Slow magnetic relaxation in high-coordinate Co(II) and Fe(II) compounds bearing neutral tetradentate ligands.
Peng, Min; Wu, Xiao-Fan; Wang, Li-Xin; Chen, Si-Huai; Xiang, Jing; Jin, Xin-Xin; Yiu, Shek-Man; Wang, Bing-Wu; Gao, Song; Lau, Tai-Chu; Dalton transactions (Cambridge, England : 2003)  (2021) –; doi:10.1039/d1dt02575a

data_7708561
_publ_section_title
;
 Slow magnetic relaxation in high-coordinate Co(II) and Fe(II) compounds
 bearing neutral tetradentate ligands.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d1dt02575a
_journal_year                    2021
_chemical_formula_moiety         'C44 H52 N8 Ni O4, 2(Cl O4)'
_chemical_formula_sum            'C44 H52 Cl2 N8 Ni O12'
_chemical_formula_weight         1014.54
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-09-14
_audit_creation_method
;
Olex2 1.5
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6380)
;
_audit_update_record
;
2021-09-14 deposited with the CCDC.	2021-09-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.070(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.9339(9)
_cell_length_b                   13.2633(6)
_cell_length_c                   16.2274(5)
_cell_measurement_reflns_used    4545
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      73.3590
_cell_measurement_theta_min      4.7020
_cell_volume                     4488.0(3)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device_type  'multiwire proportional'
_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  0.0246
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8259
_diffrn_reflns_point_group_measured_fraction_full 0.571
_diffrn_reflns_point_group_measured_fraction_max 0.549
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         73.646
_diffrn_reflns_theta_min         3.950
_exptl_absorpt_coefficient_mu    2.341
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65662
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_description       needle
_exptl_crystal_F_000             2120
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.438
_refine_diff_density_min         -0.704
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.66(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     695
_refine_ls_number_reflns         4985
_refine_ls_number_restraints     242
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0461
_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^)+(0.0754P)^2^+7.4626P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1216
_refine_ls_wR_factor_ref         0.1240
_reflns_Friedel_coverage         0.157
_reflns_Friedel_fraction_full    0.163
_reflns_Friedel_fraction_max     0.149
_reflns_number_gt                4817
_reflns_number_total             4985
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02575a2.cif
_cod_data_source_block           04
_cod_database_code               7708561
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.783
_shelx_estimated_absorpt_t_min   0.766
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.34(3)
 0.66(3)
2. 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 C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
C43 \\sim C44 \\sim C45 \\sim C46 \\sim C43' \\sim C44' \\sim C45' \\sim C46':
within 3.8A with sigma of 0.02 and sigma for terminal atoms of 0.04 within 3.8A
O5 \\sim O6' \\sim O7' \\sim O8': within 3.8A with sigma of 0.02 and sigma for
terminal atoms of 0.04 within 3.8A
O9 \\sim O10' \\sim O11' \\sim O12': within 3.8A with sigma of 0.02 and sigma
for terminal atoms of 0.04 within 3.8A
Uanis(O7') \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(O5') \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Sof(C43')=Sof(H43C)=Sof(H43D)=Sof(C44')=Sof(H44C)=Sof(H44D)=Sof(C45')=
 Sof(H45C)=Sof(H45D)=Sof(C46')=Sof(H46D)=Sof(H46E)=Sof(H46F)=1-FVAR(1)
 Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(C45)=Sof(H45A)=
 Sof(H45B)=Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(H46C)=FVAR(1)
 Sof(O11')=Sof(O10')=Sof(O12')=1-FVAR(2)
 Sof(O10)=Sof(O11)=Sof(O12)=FVAR(2)
 Sof(O5')=Sof(O8')=Sof(O7')=Sof(O6')=1-FVAR(3)
 Sof(O5)=Sof(O6)=Sof(O7)=Sof(O8)=FVAR(3)
 U11(C13)=U11(C14)=U11(C15)=U11(C16)=U11(C17)=U11(C18)=U11(C19)=U11(C20)=
 U11(C24)=FVAR(4)
 U11(C1)=U11(C2)=U11(C3)=U11(C4)=U11(C7)=U11(C8)=U11(C9)=U11(C10)=U11(C11)=
 U11(C12)=FVAR(5)
5.a Riding coordinates:
 N8(H8), C43(H43A,H43B), C43'(H43C,H43D)
5.b Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C33(H33A,H33B), C34(H34A,
 H34B), C35(H35A,H35B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B),
 C44(H44A,H44B), C45(H45A,H45B), C44'(H44C,H44D), C45'(H45C,H45D)
5.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N4(H4), N5(H5), C2(H2), C3(H3), C5(H5A), C6(H6), C8(H8A), C9(H9),
 C14(H14), C15(H15), C17(H17), C18(H18), C20(H20), C21(H21)
5.d Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C36(H36A,H36B,H36C), C41(H41A,H41B,H41C), C46(H46A,H46B,
 H46C), C46'(H46D,H46E,H46F)
;
_shelx_res_checksum              9745
_olex2_submission_special_instructions 'No special instructions were received'