Binding of halogens by a Cr<sub>8</sub> metallacrown.
Sava, Daniel Florin; Zheng, Nan; Vitórica-Yrezábal, Iñigo J; Timco, Grigore A.; Winpenny, Richard E. P.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 13771–13775; doi:10.1039/c8dt03172j

data_7047610
_publ_section_title
;
 Binding of halogens by a Cr<sub>8</sub> metallacrown.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13771
_journal_page_last               13775
_journal_paper_doi               10.1039/c8dt03172j
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C80 H144 Cr8 F8 O32, 0.37(I2)'
_chemical_formula_sum            'C80 H144 Cr8 F8 I0.74 O32'
_chemical_formula_weight         2279.53
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-05-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.18 svn.r3508 for OlexSys, GUI svn.r5497)
;
_audit_update_record
;
2018-08-02 deposited with the CCDC.
2018-09-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.347(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   44.5160(14)
_cell_length_b                   16.5380(3)
_cell_length_c                   34.6653(9)
_cell_measurement_reflns_used    24525
_cell_measurement_temperature    200.0
_cell_measurement_theta_max      26.8860
_cell_measurement_theta_min      1.9650
_cell_volume                     23769.9(12)
_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)'
_diffrn_ambient_temperature      200.0
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_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    -70.00  33.00   1.00    6.00    --   19.40  43.00  30.00  103
  2  \w    -34.00 106.00   1.00    6.00    --   19.40  29.00  90.00  140
  3  \w    -46.00 -21.00   1.00    6.00    --   19.40  60.00 -60.00   25
  4  \w      9.00 109.00   1.00    6.00    --   19.40  14.00 -30.00  100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0105606000
_diffrn_orient_matrix_UB_12      -0.0324933000
_diffrn_orient_matrix_UB_13      -0.0093347000
_diffrn_orient_matrix_UB_21      -0.0122806000
_diffrn_orient_matrix_UB_22      0.0184262000
_diffrn_orient_matrix_UB_23      0.0054758000
_diffrn_orient_matrix_UB_31      -0.0055137000
_diffrn_orient_matrix_UB_32      0.0210563000
_diffrn_orient_matrix_UB_33      -0.0191144000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_unetI/netI     0.0393
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       56
_diffrn_reflns_limit_h_min       -52
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            74339
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.732
_diffrn_reflns_theta_min         1.860
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.969
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57400
_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 dark green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_description       block
_exptl_crystal_F_000             9465
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.032
_refine_diff_density_min         -0.969
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1462
_refine_ls_number_reflns         25138
_refine_ls_number_restraints     1332
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0819
_refine_ls_R_factor_gt           0.0599
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0755P)^2^+86.6004P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1537
_refine_ls_wR_factor_ref         0.1644
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18944
_reflns_number_total             25138
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03172j2.cif
_cod_data_source_block           vt_2_200_00_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7047602--7047620.cif.'
_cod_database_code               7047610
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         Cr8F8O32C80H144I
_reflns_odcompleteness_completeness 89.41
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.71
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C10-C16 = C10-C15 = C10-C14 = C13-C10 = C12-C10 = C10-C11
 1.54 with sigma of 0.02
 C65-C63 \\sim C65-C61 \\sim C63-C61 \\sim C62-C64 \\sim C62-C60 \\sim C64-C60
 with sigma of 0.004
 C59-C58 \\sim C59-C65 \\sim C59-C63 \\sim C59-C61 \\sim C59-C62 \\sim C59-C64
\\sim C59-C60
 with sigma of 0.002
 C96-C94 \\sim C96-C92 \\sim C94-C92 \\sim C95-C97 \\sim C95-C93 \\sim C97-C93
 with sigma of 0.004
 C91-C90 \\sim C91-C96 \\sim C91-C94 \\sim C91-C92 \\sim C91-C95 \\sim C91-C97
\\sim C91-C93
 with sigma of 0.002
 C42-C40 \\sim C42-C44 \\sim C40-C44 \\sim C39-C41 \\sim C39-C43 \\sim C41-C43
 with sigma of 0.004
 C38-C37 \\sim C38-C42 \\sim C38-C40 \\sim C38-C44 \\sim C38-C39 \\sim C38-C41
\\sim C38-C43
 with sigma of 0.002
 C70-C72 \\sim C70-C68 \\sim C72-C68 \\sim C69-C71 \\sim C69-C73 \\sim C71-C73
 with sigma of 0.004
 C67-C66 \\sim C67-C70 \\sim C67-C72 \\sim C67-C68 \\sim C67-C69 \\sim C67-C71
