Anisotropy of Co<sup>II</sup> transferred to the Cr<sub>7</sub>Co polymetallic cluster <i>via</i> strong exchange interactions.
Garlatti, Elena; Guidi, Tatiana; Chiesa, Alessandro; Ansbro, Simon; Baker, Michael L.; Ollivier, Jacques; Mutka, Hannu; Timco, Grigore A.; Vitorica-Yrezabal, Inigo; Pavarini, Eva; Santini, Paolo; Amoretti, Giuseppe; Winpenny, Richard E. P.; Carretta, Stefano; Chemical science 9 (2018) 3555–3562; doi:10.1039/c8sc00163d

data_1549029
_publ_section_title
;
 Anisotropy of Co<sup>II</sup> transferred to the Cr<sub>7</sub>Co
 polymetallic cluster <i>via</i> strong exchange interactions.
;
_journal_issue                   14
_journal_name_full               'Chemical science'
_journal_page_first              3555
_journal_page_last               3562
_journal_paper_doi               10.1039/c8sc00163d
_journal_volume                  9
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C80 H144 Co Cr7 F8 O32, 0.25(C8 H8 N4), C4 H10 O'
_chemical_formula_sum            'C86 H162 Co Cr7 F8 N O33'
_chemical_formula_weight         2313.09
_space_group_crystal_system      tetragonal
_space_group_IT_number           79
_space_group_name_Hall           'I 4'
_space_group_name_H-M_alt        'I 4'
_symmetry_space_group_name_Hall  'I 4'
_symmetry_space_group_name_H-M   'I 4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-12-12
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-12-12 deposited with the CCDC.
2018-03-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.9066(6)
_cell_length_b                   19.9066(6)
_cell_length_c                   16.1991(9)
_cell_measurement_reflns_used    5481
_cell_measurement_temperature    150.02(10)
_cell_measurement_theta_max      27.1120
_cell_measurement_theta_min      3.8210
_cell_volume                     6419.3(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.02(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.881
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -82.00  33.00   1.00    2.50    --  -17.77   0.00  60.00  115
  2  \w    -69.00   9.00   1.00    2.50    --  -17.77 -77.00-120.00   78
  3  \w     18.00  58.00   1.00    2.50    --   18.70-102.00 -39.00   40
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0051763000
_diffrn_orient_matrix_UB_12      0.0333401000
_diffrn_orient_matrix_UB_13      -0.0141737000
_diffrn_orient_matrix_UB_21      0.0345003000
_diffrn_orient_matrix_UB_22      0.0071994000
_diffrn_orient_matrix_UB_23      0.0064192000
_diffrn_orient_matrix_UB_31      0.0072406000
_diffrn_orient_matrix_UB_32      -0.0103523000
_diffrn_orient_matrix_UB_33      -0.0409133000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_unetI/netI     0.0683
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.881
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15604
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.833
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.255
_diffrn_reflns_theta_min         3.318
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.768
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53625
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.197
_exptl_crystal_description       block
_exptl_crystal_F_000             2432
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.942
_refine_diff_density_min         -0.785
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details
;
 Flack x determined using 2205 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.021(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         7329
_refine_ls_number_restraints     282
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0839
_refine_ls_R_factor_gt           0.0675
_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^)+(0.1228P)^2^+1.1679P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1852
_refine_ls_wR_factor_ref         0.2016
_reflns_Friedel_coverage         0.830
_reflns_Friedel_fraction_full    0.986
_reflns_Friedel_fraction_max     0.782
_reflns_number_gt                5896
_reflns_number_total             7329
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc00163d2.cif
_cod_data_source_block           arepw1038
_cod_depositor_comments          'Adding full bibliography for 1549029.cif.'
_cod_original_cell_volume        6419.3(5)
_cod_database_code               1549029
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         Cr7CoF8O32C80N1H100
_reflns_odcompleteness_completeness 99.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{Co1, Cr1}
{Co2, Cr2}
3. Restrained distances
 C2-C15
 1.54 with sigma of 0.02
 C15-O3
 1.45 with sigma of 0.02
 C13-C11 \\sim C14-C11 \\sim C12-C11 \\sim C28-C25 \\sim C27-C25 \\sim C26-C25
\\sim C21-C18 \\sim C20-C18
 \\sim C19-C18 \\sim C7-C4 \\sim C6-C4 \\sim C5-C4
 with sigma of 0.001
 C12-C13 \\sim C13-C14 \\sim C14-C12
 with sigma of 0.001
4. Uiso/Uaniso restraints and constraints
C11 \\sim C13 \\sim C12: within 2A with sigma of 0.002 and sigma for terminal
atoms of 0.004
Uanis(Cr1) = Uanis(Co1)
Uanis(Co1) = Uanis(Cr1)
Uanis(Cr2) = Uanis(Co2)
Uanis(Co2) = Uanis(Cr2)
5. Rigid body (RIGU) restrains
 C14, C13, C12, C11, O8, C10, O9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C6, C4, C5, C7, C3, O1, O2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C20, C18, C19, C21, C17, O15, O16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C28, C25, C27, C26, O23, C24, O22
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C2, C15, O3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C31, N30, C29
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: Cr1(0.875) Cr2(0.875) N30(0.25) H30A(0.25) H30B(0.25) Co2(0.125)
 Co1(0.125) C2(0.5) H2A(0.5) H2B(0.5) H2C(0.5) C15(0.5) H15A(0.5) H15B(0.5)
7.a Secondary CH2 refined with riding coordinates:
 N30(H30A,H30B), C15(H15A,H15B)
7.b Me refined with riding coordinates:
 C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C5(H5A,H5B,H5C), C19(H19A,H19B,
 H19C), C7(H7A,H7B,H7C), C21(H21A,H21B,H21C), C13(H13A,H13B,H13C), C27(H27A,
 H27B,H27C), C12(H12A,H12B,H12C), C20(H20A,H20B,H20C), C14(H14A,H14B,H14C),
 C6(H6A,H6B,H6C), C2(H2A,H2B,H2C)
;
_shelx_res_checksum              9020
_shelx_hkl_checksum              21047
_olex2_date_sample_data_collection 2015-10-19
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.362
_oxdiff_exptl_absorpt_empirical_full_min 0.625