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_4349775
_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_compound_source        no
_chemical_formula_moiety         'C30 H38 Co N6 O4, 2(Cl O4)'
_chemical_formula_sum            'C30 H38 Cl2 Co N6 O12'
_chemical_formula_weight         804.49
_chemical_name_common            Co(L2)2(ClO4)2
_chemical_name_systematic        2
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-04-15
_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            8
_cell_length_a                   13.8991(4)
_cell_length_b                   19.9517(6)
_cell_length_c                   25.3128(8)
_cell_measurement_reflns_used    8397
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      28.0200
_cell_measurement_theta_min      3.3150
_cell_volume                     7019.5(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      180.00(10)
_diffrn_detector_area_resol_mean 10.3914
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega  -17.00   19.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.5566  -99.0000   30.0000 36

  2 omega    1.00   27.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.5566  -99.0000 -150.0000 26

  3 omega -103.00   57.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.5566    0.0000  -90.0000 160
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0012883000
_diffrn_orient_matrix_UB_12      0.0332584000
_diffrn_orient_matrix_UB_13      0.0098599000
_diffrn_orient_matrix_UB_21      0.0275101000
_diffrn_orient_matrix_UB_22      -0.0100855000
_diffrn_orient_matrix_UB_23      0.0222308000
_diffrn_orient_matrix_UB_31      0.0429677000
_diffrn_orient_matrix_UB_32      0.0074565000
_diffrn_orient_matrix_UB_33      -0.0139252000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            33613
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         2.931
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.711
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90957
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             3336
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.26
_refine_diff_density_max         1.596
_refine_diff_density_min         -0.761
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         6896
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.0868
_refine_ls_R_factor_gt           0.0672
_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^)+(0.0820P)^2^+19.4220P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1695
_refine_ls_wR_factor_ref         0.1865
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5322
_reflns_number_total             6896
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7qi00547d2.cif
_cod_data_source_block           2
_cod_database_code               4349775
_chemical_oxdiff_formula         'C25 H27 N3 Co1 cl3 o4'
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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
2. Restrained distances
 Cl2-O9 \\sim Cl2-O10A \\sim Cl2-O11A \\sim Cl2-O12A
 with sigma of 0.01
 Cl2-O9 \\sim Cl2-O11A \\sim Cl2-O11B \\sim Cl2-O11B
 with sigma of 0.01
 O9-O10A \\sim O10A-O11A \\sim O11A-O12A \\sim O12A-O9
 with sigma of 0.02
 O9-O10B \\sim O10B-O11B \\sim O11B-O12B \\sim O12B-O9
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O10A) \\sim Ueq, Uanis(O11A) \\sim Ueq, Uanis(O12A) \\sim Ueq,
Uanis(O10B) \\sim Ueq, Uanis(O11B) \\sim Ueq, Uanis(O12B) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(O10B)=Sof(O11B)=Sof(O12B)=1-FVAR(1)
 Sof(O10A)=Sof(O11A)=Sof(O12A)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C12(H12A,H12B), C19(H19A,H19B), C27(H27A,H27B)
5.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C22(H22), C23(H23), C24(H24)
5.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C)
;
_shelx_res_checksum              18075
_shelx_hkl_checksum              96314
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_solvent_exptl_crystal_recrystallization_method methanol