Electronic Structure of a Mixed-Metal Fluoride-Centered Triangle Complex: A Potential Qubit Component.
Walsh, James P. S.; Meadows, Sarah B.; Ghirri, Alberto; Moro, Fabrizio; Jennings, Martin; Smith, William F.; Graham, Darren M.; Kihara, Takumi; Nojiri, Hiroyuki; Vitorica-Yrezabal, Iñigo J; Timco, Grigore A.; Collison, David; McInnes, Eric J. L.; Winpenny, Richard E. P.; Inorganic chemistry 54 (2015) 12019–12026; doi:10.1021/acs.inorgchem.5b01898

data_4346652
_publ_section_title
;
 Electronic Structure of a Mixed-Metal Fluoride-Centered Triangle Complex:
 A Potential Qubit Component.
;
_journal_issue                   24
_journal_name_full               'Inorganic chemistry'
_journal_page_first              12019
_journal_page_last               12026
_journal_paper_doi               10.1021/acs.inorgchem.5b01898
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C48 H75 Cr F N3 Ni2 O12'
_chemical_formula_sum            'C48 H75 Cr F N3 Ni2 O12'
_chemical_formula_weight         1074.53
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-07-25
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 107.789(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.6137(8)
_cell_length_b                   20.4729(11)
_cell_length_c                   12.3998(9)
_cell_measurement_reflns_used    2820
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.0200
_cell_measurement_theta_min      3.3900
_cell_volume                     2807.3(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
(compiled Mar 18 2013,11:47:30)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
(compiled Mar 18 2013,11:47:30)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
(compiled Mar 18 2013,11:47:30)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3367
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega   -5.00  108.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4473   37.0000  -60.0000 113

  2 omega   -4.00  108.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4473   77.0000  150.0000 112
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0454866000
_diffrn_orient_matrix_UB_12      0.0070063000
_diffrn_orient_matrix_UB_13      -0.0516918000
_diffrn_orient_matrix_UB_21      0.0361038000
_diffrn_orient_matrix_UB_22      -0.0144685000
_diffrn_orient_matrix_UB_23      -0.0304049000
_diffrn_orient_matrix_UB_31      -0.0273712000
_diffrn_orient_matrix_UB_32      -0.0307031000
_diffrn_orient_matrix_UB_33      0.0026222000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0531
_diffrn_reflns_av_unetI/netI     0.1103
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10578
_diffrn_reflns_point_group_measured_fraction_full 0.787
_diffrn_reflns_point_group_measured_fraction_max 0.770
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.896
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.913
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70378
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
(compiled Mar 18 2013,11:47:30)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_description       block
_exptl_crystal_F_000             1138
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.595
_refine_diff_density_min         -0.772
_refine_diff_density_rms         0.124
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
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_refine_ls_abs_structure_Flack   0.04(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         8858
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0996
_refine_ls_R_factor_gt           0.0738
_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^)+(0.0879P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1683
_refine_ls_wR_factor_ref         0.1983
_reflns_Friedel_coverage         0.504
_reflns_Friedel_fraction_full    0.564
_reflns_Friedel_fraction_max     0.532
_reflns_number_gt                6821
_reflns_number_total             8858
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01898_si_002.cif
_cod_data_source_block           3
_cod_database_code               4346652
_chemical_oxdiff_formula         C48H75FNi2CrO12
