Large Anisotropy Barrier in a Tetranuclear Single-Molecule Magnet Featuring Low-Coordinate Cobalt Centers.
Chakarawet, Khetpakorn; Bunting, Philip C.; Long, Jeffrey R.; Journal of the American Chemical Society  (2018) –; doi:10.1021/jacs.7b13394

data_4127133
_publ_section_title
;
 Large Anisotropy Barrier in a Tetranuclear Single-Molecule Magnet
 Featuring Low-Coordinate Cobalt Centers.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b13394
_journal_year                    2018
_chemical_formula_moiety
'C48 H108 Co4 N4 P4, B C24 F20, 1.61(C6 H4 F2)'
_chemical_formula_sum            'C81.68 H114.45 B Co4 F23.23 N4 P4'
_chemical_formula_weight         1964.00
_chemical_name_common            '[{Co(NPtBu3)}4][B(C6F5)4]'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'intrinsic phasing'
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-03-14
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_cell_angle_alpha                105.210(3)
_cell_angle_beta                 98.201(3)
_cell_angle_gamma                90.612(3)
_cell_formula_units_Z            2
_cell_length_a                   12.9197(7)
_cell_length_b                   17.4852(9)
_cell_length_c                   20.7494(11)
_cell_measurement_reflns_used    9546
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      28.99
_cell_measurement_theta_min      2.57
_cell_volume                     4471.2(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            59933
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         28.575
_diffrn_reflns_theta_min         2.128
_diffrn_source
;
Advanced Light Source, station 11.3.1
;
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.124
_exptl_absorpt_correction_T_max  0.972
_exptl_absorpt_correction_T_min  0.887
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0769 before and 0.0458 after correction.
The Ratio of minimum to maximum transmission is 0.9125.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2029
_exptl_crystal_size_max          0.071
_exptl_crystal_size_mid          0.054
_exptl_crystal_size_min          0.025
_refine_diff_density_max         1.647
_refine_diff_density_min         -0.800
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1254
_refine_ls_number_reflns         17562
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0556
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0803P)^2^+8.4610P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1509
_refine_ls_wR_factor_ref         0.1642
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13518
_reflns_number_total             17562
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b13394_si_002.cif
_cod_data_source_block           kjc063s
_cod_database_code               4127133
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.972
_shelx_estimated_absorpt_t_min   0.924
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 C21, C22, C22A, C23, C23A, C24, C24A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C31, C32, C32A, C33, C33A, C34, C34A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C11, C12, C12A, C13, C13A, C14, C14A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(Co1A)=Sof(Co2A)=Sof(Co3A)=Sof(Co4A)=1-FVAR(1)
 Sof(Co1)=Sof(Co2)=Sof(Co3)=Sof(Co4)=FVAR(1)
 Sof(F2E)=Sof(H2D)=1-FVAR(2)
 Sof(F2D)=Sof(H6D)=FVAR(2)
 Sof(C22A)=Sof(H22D)=Sof(H22E)=Sof(H22F)=Sof(C23A)=Sof(H23D)=Sof(H23E)=
 Sof(H23F)=Sof(C24A)=Sof(H24D)=Sof(H24E)=Sof(H24F)=1-FVAR(3)
 Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=
 Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=FVAR(3)
 Sof(F7D)=Sof(F8D)=Sof(C9D)=Sof(H9D)=Sof(C10D)=Sof(H10J)=Sof(C11D)=Sof(H11J)=
 Sof(C12D)=Sof(H12P)=Sof(C7D)=Sof(C8D)=FVAR(4)
 Sof(C32A)=Sof(H32D)=Sof(H32E)=Sof(H32F)=Sof(C33A)=Sof(H33D)=Sof(H33E)=
 Sof(H33F)=Sof(C34A)=Sof(H34D)=Sof(H34E)=Sof(H34F)=1-FVAR(5)
 Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=
 Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=FVAR(5)
 Sof(C12A)=Sof(H12M)=Sof(H12N)=Sof(H12O)=Sof(C13A)=Sof(H13D)=Sof(H13E)=
 Sof(H13F)=Sof(C14A)=Sof(H14D)=Sof(H14E)=Sof(H14F)=1-FVAR(6)
 Sof(C12)=Sof(H12J)=Sof(H12K)=Sof(H12L)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=
 Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=FVAR(6)
4.a Me refined with riding coordinates:
 C123(H12D,H12E,H12F)
4.b Aromatic/amide H refined with riding coordinates:
 C9D(H9D), C10D(H10J), C11D(H11J), C12D(H12P), C2D(H2D), C3D(H3D), C4D(H4D),
 C5D(H5D), C6D(H6D)
4.c Fitted hexagon refined as free rotating group:
 C9D(C10D,C11D,C12D,C7D,C8D)
4.d Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C52(H52A,H52B,
 H52C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C62(H62A,H62B,H62C), C63(H63A,
 H63B,H63C), C64(H64A,H64B,H64C), C72(H72A,H72B,H72C), C73(H73A,H73B,H73C),
 C74(H74A,H74B,H74C), C82(H82A,H82B,H82C), C83(H83A,H83B,H83C), C84(H84A,H84B,
 H84C), C92(H92A,H92B,H92C), C93(H93A,H93B,H93C), C94(H94A,H94B,H94C),
 C102(H10A,H10B,H10C), C103(H10D,H10E,H10F), C104(H10G,H10H,H10I), C112(H11A,
 H11B,H11C), C113(H11D,H11E,H11F), C114(H11G,H11H,H11I), C122(H12A,H12B,H12C),
 C124(H12G,H12H,H12I), C12(H12J,H12K,H12L), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C32(H32A,
 H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C12A(H12M,H12N,H12O),
 C13A(H13D,H13E,H13F), C14A(H14D,H14E,H14F), C22A(H22D,H22E,H22F), C23A(H23D,
 H23E,H23F), C24A(H24D,H24E,H24F), C32A(H32D,H32E,H32F), C33A(H33D,H33E,H33F),
 C34A(H34D,H34E,H34F)
;
_shelx_res_checksum              59743
_shelx_hkl_checksum              94469
_olex2_submission_special_instructions 'No special instructions were received'