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_7714656
_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         'I, C21 H23 B Co N9 O3'
_chemical_formula_sum            'C21 H23 B Co I N9 O3'
_chemical_formula_weight         646.12
_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   mixed
_audit_creation_date             2023-07-30
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-08-02 deposited with the CCDC.	2023-12-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.775(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.7090(17)
_cell_length_b                   28.144(6)
_cell_length_c                   10.552(2)
_cell_measurement_reflns_used    1270
_cell_measurement_temperature    120.15
_cell_measurement_theta_max      23.76
_cell_measurement_theta_min      2.37
_cell_volume                     2548.8(9)
_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)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      120.15
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII DUO CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1521
_diffrn_reflns_av_unetI/netI     0.1110
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            22802
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.088
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.927
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5293
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.684
_exptl_crystal_description       plate
_exptl_crystal_F_000             1284
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.107
_refine_diff_density_min         -1.945
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         4497
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.1336
_refine_ls_R_factor_gt           0.0749
_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^)+(0.1095P)^2^+13.2313P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1862
_refine_ls_wR_factor_ref         0.2241
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2709
_reflns_number_total             4497
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03025c2.cif
_cod_data_source_block           ss370
_cod_depositor_comments
'Adding full bibliography for 7714650--7714658.cif.'
_cod_database_code               7714656
_shelxl_version_number           2014/6
_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
 C16-B1 \\sim C16'-B1
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C16') \\sim Ueq, Uanis(C16) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C16') \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C18')
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C19) \\sim Ueq, Uanis(C19') \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C21') = Uanis(C21)
Uanis(C18) = Uanis(C18')
Uanis(C17') = Uanis(C17)
Uanis(C20') = Uanis(C20)
Uanis(C19') = Uanis(C19)
Uanis(C16') = Uanis(C16)
4. Others
 Sof(C16')=Sof(C17')=Sof(H17')=Sof(C18')=Sof(H18')=Sof(C19')=Sof(H19')=
 Sof(C20')=Sof(H20')=Sof(C21')=Sof(H21')=1-FVAR(1)
 Sof(C16)=Sof(C17)=Sof(H17)=Sof(C18)=Sof(H18)=Sof(C19)=Sof(H19)=Sof(C20)=
 Sof(H20)=Sof(C21)=Sof(H21)=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), C17'(H17'), C18'(H18'), C19'(H19'), C20'(H20'),
 C21'(H21')
5.c Fitted hexagon refined as free rotating group:
 C16(C17,C18,C19,C20,C21), C16'(C17',C18',C19',C20',C21')
5.d Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C10(H10A,H10B,H10C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              57030
_shelx_hkl_checksum              46397
_olex2_submission_special_instructions 'No special instructions were received'