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_7714651
_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, C3 H6 O'
_chemical_formula_sum            'C24 H29 B Cl Co N9 O4'
_chemical_formula_weight         612.75
_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             2023-07-26
_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                78.627(6)
_cell_angle_beta                 77.176(6)
_cell_angle_gamma                80.835(6)
_cell_formula_units_Z            2
_cell_length_a                   8.096(2)
_cell_length_b                   10.116(3)
_cell_length_c                   18.105(5)
_cell_measurement_reflns_used    2277
_cell_measurement_temperature    120.15
_cell_measurement_theta_max      29.86
_cell_measurement_theta_min      2.54
_cell_volume                     1407.0(7)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0716
_diffrn_reflns_av_unetI/netI     0.1114
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            15903
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.998
_diffrn_reflns_theta_min         2.069
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.753
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5965
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0816 before and 0.0596 after correction.
The Ratio of minimum to maximum transmission is 0.7995.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_description       plate
_exptl_crystal_F_000             634
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.217
_refine_diff_density_min         -1.203
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         7435
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.1173
_refine_ls_R_factor_gt           0.0775
_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^)+(0.0999P)^2^+2.9917P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2092
_refine_ls_wR_factor_ref         0.2351
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4758
_reflns_number_total             7435
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03025c2.cif
_cod_data_source_block           AB384
_cod_depositor_comments
'Adding full bibliography for 7714650--7714658.cif.'
_cod_original_cell_volume        1406.9(6)
_cod_database_code               7714651
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.895
_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.a Riding coordinates:
 N3(H3), N6(H6), N9(H9)
2.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)
2.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C10(H10A,H10B,H10C), C15(H15A,H15B,H15C), C2S(H2SA,H2SB,
 H2SC), C3S(H3SA,H3SB,H3SC)
;
_shelx_res_checksum              84556
_shelx_hkl_checksum              4676
_olex2_submission_special_instructions 'No special instructions were received'