Chromium chains as polydentate fluoride ligands for actinides and group IV metals.
Leng, Ji-Dong; Kostopoulos, Andreas K.; Isherwood, Liam H.; Ariciu, Ana-Maria; Tuna, Floriana; Vitórica-Yrezábal, Iñigo J; Pritchard, Robin G.; Whitehead, George F. S.; Timco, Grigore A.; Mills, David P.; Winpenny, Richard E. P.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 6361–6369; doi:10.1039/c8dt00803e

data_7046048
_publ_section_title
;
 Chromium chains as polydentate fluoride ligands for actinides and group
 IV metals.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6361
_journal_page_last               6369
_journal_paper_doi               10.1039/c8dt00803e
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety
'C77 H141 Cr6 F7 O31 S Th, C4 H8 O, C5 H10 O2, 2(C2 H3 N)'
_chemical_formula_sum            'C90 H165 Cr6 F7 N2 O34 S Th'
_chemical_formula_weight         2528.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-02-15
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-02-15 deposited with the CCDC.
2018-03-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.4775(14)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   35.4782(4)
_cell_length_b                   29.7042(3)
_cell_length_c                   24.7842(4)
_cell_measurement_reflns_used    20709
_cell_measurement_temperature    150.02(10)
_cell_measurement_theta_max      25.9320
_cell_measurement_theta_min      2.6000
_cell_volume                     25171.7(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_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 16.1428
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.992
_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    -19.00  25.00   0.50   15.00    --  -20.24 -99.00   0.00   88
  2  \w    -46.00  49.00   0.50   15.00    --   21.65 -77.00 120.00  190
  3  \w    -18.00  45.00   0.50   15.00    --   21.65 -77.00-120.00  126
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0140650000
_diffrn_orient_matrix_UB_12      0.0137496000
_diffrn_orient_matrix_UB_13      0.0076800000
_diffrn_orient_matrix_UB_21      0.0152590000
_diffrn_orient_matrix_UB_22      0.0127733000
_diffrn_orient_matrix_UB_23      0.0177666000
_diffrn_orient_matrix_UB_31      -0.0001010000
_diffrn_orient_matrix_UB_32      0.0147655000
_diffrn_orient_matrix_UB_33      -0.0225222000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_unetI/netI     0.0846
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            88604
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.406
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.769
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81287
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.30c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_description       block
_exptl_crystal_F_000             10432
_exptl_crystal_size_max          0.303
_exptl_crystal_size_mid          0.245
_exptl_crystal_size_min          0.109
_refine_diff_density_max         1.166
_refine_diff_density_min         -1.058
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3186
_refine_ls_number_reflns         51081
_refine_ls_number_restraints     8175
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.1093
_refine_ls_R_factor_gt           0.0578
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0421P)^2^+57.3690P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1122
_refine_ls_wR_factor_ref         0.1343
_reflns_Friedel_coverage         0.000
_reflns_number_gt                32762
_reflns_number_total             51081
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00803e2.cif
_cod_data_source_block           adpm291
_cod_depositor_comments
'Adding full bibliography for 7046044--7046048.cif.'
