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_7710997
_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         'C50 H38 Co2 N22 O4, 4(Cl O4), 4(C H4 O)'
_chemical_formula_sum            'C54 H54 Cl4 Co2 N22 O24'
_chemical_formula_weight         1654.85
_chemical_name_systematic        Co2
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2022-01-24
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-03-29 deposited with the CCDC.	2022-08-16 downloaded from the CCDC.
;
_cell_angle_alpha                89.526(2)
_cell_angle_beta                 75.536(2)
_cell_angle_gamma                72.6610(10)
_cell_formula_units_Z            1
_cell_length_a                   10.4794(3)
_cell_length_b                   11.2095(3)
_cell_length_c                   15.2781(4)
_cell_measurement_reflns_used    6285
_cell_measurement_temperature    173.0
_cell_measurement_theta_max      58.835
_cell_measurement_theta_min      2.995
_cell_volume                     1654.59(8)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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      173.0
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_av_unetI/netI     0.0518
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10996
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        58.918
_diffrn_reflns_theta_max         58.918
_diffrn_reflns_theta_min         2.995
_diffrn_source_current           1.1
_diffrn_source_power             0.055
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    6.271
_exptl_absorpt_correction_T_max  0.330
_exptl_absorpt_correction_T_min  0.325
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_description       block
_exptl_crystal_F_000             846
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.807
_refine_diff_density_min         -0.976
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         4674
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.1050
_refine_ls_R_factor_gt           0.0933
_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^)+(0.1831P)^2^+7.6377P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2643
_refine_ls_wR_factor_ref         0.2776
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3944
_reflns_number_total             4674
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02451a2.cif
_cod_data_source_block           1
_cod_database_code               7710997
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.398
_shelx_estimated_absorpt_t_min   0.367
_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
 O9-O10 = O9-O11 = O9-O12 = O10-O11 = O10-O12 = O11-O12
 2.35 with sigma of 0.02
 O8-C27
 1.42 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O10) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O7) \\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(O11) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(O8) \\sim Ueq, Uanis(C27) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4.a Riding coordinates:
 O8(H8)
4.b Aromatic/amide H refined with riding coordinates:
 N5(H5), N7(H7), C1(H1), C2(H2), C3(H3), C5(H5A), C6(H6), C7(H7A), C9(H9),
 C12(H12), C13(H13), C14(H14), C17(H17), C19(H19), C20(H20), C21(H21), C23(H23),
  C24(H24), C25(H25)
4.c Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C)
4.d Idealised tetrahedral OH refined as rotating group:
 O1(H1A)
;
_shelx_res_checksum              13045
_olex2_submission_special_instructions 'No special instructions were received'