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_4346650
_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         'C45 H84 Cr F Ni2 O18'
_chemical_formula_sum            'C45 H84 Cr F Ni2 O18'
_chemical_formula_weight         1101.54
_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_Hall           '-C 2c 2'
_space_group_name_H-M_alt        'C m c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-09-26
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.4480(10)
_cell_length_b                   20.356(2)
_cell_length_c                   17.1920(10)
_cell_measurement_reflns_used    11624
_cell_measurement_temperature    230
_cell_measurement_theta_max      25.7430
_cell_measurement_theta_min      3.4430
_cell_volume                     6456.1(8)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49)'
_computing_data_collection
'CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49)'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49)'
_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      230
_diffrn_detector_area_resol_mean 8.0714
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega   28.00   54.00   1.0000    1.8900
omega____ theta____ kappa____ phi______ frames
    -       20.9454  -77.0000  -90.0000 26

  2 omega   36.00  103.00   1.0000    1.8900
omega____ theta____ kappa____ phi______ frames
    -       20.9454 -178.0000  -60.0000 67

  3 omega  -20.00   66.00   1.0000    1.8900
omega____ theta____ kappa____ phi______ frames
    -       20.9454  -99.0000  120.0000 86

  4 omega  -42.00   27.00   1.0000    1.8900
omega____ theta____ kappa____ phi______ frames
    -       20.9454  -57.0000  -90.0000 69

  5 omega  -50.00  -24.00   1.0000    1.8900
omega____ theta____ kappa____ phi______ frames
    -       20.9454  -77.0000  -90.0000 26

  6 omega  -90.00   12.00   1.0000    1.8900
omega____ theta____ kappa____ phi______ frames
    -      -21.1798  -77.0000  150.0000 102

  7 omega  -93.00   11.00   1.0000    1.8900
omega____ theta____ kappa____ phi______ frames
    -      -21.1798  -77.0000  -90.0000 104

  8 omega  -44.00   49.00   1.0000    1.8900
omega____ theta____ kappa____ phi______ frames
    -      -21.1798   57.0000   30.0000 93

  9 omega  -93.00   11.00   1.0000    1.8900
omega____ theta____ kappa____ phi______ frames
    -      -21.1798  -77.0000   30.0000 104

 10 omega   -5.00   49.00   1.0000    1.8900
omega____ theta____ kappa____ phi______ frames
    -      -21.1798   57.0000  150.0000 54
;
_diffrn_measurement_device_type  'SuperNova, Sungle source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0322473000
_diffrn_orient_matrix_UB_12      -0.0033231000
_diffrn_orient_matrix_UB_13      0.0228278000
_diffrn_orient_matrix_UB_21      -0.0173166000
_diffrn_orient_matrix_UB_22      0.0170170000
_diffrn_orient_matrix_UB_23      0.0312948000
_diffrn_orient_matrix_UB_31      -0.0130878000
_diffrn_orient_matrix_UB_32      -0.0306313000
_diffrn_orient_matrix_UB_33      0.0147967000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0848
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            37659
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         3.102
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.801
_exptl_absorpt_correction_type   none
_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    1.133
_exptl_crystal_description       block
_exptl_crystal_F_000             2348
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.483
_refine_diff_density_min         -0.579
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         3168
_refine_ls_number_restraints     419
_refine_ls_restrained_S_all      1.212
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0634
_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^)+(0.1282P)^2^+9.2001P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1907
_refine_ls_wR_factor_ref         0.2017
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2680
_reflns_number_total             3168
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01898_si_002.cif
_cod_data_source_block           1
_cod_database_code               4346650
_chemical_oxdiff_formula         'C45 H84 Cr Ni2 F O18'
_reflns_odcompleteness_completeness 99.66
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Shared sites
{Cr1, Ni1}
{Cr2, Ni2}
3. Restrained distances
 C6-C9
 1.54 with sigma of 0.02
 C8-C6 = C6-C7
 1.54 with sigma of 0.02
 C4-C2 = C2-C3
 1.54 with sigma of 0.02
 C7-C10
 2.515 with sigma of 0.04
 C8-C9
 2.515 with sigma of 0.04
 C8-C7
 2.515 with sigma of 0.04
 C4-C3
 1.416 with sigma of 0.04
 O3-C5 \\sim O4-C5 \\sim O5-C5
 with sigma of 0.02
4. Rigid bond restraints
 C11, C12, C13, C14, C15, C16, C17, C19, C18, C1, C2, C4, C3, C5, C6, C10, C8,
 C9, C7
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
5. Uiso/Uaniso restraints and constraints
C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C19 \\sim
C18 \\sim C1 \\sim C2 \\sim C4 \\sim C3 \\sim C5 \\sim C6 \\sim C10 \\sim C8
\\sim C9 \\sim C7: within 1.7A with sigma of 0.04 and sigma for terminal atoms
of 0.08
Uanis(Cr1) = Uanis(Ni1)
Uanis(Cr2) = Uanis(Ni2)
6. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Fixed Sof: Ni1(0.16667) Cr1(0.08333) Ni2(0.33333) Cr2(0.16667) O2(0.25)
 H2(0.25) O5(0.25) H5(0.25) O4(0.25) H4(0.25) H19A(0.5) H19B(0.5) H19C(0.5)
 C1(0.25) C4(0.25) H4A(0.25) H4B(0.25) H4C(0.25) C3(0.5) H3A(0.5) H3B(0.5)
 H3C(0.5) C5(0.5) C10(0.25) H10A(0.25) H10B(0.25) H10C(0.25) C8(0.5) H8A(0.5)
 H8B(0.5) H8C(0.5) C9(0.5) H9A(0.5) H9B(0.5) H9C(0.5) C7(0.25) H7A(0.25)
 H7B(0.25) H7C(0.25)
8.a Me refined with riding coordinates:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C19(H19A,H19B,
 H19C), C18(H18A,H18B,H18C), C4(H4A,H4B,H4C), C3(H3A,H3B,H3C), C10(H10A,H10B,
 H10C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C7(H7A,H7B,H7C)
8.b Tetrahedral OH refined with riding coordinates:
 O2(H2), O5(H5), O4(H4)
;
_shelx_res_checksum              24059
_shelx_hkl_checksum              35937
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'