_cod_original_cell_volume        25171.6(6)
_cod_database_code               7046048
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         C90H165Cr6F7N2O34STh
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Shared sites
{C2, C2A}
{C7, C7A}
{C12, C12A}
{C17, C17A}
{C32, C32A}
{C37, C37A}
{C42, C42A}
{C47, C47A}
{C57, C57A}
{C67, C67A}
{C7B, C7C}
{C12B, C12C}
{C17B, C17C}
{C22B, C22C}
{C32B, C32C}
{C37B, C37C}
{C42B, C42C}
{C47B, C47C}
{C52B, C52C}
3. Restrained distances
 C60C-C56B
 2.4 with sigma of 0.02
 C5E-C2E = C3E-C2E = C4E-C2E = C2E-C1E
 1.54 with sigma of 0.02
 C5B-C2B \\sim C3B-C2B \\sim C4B-C2B
 with sigma of 0.02
 O1B-C2B \\sim C2B-O2B
 with sigma of 0.02
 S1A-C77A \\sim S1-C77 \\sim S1A-C76A \\sim S1-C76
 with sigma of 0.02
 S1A-O29 \\sim S1-O29
 with sigma of 0.02
 O29-C77A \\sim O29-C77 \\sim O29-C76A \\sim O29-C76
 with sigma of 0.02
 C4D-C3D \\sim C3D-C2D \\sim C2D-C1D
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C5F \\sim N3F \\sim C6F \\sim C3F \\sim N2F \\sim C4F \\sim C1F \\sim N1F \\sim
C2F \\sim N4F \\sim C7F \\sim C8F: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C77A \\sim C77 \\sim S1A \\sim S1 \\sim C76A \\sim C76: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
C2A \\sim C3A \\sim C4A \\sim C5A \\sim C7A \\sim C8A \\sim C9A \\sim C10A
\\sim C12A \\sim C13A \\sim C14A \\sim C15A \\sim C17A \\sim C18A \\sim C19A
\\sim C20A \\sim C32A \\sim C33A \\sim C34A \\sim C35A \\sim C37A \\sim C38A
\\sim C39A \\sim C40A \\sim C42A \\sim C43A \\sim C44A \\sim C45A \\sim C47A
\\sim C48A \\sim C49A \\sim C50A \\sim C57A \\sim C58A \\sim C59A \\sim C60A
\\sim C67A \\sim C68A \\sim C69A \\sim C70A \\sim C7C \\sim C8C \\sim C9C \\sim
C10C \\sim C12C \\sim C13C \\sim C14C \\sim C15C \\sim C17C \\sim C18C \\sim
C19C \\sim C20C \\sim C22C \\sim C23C \\sim C24C \\sim C25C \\sim C32C \\sim
C33C \\sim C34C \\sim C35C \\sim C37C \\sim C38C \\sim C39C \\sim C40C \\sim
C42C \\sim C43C \\sim C44C \\sim C45C \\sim C47C \\sim C48C \\sim C49C \\sim
C50C \\sim C52C \\sim C53C \\sim C54C \\sim C55C \\sim C57C \\sim C58C \\sim
C59C \\sim C60C \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C17 \\sim C18 \\sim C19
\\sim C20 \\sim C32 \\sim C33 \\sim C34 \\sim C35 \\sim C37 \\sim C38 \\sim C39
\\sim C40 \\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C47 \\sim C48 \\sim C49
\\sim C50 \\sim C57 \\sim C58 \\sim C59 \\sim C60 \\sim C67 \\sim C68 \\sim C69
\\sim C70 \\sim C7B \\sim C8B \\sim C9B \\sim C10B \\sim C12B \\sim C13B \\sim
C14B \\sim C15B \\sim C17B \\sim C18B \\sim C19B \\sim C20B \\sim C22B \\sim
C23B \\sim C24B \\sim C25B \\sim C32B \\sim C33B \\sim C34B \\sim C35B \\sim
C37B \\sim C38B \\sim C39B \\sim C40B \\sim C42B \\sim C43B \\sim C44B \\sim
