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_7046044
_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
'C80 H144 Cr7 F6 O34 Ti, C6 H16 N, C2 H5 O0.5'
_chemical_formula_sum            'C88 H165 Cr7 F6 N O34.5 Ti'
_chemical_formula_weight         2315.10
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-10-11
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2017-12-22 deposited with the CCDC.
2018-03-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.847(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.3319(14)
_cell_length_b                   16.6836(8)
_cell_length_c                   31.1000(14)
_cell_measurement_reflns_used    11526
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.9190
_cell_measurement_theta_min      3.6010
_cell_volume                     12950.1(11)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1636
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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    -77.00   7.00   1.00   15.00    --   -9.59 -57.00 -60.00   84
  2  \w    -31.00  52.00   1.00   15.00    --   -9.59  77.00-120.00   83
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0185477000
_diffrn_orient_matrix_UB_12      -0.0001317000
_diffrn_orient_matrix_UB_13      -0.0198731000
_diffrn_orient_matrix_UB_21      0.0215322000
_diffrn_orient_matrix_UB_22      -0.0001671000
_diffrn_orient_matrix_UB_23      -0.0118684000
_diffrn_orient_matrix_UB_31      0.0000073000
_diffrn_orient_matrix_UB_32      -0.0425208000
_diffrn_orient_matrix_UB_33      0.0001373000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0591
_diffrn_reflns_av_unetI/netI     0.1017
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            61269
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.442
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.695
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85181
_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 dark green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_description       needle
_exptl_crystal_F_000             4880
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.739
_refine_diff_density_min         -1.165
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1280
_refine_ls_number_reflns         26204
_refine_ls_number_restraints     2263
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1757
_refine_ls_R_factor_gt           0.0960
_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^)+(0.1689P)^2^+25.2856P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2603
_refine_ls_wR_factor_ref         0.3268
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13765
_reflns_number_total             26204
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00803e2.cif
_cod_data_source_block           orepw1860
_cod_depositor_comments
'Adding full bibliography for 7046044--7046048.cif.'
_cod_original_cell_volume        12950.0(11)
_cod_original_formula_sum        'C88 H165 Cr7 F6 N O34.50 Ti'
_cod_database_code               7046044
_shelxl_version_number           2014/6
_reflns_odcompleteness_completeness 98.75
_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 C(H,H,H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Shared sites
{Ti1, Cr1}
{Cr8, Ti8}
{Ti7, Cr7}
{Cr6, Ti6}
{Cr5, Ti5}
{Ti4, Cr4}
{Cr3, Ti3}
{Cr2, Ti2}
3. Restrained distances
 C86-C84
 2.4 with sigma of 0.02
 C84-C85
 2.4 with sigma of 0.02
 C85-C86
 2.4 with sigma of 0.02
 C113-C112
 2.4 with sigma of 0.02
 C113-C114
 2.4 with sigma of 0.02
 C114-C112
 2.4 with sigma of 0.02
 C42-C44
 2.4 with sigma of 0.02
 C42-C43
 2.4 with sigma of 0.02
 C43-C44
 2.4 with sigma of 0.02
 O1S-C3S
