Self-assembly of fish-bone and grid-like CoII-based single-molecule magnets using dihydrazone ligands with NNN and NNO pockets
Yang, Qianqian; Wang, Guo-Lu; Zhang, Yi-Quan; Tang, Jinkui; Dalton Transactions  (2022) –; doi:10.1039/D2DT02451A

data_7710998
_publ_section_title
;
 Self-assembly of fish-bone and grid-like CoII-based single-molecule
 magnets using dihydrazone ligands with NNN and NNO pockets
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02451A
_journal_year                    2022
_chemical_formula_moiety         'C84 H76 Co4 N28 O16, 4(Cl2 O8)'
_chemical_formula_sum            'C84 H76 Cl8 Co4 N28 O48'
_chemical_formula_weight         2765.04
_chemical_name_systematic        Co4
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-01-07
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-03-25 deposited with the CCDC.	2022-08-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   36.8996(9)
_cell_length_b                   19.0503(5)
_cell_length_c                   21.1241(5)
_cell_measurement_reflns_used    9868
_cell_measurement_temperature    180.0
_cell_measurement_theta_max      23.790
_cell_measurement_theta_min      2.406
_cell_volume                     14849.2(6)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      180.0
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0879
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            290382
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        24.132
_diffrn_reflns_theta_max         24.132
_diffrn_reflns_theta_min         1.916
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.662
_exptl_absorpt_correction_T_max  0.899
_exptl_absorpt_correction_T_min  0.888
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1137 before and 0.0660 after correction.
The Ratio of minimum to maximum transmission is 0.8816.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_description       block
_exptl_crystal_F_000             5616
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.393
_refine_diff_density_min         -1.302
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.682
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     853
_refine_ls_number_reflns         12176
_refine_ls_number_restraints     256
_refine_ls_restrained_S_all      1.772
_refine_ls_R_factor_all          0.1484
_refine_ls_R_factor_gt           0.1167
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3635
_refine_ls_wR_factor_ref         0.4058
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8288
_reflns_number_total             12176
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02451a2.cif
_cod_data_source_block           3
_cod_database_code               7710998
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 O5-H5
 0.87 with sigma of 0.01
 O8-H8
 0.87 with sigma of 0.01
 O4-H4
 0.87 with sigma of 0.01
 O1-H1
 0.87 with sigma of 0.01
 Cl6-O28 = Cl6-O29 = Cl6-O27 = Cl6-O30
 1.5 with sigma of 0.02
 Cl1-O9 = Cl1-O12 = Cl1-O11 = Cl1-O10
 1.5 with sigma of 0.02
 Cl2-O14 = Cl2-O16 = Cl2-O15 = Cl2-O13
 1.5 with sigma of 0.02
 Co1-H8
 2.917338 with sigma of 0.02
 Co1-H1
 2.836674 with sigma of 0.02
 C1-H1
 1.902588 with sigma of 0.02
 Co2-H4
 2.8782 with sigma of 0.02
 C43-H8
 1.892994 with sigma of 0.02
 C21-H4
 1.93115 with sigma of 0.02
 C22-H5
 1.947549 with sigma of 0.02
 Co2-H5
 2.874524 with sigma of 0.02
 Cl6-O28 \\sim Cl6-O29 \\sim Cl6-O27 \\sim Cl6-O30
 with sigma of 0.02
 O28-O27 \\sim O29-O30 \\sim O28-O30 \\sim O29-O27 \\sim O28-O29 \\sim O27-O30
 with sigma of 0.04
 Cl1-O9 \\sim Cl1-O12 \\sim Cl1-O11 \\sim Cl1-O10
 with sigma of 0.02
 O9-O11 \\sim O12-O10 \\sim O9-O10 \\sim O12-O11 \\sim O9-O12 \\sim O11-O10
 with sigma of 0.04
 Cl2-O14 \\sim Cl2-O16 \\sim Cl2-O15 \\sim Cl2-O13
 with sigma of 0.02
 O14-O15 \\sim O16-O13 \\sim O14-O13 \\sim O16-O15 \\sim O14-O16 \\sim O15-O13
 with sigma of 0.04
3. Rigid bond restraints
 Cl6, O30
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
Cl6 \\sim O27 \\sim O28 \\sim O29 \\sim O30: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
Cl1 \\sim O9 \\sim O10 \\sim O11 \\sim O12: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
Cl2 \\sim O13 \\sim O14 \\sim O15 \\sim O16: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
Uanis(O22) \\sim Ueq, Uanis(O23) \\sim Ueq, Uanis(O21) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 Cl6, O27, O28, O29, O30
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl1, O9, O10, O11, O12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl2, O13, O14, O15, O16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: O9(0.5) O11(0.5) O12(0.5) O13(0.5) O15(0.5) O16(0.5) O28(0.5)
 O30(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C21(H21A,H21B), C22(H22A,H22B), C43(H43A,H43B)
7.b Aromatic/amide H refined with riding coordinates:
 N3(H3), N5(H5A), N10(H10), N13(H13), C3(H3A), C4(H4A), C5(H5B), C7(H7),
 C10(H10A), C11(H11), C12(H12), C15(H15), C17(H17), C18(H18), C19(H19),
 C24(H24), C25(H25), C26(H26), C28(H28), C31(H31), C32(H32), C33(H33), C34(H34),
  C37(H37), C39(H39), C40(H40), C41(H41)
;
_shelx_res_checksum              19028
_shelx_fab_checksum              18120
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'