C45B \\sim C47B \\sim C48B \\sim C49B \\sim C50B \\sim C52B \\sim C53B \\sim
C54B \\sim C55B \\sim C57B \\sim C58B \\sim C59B \\sim C60B: within 2A with
sigma of 0.02 and sigma for terminal atoms of 0.01
C8D \\sim O2D \\sim C5D \\sim C6D \\sim C7D \\sim O3D \\sim C9D \\sim C12D
\\sim C10D \\sim C11D \\sim C4D \\sim O1D \\sim C1D \\sim C2D \\sim C3D \\sim
C1E \\sim O1E \\sim O2E \\sim C2E \\sim C3E \\sim C4E \\sim C5E: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C2) = Uanis(C2A)
Uanis(C7) = Uanis(C7A)
Uanis(C12) = Uanis(C12A)
Uanis(C17) = Uanis(C17A)
Uanis(C32) = Uanis(C32A)
Uanis(C37) = Uanis(C37A)
Uanis(C42) = Uanis(C42A)
Uanis(C47) = Uanis(C47A)
Uanis(C57) = Uanis(C57A)
Uanis(C67) = Uanis(C67A)
Uanis(C7B) = Uanis(C7C)
Uanis(C12B) = Uanis(C12C)
Uanis(C17B) = Uanis(C17C)
Uanis(C22B) = Uanis(C22C)
Uanis(C32B) = Uanis(C32C)
Uanis(C37B) = Uanis(C37C)
Uanis(C42B) = Uanis(C42C)
Uanis(C47B) = Uanis(C47C)
Uanis(C52B) = Uanis(C52C)
5. Rigid body (RIGU) restrains
 C5F, N3F, C6F, C3F, N2F, C4F, C1F, N1F, C2F, N4F, C7F, C8F
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C77, C77A, S1A, S1, C76A, C76
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C2, C3, C4, C5, C7, C8, C9, C10, C12, C13, C14, C15, C17, C18, C19, C20, C32,
 C33, C34, C35, C37, C38, C39, C40, C42, C43, C44, C45, C47, C48, C49, C50, C57,
  C58, C59, C60, C67, C68, C69, C70, C7B, C8B, C9B, C10B, C12B, C13B, C14B,
 C15B, C17B, C18B, C19B, C20B, C22B, C23B, C24B, C25B, C32B, C33B, C34B, C35B,
 C37B, C38B, C39B, C40B, C42B, C43B, C44B, C45B, C47B, C48B, C49B, C50B, C52B,
 C53B, C54B, C55B, C57B, C58B, C59B, C60B, C2A, C3A, C4A, C5A, C7A, C8A, C9A,
 C10A, C12A, C13A, C14A, C15A, C17A, C18A, C19A, C20A, C32A, C33A, C34A, C35A,
 C37A, C38A, C39A, C40A, C42A, C43A, C44A, C45A, C47A, C48A, C49A, C50A, C57A,
 C58A, C59A, C60A, C67A, C68A, C69A, C70A, C7C, C8C, C9C, C10C, C12C, C13C,
 C14C, C15C, C17C, C18C, C19C, C20C, C22C, C23C, C24C, C25C, C32C, C33C, C34C,
 C35C, C37C, C38C, C39C, C40C, C42C, C43C, C44C, C45C, C47C, C48C, C49C, C50C,
 C52C, C53C, C54C, C55C, C57C, C58C, C59C, C60C
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C8D, O2D, C5D, C6D, C7D, O3D, C9D, C12D, C10D, C11D, C4D, O1D, C1D, C2D, C3D,
 C1E, O1E, O2E, C2E, C3E, C4E, C5E
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Same fragment restrains
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as
{C2, C3, C4, C5}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as
{C7, C8, C9, C10}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as
{C12, C13, C14, C15}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as
{C17, C18, C19, C20}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as
{C32, C33, C34, C35}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as
