Effects of solvatomorphism, the nature of a chelating ligand synthon and a counterion on the single crystal XRD structure and SMM properties of paramagnetic monocapped cobalt(II) tris-pyrazoloximates.
Belova, Svetlana A.; Belov, Alexander S.; Danshina, Anastasia A.; Zubavichus, Yan V.; Aleshin, Dmitriy Yu; Pavlov, Alexander A.; Efimov, Nikolay N.; Voloshin, Yan Z.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 1482–1491; doi:10.1039/d3dt03025c

data_7714654
_publ_section_title
;
 Effects of solvatomorphism, the nature of a chelating ligand synthon and
 a counterion on the single crystal XRD structure and SMM properties of
 paramagnetic monocapped cobalt(II) tris-pyrazoloximates.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1482
_journal_page_last               1491
_journal_paper_doi               10.1039/d3dt03025c
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C21 H23 B Co N9 O3, Cl, C6 H6'
_chemical_formula_sum            'C27 H29 B Cl Co N9 O3'
_chemical_formula_weight         632.78
_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   mixed
_audit_creation_date             2023-08-03
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-08-03 deposited with the CCDC.	2023-12-07 downloaded from the CCDC.
;
_cell_angle_alpha                92.98(3)
_cell_angle_beta                 102.15(3)
_cell_angle_gamma                96.45(3)
_cell_formula_units_Z            2
_cell_length_a                   8.1600(16)
_cell_length_b                   13.400(3)
_cell_length_c                   13.690(3)
_cell_measurement_reflns_used    4716
_cell_measurement_temperature    100
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     1449.7(6)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type
'MarExperts mardtb goniostat and Rayonix SX 165 detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7927
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21240
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        28.400
_diffrn_reflns_theta_max         29.998
_diffrn_reflns_theta_min         3.002
_exptl_absorpt_coefficient_mu    0.986
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_correction_T_min  0.734
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0893 before and 0.0759 after correction.
The Ratio of minimum to maximum transmission is 0.7094.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_description       plate
_exptl_crystal_F_000             654
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.278
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         6059
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0326
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0473P)^2^+0.5046P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0865
_refine_ls_wR_factor_ref         0.0894
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5463
_reflns_number_total             6059
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03025c2.cif
_cod_data_source_block           ab401
_cod_depositor_comments
'Adding full bibliography for 7714650--7714658.cif.'
_cod_original_cell_volume        1449.7(5)
_cod_database_code               7714654
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.850
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C3S-C2S \\sim C1S'-C2S'
 with sigma of 0.02
 C1S'-C6S' \\sim C2S-C1S
 with sigma of 0.02
 C1S'-C6S' \\sim C6S-C1S
 with sigma of 0.02
 C5S'-C6S' \\sim C5S-C6S
 with sigma of 0.02
 C5S'-C4S' \\sim C4S-C5S
 with sigma of 0.02
 C4S'-C3S' \\sim C3S-C4S
 with sigma of 0.02
 C2S'-C3S' \\sim C3S-C2S
 with sigma of 0.02
 C1S'-C2S' \\sim C2S-C1S
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C4S) \\sim Ueq, Uanis(C4S') \\sim Ueq, Uanis(C3S') \\sim Ueq, Uanis(C3S)
\\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(C3S) \\sim Ueq, Uanis(C3S') \\sim Ueq, Uanis(C4S) \\sim Ueq, Uanis(C4S')
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1S') = Uanis(C1S)
Uanis(C6S') = Uanis(C6S)
Uanis(C5S') = Uanis(C5S)
Uanis(C4S) = Uanis(C4S')
Uanis(C3S') = Uanis(C3S)
Uanis(C2S') = Uanis(C2S)
4. Others
 Sof(C1S')=Sof(H1S')=Sof(C2S')=Sof(H2S')=Sof(C3S')=Sof(H3S')=Sof(C4S')=
 Sof(H4S')=Sof(C5S')=Sof(H5S')=Sof(C6S')=Sof(H6S')=1-FVAR(1)
 Sof(C1S)=Sof(H1S)=Sof(C2S)=Sof(H2S)=Sof(C3S)=Sof(H3S)=Sof(C4S)=Sof(H4S)=
 Sof(C5S)=Sof(H5S)=Sof(C6S)=Sof(H6S)=FVAR(1)
5.a Riding coordinates:
 N3(H3), N6(H6), N9(H9)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3A), C4(H4), C8(H8), C9(H9A), C13(H13), C14(H14), C17(H17), C18(H18),
 C19(H19), C20(H20), C21(H21), C1S(H1S), C2S(H2S), C3S(H3S), C4S(H4S), C5S(H5S),
  C6S(H6S), C1S'(H1S'), C2S'(H2S'), C3S'(H3S'), C4S'(H4S'), C5S'(H5S'),
 C6S'(H6S')
5.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C10(H10A,H10B,H10C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              96701
_shelx_hkl_checksum              75370
_olex2_submission_special_instructions 'No special instructions were received'