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_7714653
_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         'Br, C21 H23 B Co N9 O3, C4 H8 O'
_chemical_formula_sum            'C25 H31 B Br Co N9 O4'
_chemical_formula_weight         671.24
_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             2023-07-30
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-08-07 deposited with the CCDC.	2023-12-07 downloaded from the CCDC.
;
_cell_angle_alpha                89.31(3)
_cell_angle_beta                 75.61(3)
_cell_angle_gamma                78.60(3)
_cell_formula_units_Z            2
_cell_length_a                   8.1745(16)
_cell_length_b                   13.088(3)
_cell_length_c                   14.139(3)
_cell_measurement_reflns_used    2561
_cell_measurement_temperature    120.15
_cell_measurement_theta_max      28.8
_cell_measurement_theta_min      2.32
_cell_volume                     1435.2(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      120.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II 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  0.1239
_diffrn_reflns_av_unetI/netI     0.1468
_diffrn_reflns_Laue_measured_fraction_full 0.999
_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       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20076
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_min         1.488
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.039
_exptl_absorpt_correction_T_max  0.4330
_exptl_absorpt_correction_T_min  0.3655
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0943 before and 0.0568 after correction.
The Ratio of minimum to maximum transmission is 0.8441.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_description       prism
_exptl_crystal_F_000             686
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.896
_refine_diff_density_min         -0.757
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.948
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         6260
_refine_ls_number_restraints     41
_refine_ls_restrained_S_all      0.949
_refine_ls_R_factor_all          0.1299
_refine_ls_R_factor_gt           0.0555
_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^)+(0.0458P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1028
_refine_ls_wR_factor_ref         0.1247
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3436
_reflns_number_total             6260
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03025c2.cif
_cod_data_source_block           sv127_co
_cod_depositor_comments
'Adding full bibliography for 7714650--7714658.cif.'
_cod_original_cell_volume        1435.2(5)
_cod_database_code               7714653
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.870
_shelx_estimated_absorpt_t_min   0.750
_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
 O1S-C1S \\sim O1S'-C1S'
 with sigma of 0.02
 O1S'-C4S' \\sim O1S-C4S
 with sigma of 0.02
 C1S'-C2S' \\sim C2S-C1S
 with sigma of 0.02
 C2S-C3S \\sim C2S'-C3S'
 with sigma of 0.02
 C4S'-C3S' \\sim C4S-C3S
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C2S') \\sim Ueq, Uanis(C2S) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C1S') \\sim Ueq, Uanis(C1S) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O1S') \\sim Ueq, Uanis(O1S) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O1S) = Uanis(O1S')
Uanis(C1S') = Uanis(C1S)
Uanis(C2S') = Uanis(C2S)
Uanis(C3S') = Uanis(C3S)
Uanis(C4S') = Uanis(C4S)
4. Others
 Sof(O1S')=Sof(C1S')=Sof(H1SC)=Sof(H1SD)=Sof(C2S')=Sof(H2SC)=Sof(H2SD)=
 Sof(C3S')=Sof(H3SC)=Sof(H3SD)=Sof(C4S')=Sof(H4SC)=Sof(H4SD)=1-FVAR(1)
 Sof(O1S)=Sof(C1S)=Sof(H1SA)=Sof(H1SB)=Sof(C2S)=Sof(H2SA)=Sof(H2SB)=Sof(C3S)=
 Sof(H3SA)=Sof(H3SB)=Sof(C4S)=Sof(H4SA)=Sof(H4SB)=FVAR(1)
5.a Everything fixed:
 H3, H6, H9
5.b Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB), C2S(H2SA,H2SB), C3S(H3SA,H3SB), C4S(H4SA,H4SB), C1S'(H1SC,
 H1SD), C2S'(H2SC,H2SD), C3S'(H3SC,H3SD), C4S'(H4SC,H4SD)
5.c 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)
5.d Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C10(H10A,H10B,H10C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              11023
_shelx_hkl_checksum              40634
_olex2_submission_special_instructions 'No special instructions were received'