{C37, C38, C39, C40}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as
{C42, C43, C44, C45}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as
{C47, C48, C49, C50}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as
{C57, C58, C59, C60}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as
{C67, C68, C69, C70}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as
{C7B, C8B, C9B, C10B}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as
{C12B, C13B, C14B, C15B}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as
{C17B, C18B, C19B, C20B}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as
{C22B, C23B, C24B, C25B}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as
{C32B, C33B, C34B, C35B}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as
{C37B, C38B, C39B, C40B}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as
{C42B, C43B, C44B, C45B}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as
{C47B, C48B, C49B, C50B}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as
{C52B, C53B, C54B, C55B}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as
{C57B, C58B, C59B, C60B}
{O1D, C1D, C2D, C3D, C4D} sigma for 1-2: 0.02, 1-3: 0.04
as
{O2D, C5D, C6D, C7D, C8D}
{O1D, C1D, C2D, C3D, C4D} sigma for 1-2: 0.02, 1-3: 0.04
as
{O3D, C9D, C10D, C11D, C12D}
{O1E, O2E, C1E, C2E, C3E, C4E, C5E} sigma for 1-2: 0.02, 1-3: 0.04
as
{O3E, O4E, C6E, C7E, C8E, C9E, C10E}
{N1F, C1F, C2F} sigma for 1-2: 0.02, 1-3: 0.04
as
{N2F, C3F, C4F}
{N1F, C1F, C2F} sigma for 1-2: 0.02, 1-3: 0.04
as
{N3F, C5F, C6F}
{N1F, C1F, C2F} sigma for 1-2: 0.02, 1-3: 0.04
as
{N4F, C7F, C8F}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as
{C2A, C3A, C4A, C5A}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as
{C7A, C8A, C9A, C10A}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as
{C12A, C13A, C14A, C15A}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as
{C17A, C18A, C19A, C20A}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as
{C32A, C33A, C34A, C35A}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as
{C37A, C38A, C39A, C40A}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as
{C42A, C43A, C44A, C45A}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as
{C47A, C48A, C49A, C50A}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as
{C57A, C58A, C59A, C60A}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as
{C67A, C68A, C69A, C70A}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as
{C7C, C8C, C9C, C10C}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as
{C12C, C13C, C14C, C15C}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as
{C17C, C18C, C19C, C20C}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as