_reflns_odcompleteness_completeness 98.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_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. Restrained distances
 C57-C53
 1.54 with sigma of 0.02
 C58-C53 = C53-C59
 1.54 with sigma of 0.02
 C56-C53
 1.54 with sigma of 0.02
 C55-C53 = C53-C54
 1.54 with sigma of 0.02
 C45-C41
 1.54 with sigma of 0.02
 C6-C41 = C41-C47
 1.54 with sigma of 0.02
 C43-C41
 1.54 with sigma of 0.02
 C42-C41 = C41-C44
 1.54 with sigma of 0.02
 C36-C33
 1.54 with sigma of 0.02
 C35-C33 = C33-C34
 1.54 with sigma of 0.02
 C39-C33
 1.54 with sigma of 0.02
 C38-C33 = C33-C37
 1.54 with sigma of 0.02
 C23-C20
 1.54 with sigma of 0.02
 C22-C20
 1.54 with sigma of 0.02
 C25-C20
 1.54 with sigma of 0.02
 C20-C26
 1.54 with sigma of 0.02
 C24-C20 = C20-C21
 1.54 with sigma of 0.02
 C59-C57
 2.515 with sigma of 0.04
 C57-C58
 2.515 with sigma of 0.04
 C58-C59
 2.515 with sigma of 0.04
 C54-C56
 2.515 with sigma of 0.04
 C56-C55
 2.515 with sigma of 0.04
 C55-C54
 2.515 with sigma of 0.04
 C47-C45
 2.515 with sigma of 0.04
 C45-C6
 2.515 with sigma of 0.04
 C6-C47
 2.515 with sigma of 0.04
 C44-C43
 2.515 with sigma of 0.04
 C43-C42
 2.515 with sigma of 0.04
 C42-C44
 2.515 with sigma of 0.04
 C34-C36
 2.515 with sigma of 0.04
 C36-C35
 2.515 with sigma of 0.04
 C35-C34
 2.515 with sigma of 0.04
 C37-C39
 2.515 with sigma of 0.04
 C39-C38
 2.515 with sigma of 0.04
 C38-C37
 2.515 with sigma of 0.04
 C21-C23
 2.515 with sigma of 0.04
 C23-C22
 2.515 with sigma of 0.04
 C22-C21
 2.515 with sigma of 0.04
 C26-C25
 2.515 with sigma of 0.04
 C25-C24
 2.515 with sigma of 0.04
 C24-C26
 2.515 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C59) = Uanis(C54) = Uanis(C57) = Uanis(C55) = Uanis(C58) = Uanis(C56)
Uanis(C47) = Uanis(C42) = Uanis(C45) = Uanis(C43) = Uanis(C6) = Uanis(C44)
Uanis(C37) = Uanis(C34) = Uanis(C39) = Uanis(C36) = Uanis(C38) = Uanis(C35)
Uanis(C23) = Uanis(C25) = Uanis(C22) = Uanis(C24) = Uanis(C21) = Uanis(C26)
4. Others
 Sof(C58)=Sof(H58A)=Sof(H58B)=Sof(H58C)=Sof(C59)=Sof(H59A)=Sof(H59B)=Sof(H59C)=
 Sof(C57)=Sof(H57A)=Sof(H57B)=Sof(H57C)=1-FVAR(1)
 Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(H56C)=Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(H55C)=
 Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(H54C)=FVAR(1)
 Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(H44C)=Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(H43C)=
 Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(H42C)=1-FVAR(2)
 Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(H47C)=
 Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(H45C)=FVAR(2)
 Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=
 Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=1-FVAR(3)
 Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=
 Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(H37C)=FVAR(3)
 Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=
 Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=1-FVAR(4)
 Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=
 Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=FVAR(4)
5.a Me refined with riding coordinates:
 C56(H56A,H56B,H56C), C21(H21A,H21B,H21C), C6(H6A,H6B,H6C), C47(H47A,H47B,
 H47C), C45(H45A,H45B,H45C), C55(H55A,H55B,H55C), C54(H54A,H54B,H54C), C38(H38A,
 H38B,H38C), C39(H39A,H39B,H39C), C37(H37A,H37B,H37C), C22(H22A,H22B,H22C),
 C23(H23A,H23B,H23C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C57(H57A,H57B,
 H57C), C44(H44A,H44B,H44C), C43(H43A,H43B,H43C), C42(H42A,H42B,H42C), C36(H36A,
 H36B,H36C), C35(H35A,H35B,H35C), C34(H34A,H34B,H34C), C25(H25A,H25B,H25C),
 C24(H24A,H24B,H24C), C26(H26A,H26B,H26C)
5.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C5(H5), C13(H13), C17(H17), C10(H10), C1(H1), C2(H2), C16(H16),
 C14(H14), C8(H8), C4(H4), C7(H7)
5.c Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C29(H29A,H29B,H29C), C49(H49A,H49B,
 H49C), C50(H50A,H50B,H50C), C18(H18A,H18B,H18C), C51(H51A,H51B,H51C), C12(H12A,
 H12B,H12C), C1A(H1AA,H1AB,H1AC)
;
_shelx_res_checksum              3019
_shelx_hkl_checksum              21324
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'