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_7046047
_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_absolute_configuration ad
_chemical_formula_moiety
'C82 H150 Cr6 F8 O35 S U2, C6 H16 N, 2(C7 H8)'
_chemical_formula_sum            'C102 H182 Cr6 F8 N O35 S U2'
_chemical_formula_weight         2954.60
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-12-21
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-12-22 deposited with the CCDC.
2018-03-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   33.1772(7)
_cell_length_b                   32.7339(8)
_cell_length_c                   13.1235(3)
_cell_measurement_reflns_used    9857
_cell_measurement_temperature    150.00(2)
_cell_measurement_theta_max      67.569
_cell_measurement_theta_min      2.693
_cell_volume                     14252.4(6)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_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  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.00(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1236
_diffrn_reflns_av_unetI/netI     0.1132
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            105200
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.692
_diffrn_reflns_theta_min         1.331
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.689
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.4009
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.1310 before and 0.0870 after correction. The Ratio of minimum to maximum transmission is 0.5320. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_description       block
_exptl_crystal_F_000             5988
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.645
_refine_diff_density_min         -2.696
_refine_diff_density_rms         0.181
_refine_ls_abs_structure_details
;
 Flack x determined using 6108 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.002(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1557
_refine_ls_number_reflns         25941
_refine_ls_number_restraints     4230
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.1202
_refine_ls_R_factor_gt           0.0876
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1530P)^2^+23.3800P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2226
_refine_ls_wR_factor_ref         0.2549
_reflns_Friedel_coverage         0.846
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.975
_reflns_number_gt                18855
_reflns_number_total             25941
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00803e2.cif
_cod_data_source_block           xrepw772
_cod_depositor_comments
'Adding full bibliography for 7046044--7046048.cif.'
_cod_database_code               7046047
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.8339(16)
 0.1661(16)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C4X-C3X
 2.9 with sigma of 0.02
 C3X-C4X = C8X-C7X
 2.665 with sigma of 0.02
 C8X-O5X = C3X-O1X = C4X-O1X = C7X-O5X
 2.608 with sigma of 0.02
 S2X-C3X = S2X-C4X = S6X-C8X = S6X-C7X
 1.761 with sigma of 0.02
 S6X-O5X = S2X-O1X
 1.504 with sigma of 0.02
 C70-C67 = C69-C67 = C67-C68
 1.54 with sigma of 0.02
 N4C-C5C = N4B-C5B = N4C-C3C = N4B-C3B
 1.45 with sigma of 0.02
 C2B-C3B = C2C-C3C = C2C-C1C = C2B-C1B = C7C-C6C = C6C-C5C = C6B-C5B = C7B-C6B
 1.54 with sigma of 0.02
 C1C-C3C = C3B-C1B = C5C-C3C = C3B-C5B = C7B-C5B = C7C-C5C
 2.35 with sigma of 0.02
 C6AA-C3AA
 1.54 with sigma of 0.02
 C7D-C1D
 1.54 with sigma of 0.02
 S6X-C7X \\sim S6X-C8X \\sim S2X-C3X \\sim S2X-C4X
 with sigma of 0.02
 U2-F7 \\sim U1-F6
 with sigma of 0.02
 U1-O1X \\sim U2-O5X
 with sigma of 0.02
 C6D-C7D \\sim C7D-C2D
 with sigma of 0.02
 C55A-C52 \\sim C55-C52 \\sim C53A-C52 \\sim C53-C52 \\sim C54A-C52 \\sim
C54-C52
 with sigma of 0.02
 C7AA-C3AA \\sim C3AA-C8AA
 with sigma of 0.02
 O9-C21 \\sim O9-C21A \\sim O10-C21A \\sim O10-C21
 with sigma of 0.02
4. Restrained planarity
 C6AA, C1BA, C0BA, C7AA, C9AA, C8AA, C3AA
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
S6X \\sim C7X \\sim C8X: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
S2X \\sim C3X \\sim C4X: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C66 \\sim C67 \\sim C70 \\sim C68 \\sim C69: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
N4C \\sim C1C \\sim C2C \\sim C3C \\sim C5C \\sim C6C \\sim C7C \\sim N4B \\sim
C5B \\sim C3B \\sim C6B \\sim C2B \\sim C7B \\sim C1B: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