{C22C, C23C, C24C, C25C}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as
{C32C, C33C, C34C, C35C}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as
{C37C, C38C, C39C, C40C}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as
{C42C, C43C, C44C, C45C}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as
{C47C, C48C, C49C, C50C}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as
{C52C, C53C, C54C, C55C}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as
{C57C, C58C, C59C, C60C}
7. Others
 Sof(O3D)=Sof(C9D)=Sof(H9DA)=Sof(H9DB)=Sof(C10D)=Sof(H10P)=Sof(H10Q)=Sof(C11D)=
 Sof(H11A)=Sof(H11B)=Sof(C12D)=Sof(H12A)=Sof(H12B)=1-FVAR(1)
 Sof(O2D)=Sof(C5D)=Sof(H5DA)=Sof(H5DB)=Sof(C6D)=Sof(H6DA)=Sof(H6DB)=Sof(C7D)=
 Sof(H7DA)=Sof(H7DB)=Sof(C8D)=Sof(H8DA)=Sof(H8DB)=FVAR(1)
 Sof(S1A)=Sof(C76A)=Sof(H76D)=Sof(H76E)=Sof(H76F)=Sof(C77A)=Sof(H77D)=
 Sof(H77E)=Sof(H77F)=1-FVAR(2)
 Sof(S1)=Sof(C76)=Sof(H76A)=Sof(H76B)=Sof(H76C)=Sof(C77)=Sof(H77A)=Sof(H77B)=
 Sof(H77C)=FVAR(2)
 Sof(C12C)=Sof(C13C)=Sof(H13J)=Sof(H13K)=Sof(H13L)=Sof(C14C)=Sof(H14J)=
 Sof(H14K)=Sof(H14L)=Sof(C15C)=Sof(H15J)=Sof(H15K)=Sof(H15L)=1-FVAR(3)
 Sof(C12B)=Sof(C13B)=Sof(H13G)=Sof(H13H)=Sof(H13I)=Sof(C14B)=Sof(H14G)=
 Sof(H14H)=Sof(H14I)=Sof(C15B)=Sof(H15G)=Sof(H15H)=Sof(H15I)=FVAR(3)
 Sof(C17C)=Sof(C18C)=Sof(H18J)=Sof(H18K)=Sof(H18L)=Sof(C19C)=Sof(H19J)=
 Sof(H19K)=Sof(H19L)=Sof(C20C)=Sof(H20J)=Sof(H20K)=Sof(H20L)=1-FVAR(4)
 Sof(C17B)=Sof(C18B)=Sof(H18G)=Sof(H18H)=Sof(H18I)=Sof(C19B)=Sof(H19G)=
 Sof(H19H)=Sof(H19I)=Sof(C20B)=Sof(H20G)=Sof(H20H)=Sof(H20I)=FVAR(4)
 Sof(C22C)=Sof(C23C)=Sof(H23G)=Sof(H23H)=Sof(H23I)=Sof(C24C)=Sof(H24G)=
 Sof(H24H)=Sof(H24I)=Sof(C25C)=Sof(H25G)=Sof(H25H)=Sof(H25I)=1-FVAR(5)
 Sof(C22B)=Sof(C23B)=Sof(H23D)=Sof(H23E)=Sof(H23F)=Sof(C24B)=Sof(H24D)=
 Sof(H24E)=Sof(H24F)=Sof(C25B)=Sof(H25D)=Sof(H25E)=Sof(H25F)=FVAR(5)
 Sof(C37C)=Sof(C38C)=Sof(H38J)=Sof(H38K)=Sof(H38L)=Sof(C39C)=Sof(H39J)=
 Sof(H39K)=Sof(H39L)=Sof(C40C)=Sof(H40J)=Sof(H40K)=Sof(H40L)=1-FVAR(6)
 Sof(C37B)=Sof(C38B)=Sof(H38G)=Sof(H38H)=Sof(H38I)=Sof(C39B)=Sof(H39G)=
 Sof(H39H)=Sof(H39I)=Sof(C40B)=Sof(H40G)=Sof(H40H)=Sof(H40I)=FVAR(6)
 Sof(C32C)=Sof(C33C)=Sof(H33J)=Sof(H33K)=Sof(H33L)=Sof(C34C)=Sof(H34J)=
 Sof(H34K)=Sof(H34L)=Sof(C35C)=Sof(H35J)=Sof(H35K)=Sof(H35L)=1-FVAR(7)
 Sof(C32B)=Sof(C33B)=Sof(H33G)=Sof(H33H)=Sof(H33I)=Sof(C34B)=Sof(H34G)=
 Sof(H34H)=Sof(H34I)=Sof(C35B)=Sof(H35G)=Sof(H35H)=Sof(H35I)=FVAR(7)
 Sof(C47C)=Sof(C48C)=Sof(H48J)=Sof(H48K)=Sof(H48L)=Sof(C49C)=Sof(H49J)=
 Sof(H49K)=Sof(H49L)=Sof(C50C)=Sof(H50J)=Sof(H50K)=Sof(H50L)=1-FVAR(8)
 Sof(C47B)=Sof(C48B)=Sof(H48G)=Sof(H48H)=Sof(H48I)=Sof(C49B)=Sof(H49G)=
 Sof(H49H)=Sof(H49I)=Sof(C50B)=Sof(H50G)=Sof(H50H)=Sof(H50I)=FVAR(8)
 Sof(C52C)=Sof(C53C)=Sof(H53G)=Sof(H53H)=Sof(H53I)=Sof(C54C)=Sof(H54G)=
