factor_gt           0.0975
_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^)+1.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2322
_refine_ls_wR_factor_ref         0.2492
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3526
_reflns_number_total             4910
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt04073e2.cif
_cod_data_source_block           ss1052
_cod_original_cell_volume        1838.4(8)
_cod_database_code               7712372
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.966
_shelx_estimated_absorpt_t_min   0.950
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C12(H12), C13(H13),
 C17(H17), C18(H18), C19(H19), C20(H20), C23(H23), C24(H24), C26(H26), C27(H27)
2.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C14(H14A,H14B,H14C), C21(H21A,H21B,H21C), C29(H29A,H29B,H29C)
;
_shelx_res_checksum              54412
_shelx_hkl_checksum              29011
_shelx_fab_checksum              45244
_olex2_submission_special_instructions 'No special instructions were received'