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_7712373
_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         'C28 H27 B Br Co N6 O3, Cl O4, C1 H2 Cl2'
_chemical_formula_sum            'C29 H29 B Br Cl3 Co N6 O7'
_chemical_formula_weight         829.58
_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
_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                90
_cell_angle_beta                 98.36(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.8994(18)
_cell_length_b                   24.847(5)
_cell_length_c                   15.741(3)
_cell_measurement_reflns_used    730
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      2.2
_cell_measurement_theta_min      36.0
_cell_volume                     3443.7(12)
_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 0.972
_diffrn_measured_fraction_theta_max 0.924
_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  0.1016
_diffrn_reflns_av_unetI/netI     0.1513
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.924
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            23815
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_theta_full        35.587
_diffrn_reflns_theta_max         38.470
_diffrn_reflns_theta_min         2.106
_exptl_absorpt_coefficient_mu    2.158
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Scala (Evans, 2006)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.600
_exptl_crystal_description       prism
_exptl_crystal_F_000             1676
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane -- hexane'
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.986
_refine_diff_density_min         -1.365
_refine_diff_density_rms         0.148
_refine_ls_extinction_coef       0.0057(5)
_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   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     459
_refine_ls_number_reflns         7049
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.1625
_refine_ls_R_factor_gt           0.0909
_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^)+20.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1937
_refine_ls_wR_factor_ref         0.2322
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3871
_reflns_number_total             7049
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt04073e2.cif
_cod_data_source_block           ss120
_cod_database_code               7712373
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.938
_shelx_estimated_absorpt_t_min   0.900
_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. Restrained distances
 Cl2B-C29B \\sim Cl3B-C29B \\sim Cl3A-C29A \\sim Cl2A-C29A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C29A) = Uanis(C29B)
4. Others
 Sof(Cl3B)=Sof(Cl2B)=Sof(C29B)=Sof(H29C)=Sof(H29D)=1-FVAR(1)
 Sof(Cl3A)=Sof(Cl2A)=Sof(C29A)=Sof(H29A)=Sof(H29B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C29A(H29A,H29B), C29B(H29C,H29D)
5.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C23(H23), C11(H11), C13(H13), C3(H3), C12(H12), C24(H24), C4(H4),
 C20(H20), C18(H18), C6(H6), C17(H17), C26(H26), C27(H27), C19(H19), C5(H5)
5.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C7(H7A,H7B,H7C), C21(H21A,H21B,H21C)
;
_shelx_res_checksum              77903
_shelx_hkl_checksum              54273
_olex2_submission_special_instructions 'No special instructions were received'