 Sof(H54H)=Sof(H54I)=Sof(C55C)=Sof(H55G)=Sof(H55H)=Sof(H55I)=1-FVAR(9)
 Sof(C52B)=Sof(C53B)=Sof(H53D)=Sof(H53E)=Sof(H53F)=Sof(C54B)=Sof(H54D)=
 Sof(H54E)=Sof(H54F)=Sof(C55B)=Sof(H55D)=Sof(H55E)=Sof(H55F)=FVAR(9)
 Sof(C57C)=Sof(C58C)=Sof(H58J)=Sof(H58K)=Sof(H58L)=Sof(C59C)=Sof(H59J)=
 Sof(H59K)=Sof(H59L)=Sof(C60C)=Sof(H60J)=Sof(H60K)=Sof(H60L)=1-FVAR(10)
 Sof(C57B)=Sof(C58B)=Sof(H58G)=Sof(H58H)=Sof(H58I)=Sof(C59B)=Sof(H59G)=
 Sof(H59H)=Sof(H59I)=Sof(C60B)=Sof(H60G)=Sof(H60H)=Sof(H60I)=FVAR(10)
 Sof(C42C)=Sof(C43C)=Sof(H43J)=Sof(H43K)=Sof(H43L)=Sof(C44C)=Sof(H44J)=
 Sof(H44K)=Sof(H44L)=Sof(C45C)=Sof(H45J)=Sof(H45K)=Sof(H45L)=1-FVAR(11)
 Sof(C42B)=Sof(C43B)=Sof(H43G)=Sof(H43H)=Sof(H43I)=Sof(C44B)=Sof(H44G)=
 Sof(H44H)=Sof(H44I)=Sof(C45B)=Sof(H45G)=Sof(H45H)=Sof(H45I)=FVAR(11)
 Sof(C7C)=Sof(C8C)=Sof(H8CA)=Sof(H8CB)=Sof(H8CC)=Sof(C9C)=Sof(H9CA)=Sof(H9CB)=
 Sof(H9CC)=Sof(C10C)=Sof(H10J)=Sof(H10K)=Sof(H10L)=1-FVAR(12)
 Sof(C7B)=Sof(C8B)=Sof(H8BA)=Sof(H8BB)=Sof(H8BC)=Sof(C9B)=Sof(H9BA)=Sof(H9BB)=
 Sof(H9BC)=Sof(C10B)=Sof(H10G)=Sof(H10H)=Sof(H10I)=FVAR(12)
 Sof(C7A)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=
 Sof(H9AC)=Sof(C10A)=Sof(H10D)=Sof(H10E)=Sof(H10F)=1-FVAR(13)
 Sof(C7)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=
 Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=FVAR(13)
 Sof(C12A)=Sof(C13A)=Sof(H13D)=Sof(H13E)=Sof(H13F)=Sof(C14A)=Sof(H14D)=
 Sof(H14E)=Sof(H14F)=Sof(C15A)=Sof(H15D)=Sof(H15E)=Sof(H15F)=1-FVAR(14)
 Sof(C12)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C14)=Sof(H14A)=Sof(H14B)=
 Sof(H14C)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=FVAR(14)
 Sof(C17A)=Sof(C18A)=Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(C19A)=Sof(H19D)=
 Sof(H19E)=Sof(H19F)=Sof(C20A)=Sof(H20D)=Sof(H20E)=Sof(H20F)=1-FVAR(15)
 Sof(C17)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(C19)=Sof(H19A)=Sof(H19B)=
 Sof(H19C)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=FVAR(15)
 Sof(C37A)=Sof(C38A)=Sof(H38D)=Sof(H38E)=Sof(H38F)=Sof(C39A)=Sof(H39D)=
 Sof(H39E)=Sof(H39F)=Sof(C40A)=Sof(H40D)=Sof(H40E)=Sof(H40F)=1-FVAR(16)
 Sof(C37)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=Sof(C39)=Sof(H39A)=Sof(H39B)=
 Sof(H39C)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=FVAR(16)
 Sof(C42A)=Sof(C43A)=Sof(H43D)=Sof(H43E)=Sof(H43F)=Sof(C44A)=Sof(H44D)=
 Sof(H44E)=Sof(H44F)=Sof(C45A)=Sof(H45D)=Sof(H45E)=Sof(H45F)=1-FVAR(17)
 Sof(C42)=Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(H43C)=Sof(C44)=Sof(H44A)=Sof(H44B)=
 Sof(H44C)=Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(H45C)=FVAR(17)
 Sof(C57A)=Sof(C58A)=Sof(H58D)=Sof(H58E)=Sof(H58F)=Sof(C59A)=Sof(H59D)=
 Sof(H59E)=Sof(H59F)=Sof(C60A)=Sof(H60D)=Sof(H60E)=Sof(H60F)=1-FVAR(18)
