Very Large Magnetic Anisotropy of Cage Cobalt(II) Complexes with a Rigid Cholesteryl Substituent from Paramagnetic NMR Spectroscopy.
Pavlov, Alexander A.; Savkina, Svetlana A.; Belov, Alexander S.; Voloshin, Yan Z.; Nelyubina, Yulia V.; Novikov, Valentin V.; ACS omega 3 (2018) 4941–4946; doi:10.1021/acsomega.8b00772

data_4515963
_publ_section_title
;
 Very Large Magnetic Anisotropy of Cage Cobalt(II) Complexes with a Rigid
 Cholesteryl Substituent from Paramagnetic NMR Spectroscopy.
;
_journal_issue                   5
_journal_name_full               'ACS omega'
_journal_page_first              4941
_journal_page_last               4946
_journal_paper_doi               10.1021/acsomega.8b00772
_journal_volume                  3
_journal_year                    2018
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C42 H63 B Co N9 O3, 2(C H Cl3), Cl'
_chemical_formula_sum            'C44 H65 B Cl7 Co N9 O3'
_chemical_formula_weight         1085.94
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 99.037(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.8545(16)
_cell_length_b                   8.0296(9)
_cell_length_c                   23.616(3)
_cell_measurement_reflns_used    6664
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     2594.6(5)
_computing_cell_refinement       'APEX2 (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'APEX2 (Bruker, 2005)'
_computing_molecular_graphics    'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX2 DUO 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  0.1196
_diffrn_reflns_av_unetI/netI     0.1087
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            49885
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_min         1.840
_exptl_absorpt_coefficient_mu    0.739
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5651
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'APEX2 (Bruker, 2005)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_description       needle
_exptl_crystal_F_000             1134
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.687
_refine_diff_density_min         -0.566
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details
;
 Flack x determined using 3228 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.037(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     594
_refine_ls_number_reflns         12514
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0951
_refine_ls_R_factor_gt           0.0568
_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^)+(0.0447P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1060
_refine_ls_wR_factor_ref         0.1210
_reflns_Friedel_coverage         0.868
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                8998
_reflns_number_total             12514
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao8b00772_si_003.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4515963
_shelx_estimated_absorpt_t_min   0.782
_shelx_estimated_absorpt_t_max   0.993
_shelxl_version_number           2014/6
_shelx_res_checksum              86631
_shelx_hkl_checksum              11445