Probing the influence of molecular symmetry on the magnetic anisotropy of octahedral cobalt(ii) complexes
Ding, Zhong-Yu; Meng, Yin-Shan; Xiao, Yi; Zhang, Yi-Quan; Zhu, Yuan-Yuan; Gao, Song; Inorganic Chemistry Frontiers 4 (2017) 1909–; doi:10.1039/C7QI00547D

data_4349779
_publ_section_title
;
 Probing the influence of molecular symmetry on the magnetic anisotropy of
 octahedral cobalt(ii) complexes
;
_journal_issue                   11
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              1909
_journal_paper_doi               10.1039/C7QI00547D
_journal_volume                  4
_journal_year                    2017
_chemical_absolute_configuration meso
_chemical_compound_source        no
_chemical_formula_moiety         'C40 H44 Co N8 O4, 2(Cl O4), 2(H2 O)'
_chemical_formula_sum            'C40 H48 Cl2 Co N8 O14'
_chemical_formula_weight         994.69
_chemical_name_common            Co(L4)2(ClO4)2
_chemical_name_systematic        5
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-04-19
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-05-02 deposited with the CCDC.
2017-09-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   25.736(3)
_cell_length_b                   75.453(7)
_cell_length_c                   9.3523(9)
_cell_measurement_reflns_used    5651
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      19.907
_cell_measurement_theta_min      2.333
_cell_volume                     18161(3)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_av_unetI/netI     0.0619
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       93
_diffrn_reflns_limit_k_min       -92
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            34526
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         1.672
_exptl_absorpt_coefficient_mu    0.570
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6712
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0864 before and 0.0510 after correction.
The Ratio of minimum to maximum transmission is 0.9003.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_description       block
_exptl_crystal_F_000             8272
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.671
_refine_diff_density_min         -0.548
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     594
_refine_ls_number_reflns         8535
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0629
_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^)+(0.1219P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1672
_refine_ls_wR_factor_ref         0.1851
_reflns_Friedel_coverage         0.881
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                6299
_reflns_number_total             8535
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7qi00547d2.cif
_cod_data_source_block           5_CCDC1
_cod_database_code               4349779
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 Cl1-O5 \\sim Cl1-O6 \\sim Cl1-O7 \\sim Cl1-O8
 with sigma of 0.01
 Cl2-O9 \\sim Cl2-O10 \\sim Cl2-O11 \\sim Cl2-O12
 with sigma of 0.01
 O9-O10 \\sim O10-O11 \\sim O11-O12 \\sim O12-O9
 with sigma of 0.02
 O5-O6 \\sim O6-O7 \\sim O7-O8 \\sim O8-O5
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O9) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(O12)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O5) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O8) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Riding coordinates:
 O13(H13A,H13B), O14(H14A,H14B)
4.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C17(H17A,H17B), C24(H24A,H24B), C37(H37A,H37B)
4.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C27(H27), C30(H30),
 C31(H31), C32(H32), C33(H33), C34(H34)
4.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C),
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C39(H39A,H39B,H39C), C40(H40A,H40B,
 H40C)
;
_shelx_res_checksum              84517
_shelx_hkl_checksum              41360
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_solvent_exptl_crystal_recrystallization_method acetonitrile/ether