F7 \\sim O5X \\sim S6X \\sim C7X \\sim C8X \\sim C3X \\sim S2X \\sim C4X \\sim
O1X \\sim F6: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C6AA \\sim C8AA \\sim C7AA \\sim C3AA \\sim C9AA \\sim C1BA \\sim C0BA: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C53 \\sim C52 \\sim C54A \\sim C54 \\sim C55A \\sim C55 \\sim C53A: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C66) \\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(C70) \\sim Ueq, Uanis(C68)
\\sim Ueq, Uanis(C69) \\sim Ueq: with sigma of 0.02 and sigma for terminal
atoms of 0.04
Uanis(C4X) \\sim Ueq, Uanis(C7X) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(F35) \\sim Ueq, Uanis(O28) \\sim Ueq, Uanis(F34) \\sim Ueq: with sigma of
0.02 and sigma for terminal atoms of 0.04
Uanis(C1D) \\sim Ueq, Uanis(C6D) \\sim Ueq, Uanis(C2D) \\sim Ueq, Uanis(C7D)
\\sim Ueq, Uanis(C5D) \\sim Ueq, Uanis(C3D) \\sim Ueq, Uanis(C4D) \\sim Ueq:
with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C7C) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
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. Same fragment restrains
{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
{C22, C23, C24, C25}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as
{C27, C28, C29, C30}
{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
{C52, C53, C54, C55}
{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
{C62, C63, C64, C65}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as
{C72, C73, C74, C75}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as
{C77, C78, C79, C80}
{C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as
{C67, C68, C69, C70}
{C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as
{C53A, C54A, C55A}
{C1, C2, C3, C4, C5} sigma for 1-2: 0.02, 1-3: 0.04
as
{C21A, C22A, C23A, C24A, C25A}
8. Others
 Sof(F7)=Sof(S2X)=Sof(O1X)=Sof(C3X)=Sof(H3XA)=Sof(H3XB)=Sof(H3XC)=Sof(C4X)=
 Sof(H4XA)=Sof(H4XB)=Sof(H4XC)=1-FVAR(1)
 Sof(F6)=Sof(S6X)=Sof(O5X)=Sof(C7X)=Sof(H7XA)=Sof(H7XB)=Sof(H7XC)=Sof(C8X)=
 Sof(H8XA)=Sof(H8XB)=Sof(H8XC)=FVAR(1)
 Sof(C1C)=Sof(H1CA)=Sof(H1CB)=Sof(H1CC)=Sof(C2C)=Sof(H2CA)=Sof(H2CB)=Sof(C3C)=
 Sof(H3CA)=Sof(H3CB)=Sof(N4C)=Sof(H4CA)=Sof(H4CB)=Sof(C5C)=Sof(H5CA)=Sof(H5CB)=
 Sof(C6C)=Sof(H6CA)=Sof(H6CB)=Sof(C7C)=Sof(H7CA)=Sof(H7CB)=Sof(H7CC)=1-FVAR(2)
 Sof(N4B)=Sof(H4BA)=Sof(H4BB)=Sof(C5B)=Sof(H5BA)=Sof(H5BB)=Sof(C1B)=Sof(H1BA)=
 Sof(H1BB)=Sof(H1BC)=Sof(C6B)=Sof(H6BA)=Sof(H6BB)=Sof(C7B)=Sof(H7BA)=Sof(H7BB)=
 Sof(H7BC)=Sof(C2B)=Sof(H2BA)=Sof(H2BB)=Sof(C3B)=Sof(H3BA)=Sof(H3BB)=FVAR(2)
 Sof(C53A)=Sof(H53D)=Sof(H53E)=Sof(H53F)=Sof(C54A)=Sof(H54D)=Sof(H54E)=
 Sof(H54F)=Sof(C55A)=Sof(H55D)=Sof(H55E)=Sof(H55F)=1-FVAR(3)
 Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(H53C)=Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(H54C)=
 Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(H55C)=FVAR(3)
 Sof(C21A)=Sof(C22A)=Sof(C23A)=Sof(H23D)=Sof(H23E)=Sof(H23F)=Sof(C24A)=
 Sof(H24D)=Sof(H24E)=Sof(H24F)=Sof(C25A)=Sof(H25D)=Sof(H25E)=Sof(H25F)=1-FVAR(4)
 Sof(C21)=Sof(C22)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C24)=Sof(H24A)=
 Sof(H24B)=Sof(H24C)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=FVAR(4)
9.a Secondary CH2 refined with riding coordinates:
 N4B(H4BA,H4BB), C5B(H5BA,H5BB), C6B(H6BA,H6BB), C2B(H2BA,H2BB), C3B(H3BA,
 H3BB), C2C(H2CA,H2CB), C3C(H3CA,H3CB), N4C(H4CA,H4CB), C5C(H5CA,H5CB),
 C6C(H6CA,H6CB)
9.b 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), C73(H73A,H73B,H73C), C74(H74A,H74B,H74C),
 C75(H75A,H75B,H75C), C78(H78A,H78B,H78C), C79(H79A,H79B,H79C), C80(H80A,H80B,
 H80C), C68(H68A,H68B,H68C), C69(H69A,H69B,H69C), C70(H70A,H70B,H70C), C7X(H7XA,
 H7XB,H7XC), C8X(H8XA,H8XB,H8XC), C3X(H3XA,H3XB,H3XC), C4X(H4XA,H4XB,H4XC),
 C1B(H1BA,H1BB,H1BC), C7B(H7BA,H7BB,H7BC), C7D(H7DA,H7DB,H7DC), C1C(H1CA,H1CB,
 H1CC), C7C(H7CA,H7CB,H7CC), C53A(H53D,H53E,H53F), C54A(H54D,H54E,H54F),
 C55A(H55D,H55E,H55F), C3AA(H3AA,H3AB,H3AC), C23A(H23D,H23E,H23F), C24A(H24D,
 H24E,H24F), C25A(H25D,H25E,H25F)
9.c Aromatic/amide H refined with riding coordinates:
 C6D(H6D), C5D(H5D), C4D(H4D), C3D(H3D), C2D(H2D), C8AA(H8AA), C9AA(H9AA),
 C0BA(H0BA), C1BA(H1BD), C7AA(H7AA)
9.d Fitted hexagon refined as free rotating group:
 C1D(C6D,C5D,C4D,C3D,C2D), C6AA(C8AA,C9AA,C0BA,C1BA,C7AA)
;
_shelx_res_checksum              89447
_shelx_fab_checksum              16503
_olex2_submission_special_instructions 'No special instructions were received'