 Sof(C57)=Sof(C58)=Sof(H58A)=Sof(H58B)=Sof(H58C)=Sof(C59)=Sof(H59A)=Sof(H59B)=
 Sof(H59C)=Sof(C60)=Sof(H60A)=Sof(H60B)=Sof(H60C)=FVAR(18)
 Sof(C67A)=Sof(C68A)=Sof(H68D)=Sof(H68E)=Sof(H68F)=Sof(C69A)=Sof(H69D)=
 Sof(H69E)=Sof(H69F)=Sof(C70A)=Sof(H70D)=Sof(H70E)=Sof(H70F)=1-FVAR(19)
 Sof(C67)=Sof(C68)=Sof(H68A)=Sof(H68B)=Sof(H68C)=Sof(C69)=Sof(H69A)=Sof(H69B)=
 Sof(H69C)=Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(H70C)=FVAR(19)
 Sof(C32A)=Sof(C33A)=Sof(H33D)=Sof(H33E)=Sof(H33F)=Sof(C34A)=Sof(H34D)=
 Sof(H34E)=Sof(H34F)=Sof(C35A)=Sof(H35D)=Sof(H35E)=Sof(H35F)=1-FVAR(20)
 Sof(C32)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=Sof(C34)=Sof(H34A)=Sof(H34B)=
 Sof(H34C)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=FVAR(20)
 Sof(C2A)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=
 Sof(H4AC)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(H5AC)=1-FVAR(21)
 Sof(C2)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=
 Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=FVAR(21)
 Sof(C47A)=Sof(C48A)=Sof(H48D)=Sof(H48E)=Sof(H48F)=Sof(C49A)=Sof(H49D)=
 Sof(H49E)=Sof(H49F)=Sof(C50A)=Sof(H50D)=Sof(H50E)=Sof(H50F)=1-FVAR(22)
 Sof(C47)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(H48C)=Sof(C49)=Sof(H49A)=Sof(H49B)=
 Sof(H49C)=Sof(C50)=Sof(H50A)=Sof(H50B)=Sof(H50C)=FVAR(22)
8.a Riding coordinates:
 O1E(H1E), O3E(H3E)
8.b Secondary CH2 refined with riding coordinates:
 C1D(H1DA,H1DB), C2D(H2DA,H2DB), C3D(H3DA,H3DB), C4D(H4DA,H4DB), C5D(H5DA,
 H5DB), C6D(H6DA,H6DB), C7D(H7DA,H7DB), C8D(H8DA,H8DB), C9D(H9DA,H9DB),
 C10D(H10P,H10Q), C11D(H11A,H11B), C12D(H12A,H12B)
8.c Me refined with riding coordinates:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C8(H8A,H8B,H8C), C9(H9A,
 H9B,H9C), C10(H10A,H10B,H10C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C15(H15A,H15B,H15C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C28(H28A,
 H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C33(H33A,H33B,H33C),
 C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C38(H38A,H38B,H38C), C39(H39A,H39B,
 H39C), C40(H40A,H40B,H40C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,
 H45B,H45C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C),
 C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C58(H58A,H58B,
 H58C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C63(H63A,H63B,H63C), C64(H64A,
 H64B,H64C), C65(H65A,H65B,H65C), C68(H68A,H68B,H68C), C69(H69A,H69B,H69C),
 C70(H70A,H70B,H70C), C73(H73A,H73B,H73C), C74(H74A,H74B,H74C), C75(H75A,H75B,
 H75C), C76(H76A,H76B,H76C), C77(H77A,H77B,H77C), C76A(H76D,H76E,H76F),
 C77A(H77D,H77E,H77F), C3B(H3BA,H3BB,H3BC), C4B(H4BA,H4BB,H4BC), C5B(H5BA,H5BB,
 H5BC), C8B(H8BA,H8BB,H8BC), C9B(H9BA,H9BB,H9BC), C10B(H10G,H10H,H10I),
