Mononuclear Single-Molecule Magnets: Tailoring the Magnetic Anisotropy of First-Row Transition-Metal Complexes
Silvia Gomez-Coca; Eduard Cremades; Núria Aliaga-Alcalde; Eliseo Ruiz; Journal of the American Chemical Society 135 (2013) 7010–7018; doi:10.1021/ja4015138

data_4119724
_publ_contact_author_name
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;
_publ_section_title
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 Mononuclear Single-Molecule Magnets: Tailoring the Magnetic Anisotropy of
 First-Row Transition-Metal Complexes
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_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7010
_journal_page_last               7018
_journal_paper_doi               10.1021/ja4015138
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C39 H73 Co2 K2 N9 O7'
_chemical_formula_sum            'C39 H73 Co2 K2 N9 O7'
_chemical_formula_weight         976.12
_chemical_name_systematic
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 ?
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_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-01-22
_audit_creation_method
;
  Olex2 1.2
  (compiled 2012.12.05 svn.r2549, GUI svn.r4385)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 102.82(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.951(10)
_cell_length_b                   9.858(4)
_cell_length_c                   28.893(8)
_cell_measurement_reflns_used    252
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      31
_cell_measurement_theta_min      3
_cell_volume                     5263(4)
_computing_cell_refinement       'AUTOMAR (Claudio Klein, 2007)'
_computing_data_collection       'MARXDS (Claudio Klein, 2005)'
_computing_data_reduction        'MARSCALE (Claudio Klein, 2007)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
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O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
olex2.refine (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_computing_structure_solution
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.754
_diffrn_measured_fraction_theta_max 0.575
_diffrn_measurement_device_type  'MAR345 with image plate detector'
_diffrn_measurement_method       'phi scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_unetI/netI     0.0562
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            11564
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.71
_diffrn_reflns_theta_min         1.45
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.837
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_description       prism
_exptl_crystal_F_000             2072
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.356
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         4709
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0554
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0888P)^2^+3.1525P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1653
_refine_ls_wR_factor_ref         0.1763
_reflns_number_gt                3552
_reflns_number_total             4709
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4015138_si_002.cif
_cod_data_source_block           nuom141a
_cod_database_code               4119724
_olex2_refinement_description
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1. others
 Fixed Sof: C19(0.5) C20(0.5) C21(0.5)
 Fixed U12: N5(0) O4(0)
 Fixed U23: N5(0) O4(0)
 Fixed Uiso: H1A(0.081) H1B(0.081) H4A(0.097) H4B(0.097) H4C(0.097) H5A(0.122)
 H5B(0.122) H5C(0.122) H6A(0.115) H6B(0.115) H6C(0.115) H7A(0.08) H7B(0.08)
 H10A(0.141) H10B(0.141) H10C(0.141) H11A(0.149) H11B(0.149) H11C(0.149)
 H12A(0.14) H12B(0.14) H12C(0.14) H13A(0.076) H13B(0.076) H16A(0.119)
 H16B(0.119) H16C(0.119) H17A(0.127) H17B(0.127) H17C(0.127) H18A(0.138)
 H18B(0.138) H18C(0.138)
 Fixed X: H1A(0.2313) H1B(0.1745) H4A(0.1327) H4B(0.0497) H4C(0.0903) H5A(0)
 H5B(-0.0393) H5C(-0.0121) H6A(0.1161) H6B(0.0602) H6C(0.0329) H7A(0.1204)
 H7B(0.1854) H10A(0.1979) H10B(0.2194) H10C(0.2709) H11A(0.2687) H11B(0.2174)
 H11C(0.1949) H12A(0.0791) H12B(0.0778) H12C(0.1005) H13A(0.3023) H13B(0.3073)
 H16A(0.4427) H16B(0.431) H16C(0.3815) H17A(0.2644) H17B(0.2725) H17C(0.3223)
 H18A(0.3603) H18B(0.4184) H18C(0.4293) N5(0.5) O4(0.5)
 Fixed Y: H1A(0.7628) H1B(0.711) H4A(0.6216) H4B(0.6034) H4C(0.5029)
 H5A(0.5587) H5B(0.66) H5C(0.7097) H6A(0.8561) H6B(0.8954) H6C(0.8454)
 H7A(0.496) H7B(0.4289) H10A(0.3448) H10B(0.1932) H10C(0.2877) H11A(0.1222)
 H11B(0.0266) H11C(0.0748) H12A(0.267) H12B(0.165) H12C(0.1148) H13A(0.4442)
 H13B(0.5909) H16A(0.5117) H16B(0.5531) H16C(0.4424) H17A(0.7262) H17B(0.574)
 H17C(0.6849) H18A(0.8367) H18B(0.7973) H18C(0.7546)
 Fixed Z: H1A(0.1954) H1B(0.2234) H4A(0.023) H4B(0.0016) H4C(0.0406)
 H5A(0.0908) H5B(0.0517) H5C(0.1042) H6A(0.0454) H6B(0.0758) H6C(0.0234)
 H7A(0.2007) H7B(0.2364) H10A(0.0437) H10B(0.0378) H10C(0.074) H11A(0.1397)
 H11B(0.1039) H11C(0.1503) H12A(0.0601) H12B(0.1016) H12C(0.0555) H13A(0.2197)
 H13B(0.241) H16A(0.1195) H16B(0.0659) H16C(0.0814) H17A(0.0553) H17B(0.0417)
 H17C(0.0267) H18A(0.1176) H18B(0.0888) H18C(0.1422) N5(0.25) O4(0.25)
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