Modulating axial anisotropy in tetrahedral Co(II) phosphonate single-ion magnets through N-donor ligands.
Patwal, Ananta; Rana, Rajanikanta; Rajaraman, Gopalan; Murugavel, Ramaswamy; Dalton transactions (Cambridge, England : 2003) 54 (2025) 15259–15270; doi:10.1039/d5dt01461a

data_1575633
_publ_section_title
;
 Modulating axial anisotropy in tetrahedral Co(II) phosphonate single-ion
 magnets through N-donor ligands.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15259
_journal_page_last               15270
_journal_paper_doi               10.1039/d5dt01461a
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C44 H60 Co N4 O8 P2'
_chemical_formula_sum            'C44 H60 Co N4 O8 P2'
_chemical_formula_weight         893.83
_chemical_name_systematic        RM_ANN_158
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2025-04-02
_audit_creation_method
;
Olex2 1.5
(compiled 2025.03.04 svn.red2d20d0 for OlexSys, GUI svn.r7188)
;
_audit_update_record
;
2025-05-03 deposited with the CCDC.	2025-09-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.138(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.665(5)
_cell_length_b                   10.1074(15)
_cell_length_c                   22.703(5)
_cell_measurement_reflns_used    9020
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.151
_cell_measurement_theta_min      2.744
_cell_volume                     4705.2(17)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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    'XS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1084
_diffrn_reflns_av_unetI/netI     0.0522
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            75470
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         2.208
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.486
_exptl_absorpt_correction_T_max  0.5939
_exptl_absorpt_correction_T_min  0.4706
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1658 before and 0.1245 after correction.
The Ratio of minimum to maximum transmission is 0.7924.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_description       block
_exptl_crystal_F_000             1892
_exptl_crystal_size_max          0.758
_exptl_crystal_size_mid          0.306
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.352
_refine_diff_density_min         -0.825
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     548
_refine_ls_number_reflns         8243
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0803
_refine_ls_R_factor_gt           0.0681
_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^)+(0.0852P)^2^+14.3312P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1732
_refine_ls_wR_factor_ref         0.1829
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6871
_reflns_number_total             8243
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01461a2.cif
_cod_data_source_block           rm_ann_158_0m
_cod_depositor_comments
'Adding full bibliography for 1575632--1575634.cif.'
_cod_original_cell_volume        4705.3(17)
_cod_database_code               1575633
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.897
_shelx_estimated_absorpt_t_min   0.710
_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, All O(H) groups
2. Restrained distances
 O4-H4
 0.85 with sigma of 0.01
 C13-H4
 1.913567 with sigma of 0.02
 Co1-H4
 3.010179 with sigma of 0.02
3. Rigid bond restraints
 C2, C3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C7, C9
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C10, C12
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
Uanis(C3) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(C4) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(C5) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(C9) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(C12) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
5.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C32(H32), C35(H35)
5.b Aromatic/amide H refined with riding coordinates:
 N2(H2), N4(H4A), C3(H3), C4(H4B), C5(H5), C17(H17), C18(H18), C19(H19),
 C20(H20), C22(H22), C28(H28), C29(H29), C30(H30), C39(H39), C40(H40), C41(H41),
  C42(H42), C44(H44)
5.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C37(H37A,
 H37B,H37C)
5.d Idealised tetrahedral OH refined as rotating group:
 O8(H8)
;
_shelx_res_checksum              34400
_shelx_hkl_checksum              19504
_olex2_submission_special_instructions 'No special instructions were received'