 C13B(H13G,H13H,H13I), C14B(H14G,H14H,H14I), C15B(H15G,H15H,H15I), C18B(H18G,
 H18H,H18I), C19B(H19G,H19H,H19I), C20B(H20G,H20H,H20I), C23B(H23D,H23E,H23F),
 C24B(H24D,H24E,H24F), C25B(H25D,H25E,H25F), C28B(H28D,H28E,H28F), C29B(H29D,
 H29E,H29F), C30B(H30D,H30E,H30F), C33B(H33G,H33H,H33I), C34B(H34G,H34H,H34I),
 C35B(H35G,H35H,H35I), C38B(H38G,H38H,H38I), C39B(H39G,H39H,H39I), C40B(H40G,
 H40H,H40I), C43B(H43G,H43H,H43I), C44B(H44G,H44H,H44I), C45B(H45G,H45H,H45I),
 C48B(H48G,H48H,H48I), C49B(H49G,H49H,H49I), C50B(H50G,H50H,H50I), C53B(H53D,
 H53E,H53F), C54B(H54D,H54E,H54F), C55B(H55D,H55E,H55F), C58B(H58G,H58H,H58I),
 C59B(H59G,H59H,H59I), C60B(H60G,H60H,H60I), C63B(H63D,H63E,H63F), C64B(H64D,
 H64E,H64F), C65B(H65D,H65E,H65F), C68B(H68G,H68H,H68I), C69B(H69G,H69H,H69I),
 C70B(H70G,H70H,H70I), C73B(H73D,H73E,H73F), C74B(H74D,H74E,H74F), C75B(H75D,
 H75E,H75F), C76B(H76G,H76H,H76I), C77B(H77G,H77H,H77I), C3E(H3EA,H3EB,H3EC),
 C4E(H4EA,H4EB,H4EC), C5E(H5EA,H5EB,H5EC), C8E(H8EA,H8EB,H8EC), C9E(H9EA,H9EB,
 H9EC), C10E(H10M,H10N,H10O), C3A(H3AA,H3AB,H3AC), C4A(H4AA,H4AB,H4AC),
 C5A(H5AA,H5AB,H5AC), C8A(H8AA,H8AB,H8AC), C9A(H9AA,H9AB,H9AC), C10A(H10D,H10E,
 H10F), C13A(H13D,H13E,H13F), C14A(H14D,H14E,H14F), C15A(H15D,H15E,H15F),
 C18A(H18D,H18E,H18F), C19A(H19D,H19E,H19F), C20A(H20D,H20E,H20F), C33A(H33D,
 H33E,H33F), C34A(H34D,H34E,H34F), C35A(H35D,H35E,H35F), C38A(H38D,H38E,H38F),
 C39A(H39D,H39E,H39F), C40A(H40D,H40E,H40F), C43A(H43D,H43E,H43F), C44A(H44D,
 H44E,H44F), C45A(H45D,H45E,H45F), C48A(H48D,H48E,H48F), C49A(H49D,H49E,H49F),
 C50A(H50D,H50E,H50F), C58A(H58D,H58E,H58F), C59A(H59D,H59E,H59F), C60A(H60D,
 H60E,H60F), C68A(H68D,H68E,H68F), C69A(H69D,H69E,H69F), C70A(H70D,H70E,H70F),
 C8C(H8CA,H8CB,H8CC), C9C(H9CA,H9CB,H9CC), C10C(H10J,H10K,H10L), C13C(H13J,H13K,
 H13L), C14C(H14J,H14K,H14L), C15C(H15J,H15K,H15L), C18C(H18J,H18K,H18L),
 C19C(H19J,H19K,H19L), C20C(H20J,H20K,H20L), C23C(H23G,H23H,H23I), C24C(H24G,
 H24H,H24I), C25C(H25G,H25H,H25I), C33C(H33J,H33K,H33L), C34C(H34J,H34K,H34L),
 C35C(H35J,H35K,H35L), C38C(H38J,H38K,H38L), C39C(H39J,H39K,H39L), C40C(H40J,
 H40K,H40L), C43C(H43J,H43K,H43L), C44C(H44J,H44K,H44L), C45C(H45J,H45K,H45L),
 C48C(H48J,H48K,H48L), C49C(H49J,H49K,H49L), C50C(H50J,H50K,H50L), C53C(H53G,
 H53H,H53I), C54C(H54G,H54H,H54I), C55C(H55G,H55H,H55I), C58C(H58J,H58K,H58L),
 C59C(H59J,H59K,H59L), C60C(H60J,H60K,H60L)
8.d Idealised Me refined as rotating group:
 C2F(H2FA,H2FB,H2FC), C4F(H4FA,H4FB,H4FC), C6F(H6FA,H6FB,H6FC), C8F(H8FA,H8FB,
 H8FC)
;
_shelx_res_checksum              85450
_olex2_date_sample_data_collection 2016-01-30
_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 1.274
_oxdiff_exptl_absorpt_empirical_full_min 0.759