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_7710996
_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         'C42 H38 Co2 N14 O8, 4(Cl O4)'
_chemical_formula_sum            'C42 H38 Cl4 Co2 N14 O24'
_chemical_formula_weight         1382.52
_chemical_name_systematic        Co2
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2021-10-21
_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                 92.001(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.4910(14)
_cell_length_b                   9.5103(12)
_cell_length_c                   25.965(4)
_cell_measurement_reflns_used    2251
_cell_measurement_temperature    300.0
_cell_measurement_theta_max      24.47
_cell_measurement_theta_min      2.45
_cell_volume                     2589.0(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      300.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1421
_diffrn_reflns_av_unetI/netI     0.0734
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            32854
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.051
_diffrn_reflns_theta_max         25.051
_diffrn_reflns_theta_min         1.942
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.950
_exptl_absorpt_correction_T_max  0.867
_exptl_absorpt_correction_T_min  0.843
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1135 before and 0.0756 after correction.
The Ratio of minimum to maximum transmission is 0.8455.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.773
_exptl_crystal_description       plate
_exptl_crystal_F_000             1404
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.148
_refine_diff_density_min         -0.999
_refine_diff_density_rms         0.119
_refine_ls_extinction_coef       0.0070(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         4575
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.1701
_refine_ls_R_factor_gt           0.0895
_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^)+(0.1636P)^2^+9.8948P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2318
_refine_ls_wR_factor_ref         0.3228
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2367
_reflns_number_total             4575
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02451a2.cif
_cod_data_source_block           2
_cod_database_code               7710996
_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
 O1-H1
 0.85 with sigma of 0.01
 Cl2-O12 = Cl2-O9 = Cl2-O11 = Cl2-O10
 1.44 with sigma of 0.01
 O12-O9 = O12-O11 = O12-O10 = O9-O11 = O9-O10 = O11-O10
 2.35 with sigma of 0.02
 Co1-H1
 2.823552 with sigma of 0.02
 C1-H1
 1.889089 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl2 \\sim O9 \\sim O10 \\sim O11 \\sim O12: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
Uanis(O7) \\sim Ueq, Uanis(O6) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4.a Riding coordinates:
 O4(H4)
4.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C21(H21A,H21B)
4.c Aromatic/amide H refined with riding coordinates:
 N3(H3), N5(H5), C3(H3A), C4(H4A), C5(H5A), C7(H7), C10(H10), C11(H11),
 C12(H12), C15(H15), C17(H17), C18(H18), C19(H19)
;
_shelx_res_checksum              19324
_olex2_submission_special_instructions 'No special instructions were received'