 2.4 with sigma of 0.02
 O1S-C2S
 1.45 with sigma of 0.02
 C3S-C2S
 1.54 with sigma of 0.02
 C2S-C2S_$1
 2.4 with sigma of 0.002
 O1S-C2S = O1S-C2S_$1
 1.45 with sigma of 0.002
 N1T-C7T \\sim N2T-C7T \\sim N2T-C3T \\sim N1T-C3T
 with sigma of 0.001
 C6T-C5T \\sim C6T-C4T \\sim C5T-C3T \\sim C4T-C3T \\sim C7T-C9T \\sim O81-C82
\\sim C10T-C8T \\sim C10T-C9T
 with sigma of 0.001
 C86-C83 \\sim C83-C85 \\sim C84-C83
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C4T \\sim C5T: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
N2T \\sim N1T: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
C9T \\sim C8T: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
F7 \\sim O7 \\sim F8 \\sim O8 \\sim F1 \\sim O1 \\sim F2 \\sim O2 \\sim F3
\\sim O3 \\sim F4 \\sim O4 \\sim F5 \\sim O5 \\sim F6 \\sim O6: within 2A with
sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(F2) = Uanis(O2)
Uanis(F3) = Uanis(O3)
Uanis(F4) = Uanis(O4)
Uanis(O5) = Uanis(F5)
Uanis(O6) = Uanis(F6)
Uanis(F8) = Uanis(O8)
Uanis(Ti8) = Uanis(Cr8)
Uanis(Ti2) = Uanis(Cr2)
Uanis(Cr4) = Uanis(Ti4)
Uanis(Cr7) = Uanis(Ti7)
Uanis(Ti1) = Uanis(Cr1)
Uanis(Cr6) = Uanis(Ti6)
Uanis(Cr5) = Uanis(Ti5)
Uanis(Cr3) = Uanis(Ti3)
Uanis(F1) = Uanis(O1)
Uanis(O7) = Uanis(F7)
5. 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
6. Others
 Sof(H3TC)=Sof(H3TD)=Sof(H7TC)=Sof(H7TD)=Sof(H6TD)=Sof(H6TE)=Sof(H6TF)=
 Sof(H10P)=Sof(H10Q)=Sof(H10R)=Sof(C5T)=Sof(H5TA)=Sof(H5TB)=Sof(N2T)=Sof(H2TA)=
 Sof(H2TB)=Sof(C9T)=Sof(H9TA)=Sof(H9TB)=1-FVAR(1)
 Sof(H3TA)=Sof(H3TB)=Sof(H7TA)=Sof(H7TB)=Sof(H6TA)=Sof(H6TB)=Sof(H6TC)=
 Sof(N1T)=Sof(H1TA)=Sof(H1TB)=Sof(H10M)=Sof(H10N)=Sof(H10O)=Sof(C8T)=Sof(H8TA)=
 Sof(H8TB)=Sof(C4T)=Sof(H4TA)=Sof(H4TB)=FVAR(1)
 Fixed Sof: Cr4(0.875) Cr2(0.875) Cr3(0.875) Cr6(0.875) Cr5(0.875) Cr8(0.875)
 Cr7(0.875) Cr1(0.875) F2(0.75) F3(0.75) F4(0.75) F7(0.75) F6(0.75) F5(0.75)
 F1(0.75) F8(0.75) O1S(0.5) Ti5(0.125) Ti4(0.125) Ti3(0.125) Ti2(0.125)
 Ti1(0.125) Ti8(0.125) Ti7(0.125) Ti6(0.125) O5(0.25) O4(0.25) O3(0.25)
 O2(0.25) O1(0.25) O8(0.25) O7(0.25) O6(0.25)
7.a Secondary CH2 refined with riding coordinates:
 C3T(H3TA,H3TB), C3T(H3TC,H3TD), C7T(H7TA,H7TB), C7T(H7TC,H7TD), N1T(H1TA,
 H1TB), C8T(H8TA,H8TB), C4T(H4TA,H4TB), C2S(H2SA,H2SB), C5T(H5TA,H5TB),
 N2T(H2TA,H2TB), C9T(H9TA,H9TB)
7.b Me refined with riding coordinates:
 C51(H51A,H51B,H51C), C15(H15A,H15B,H15C), C30(H30A,H30B,H30C), C6T(H6TA,H6TB,
 H6TC), C6T(H6TD,H6TE,H6TF), C72(H72A,H72B,H72C), C106(H10A,H10B,H10C),
 C114(H11A,H11B,H11C), C71(H71A,H71B,H71C), C65(H65A,H65B,H65C), C57(H57A,H57B,
 H57C), C64(H64A,H64B,H64C), C70(H70A,H70B,H70C), C63(H63A,H63B,H63C), C56(H56A,
 H56B,H56C), C105(H10D,H10E,H10F), C29(H29A,H29B,H29C), C98(H98A,H98B,H98C),
 C16(H16A,H16B,H16C), C119(H11D,H11E,H11F), C22(H22A,H22B,H22C), C100(H10G,H10H,
 H10I), C107(H10J,H10K,H10L), C35(H35A,H35B,H35C), C21(H21A,H21B,H21C),
 C58(H58A,H58B,H58C), C28(H28A,H28B,H28C), C42(H42A,H42B,H42C), C37(H37A,H37B,
 H37C), C92(H92A,H92B,H92C), C99(H99A,H99B,H99C), C49(H49A,H49B,H49C), C36(H36A,
 H36B,H36C), C14(H14A,H14B,H14C), C121(H12A,H12B,H12C), C23(H23A,H23B,H23C),
 C10T(H10M,H10N,H10O), C10T(H10P,H10Q,H10R), C93(H93A,H93B,H93C), C44(H44A,H44B,
 H44C), C120(H12D,H12E,H12F), C79(H79A,H79B,H79C), C84(H84A,H84B,H84C),
 C113(H11G,H11H,H11I), C78(H78A,H78B,H78C), C85(H85A,H85B,H85C), C91(H91A,H91B,
 H91C), C77(H77A,H77B,H77C), C50(H50A,H50B,H50C), C86(H86A,H86B,H86C),
 C112(H11J,H11K,H11L), C43(H43A,H43B,H43C), C3S(H3SA,H3SB,H3SC)
;
_shelx_res_checksum              30590
_olex2_date_sample_data_collection 2015-12-11
_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 1.221
_oxdiff_exptl_absorpt_empirical_full_min 0.778