\\sim C67-C73
 with sigma of 0.002
 C88-C86 \\sim C88-C84 \\sim C86-C84 \\sim C89-C85 \\sim C89-C87 \\sim C85-C87
 with sigma of 0.004
 C83-C82 \\sim C83-C88 \\sim C83-C86 \\sim C83-C84 \\sim C83-C89 \\sim C83-C85
\\sim C83-C87
 with sigma of 0.002
 C7-C5 \\sim C7-C3 \\sim C5-C3 \\sim C8-C4 \\sim C8-C6 \\sim C4-C6
 with sigma of 0.004
 C2-C1 \\sim C2-C7 \\sim C2-C5 \\sim C2-C3 \\sim C2-C8 \\sim C2-C4 \\sim C2-C6
 with sigma of 0.002
 C79-C77 \\sim C79-C81 \\sim C77-C81 \\sim C80-C76 \\sim C80-C78 \\sim C76-C78
 with sigma of 0.004
 C75-C74 \\sim C75-C79 \\sim C75-C77 \\sim C75-C81 \\sim C75-C80 \\sim C75-C76
\\sim C75-C78
 with sigma of 0.002
 C54-C52 \\sim C54-C56 \\sim C52-C56 \\sim C57-C53 \\sim C57-C55 \\sim C53-C55
 with sigma of 0.004
 C51-C50 \\sim C51-C54 \\sim C51-C52 \\sim C51-C56 \\sim C51-C57 \\sim C51-C53
\\sim C51-C55
 with sigma of 0.002
 C12-C16 \\sim C12-C14 \\sim C16-C14 \\sim C15-C11 \\sim C15-C13 \\sim C11-C13
 with sigma of 0.004
 C10-C9 \\sim C10-C12 \\sim C10-C16 \\sim C10-C14 \\sim C10-C15 \\sim C10-C11
\\sim C10-C13
 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
C33 \\sim C34 \\sim C35 \\sim C36: within 2A with sigma of 0.002 and sigma for
terminal atoms of 0.004
C28 \\sim C29 \\sim C30 \\sim C31: within 2A with sigma of 0.002 and sigma for
terminal atoms of 0.004
C77 \\sim C78 \\sim C79 \\sim C80 \\sim C81 \\sim C76 \\sim C75: within 2A with
sigma of 0.002 and sigma for terminal atoms of 0.004
C25 \\sim C23 \\sim C26 \\sim C24: within 2A with sigma of 0.002 and sigma for
terminal atoms of 0.004
C7 \\sim C8 \\sim C6 \\sim C5 \\sim C4 \\sim C3 \\sim C2: within 2A with sigma
of 0.002 and sigma for terminal atoms of 0.004
C88 \\sim C89 \\sim C83 \\sim C85 \\sim C84 \\sim C86 \\sim C87: within 2A with
sigma of 0.002 and sigma for terminal atoms of 0.004
C73 \\sim C72 \\sim C71 \\sim C70 \\sim C69 \\sim C68 \\sim C67: within 2A with
sigma of 0.002 and sigma for terminal atoms of 0.004
C55 \\sim C54 \\sim C51 \\sim C56 \\sim C57 \\sim C52 \\sim C53: within 2A with
sigma of 0.002 and sigma for terminal atoms of 0.004
C41 \\sim C42 \\sim C43 \\sim C44 \\sim C39 \\sim C40 \\sim C38: within 2A with
sigma of 0.002 and sigma for terminal atoms of 0.004
C14 \\sim C13 \\sim C10 \\sim C15 \\sim C16 \\sim C11 \\sim C12: within 2A with
sigma of 0.002 and sigma for terminal atoms of 0.004
C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C59 \\sim C65: within 2A with
sigma of 0.002 and sigma for terminal atoms of 0.004
C94 \\sim C93 \\sim C92 \\sim C91 \\sim C97 \\sim C96 \\sim C95: within 2A with
sigma of 0.002 and sigma for terminal atoms of 0.004
C49 \\sim C48 \\sim C46 \\sim C47: within 2A with sigma of 0.002 and sigma for
terminal atoms of 0.004
4. Rigid body (RIGU) restrains
 C59, C61, C63, C65, C60, C62, C64
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C91, C92, C94, C96, C93, C95, C97
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C38, C40, C42, C44, C39, C41, C43
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C67, C68, C70, C72, C69, C71, C73
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C83, C84, C86, C88, C85, C87, C89
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C2, C3, C5, C7, C4, C6, C8
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C75, C77, C79, C81, C76, C78, C80
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C51, C52, C54, C56, C53, C55, C57
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C10, C12, C14, C16, C11, C13, C15
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(I1)=Sof(I2)=FVAR(1)
 Sof(I3)=Sof(I4)=FVAR(2)
 Sof(I5)=Sof(I6)=FVAR(3)
 Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=
 Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=1-FVAR(4)
 Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=
 Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=FVAR(4)
 Sof(C60)=Sof(H60A)=Sof(H60B)=Sof(H60C)=Sof(C62)=Sof(H62A)=Sof(H62B)=Sof(H62C)=
 Sof(C64)=Sof(H64A)=Sof(H64B)=Sof(H64C)=1-FVAR(5)
 Sof(C61)=Sof(H61A)=Sof(H61B)=Sof(H61C)=Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(H63C)=
 Sof(C65)=Sof(H65A)=Sof(H65B)=Sof(H65C)=FVAR(5)
 Sof(C93)=Sof(H93A)=Sof(H93B)=Sof(H93C)=Sof(C95)=Sof(H95A)=Sof(H95B)=Sof(H95C)=
 Sof(C97)=Sof(H97A)=Sof(H97B)=Sof(H97C)=1-FVAR(6)
 Sof(C92)=Sof(H92A)=Sof(H92B)=Sof(H92C)=Sof(C94)=Sof(H94A)=Sof(H94B)=Sof(H94C)=
 Sof(C96)=Sof(H96A)=Sof(H96B)=Sof(H96C)=FVAR(6)
 Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=
 Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(H43C)=1-FVAR(7)
 Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(H42C)=
 Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(H44C)=FVAR(7)
 Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(H53C)=Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(H55C)=
 Sof(C57)=Sof(H57A)=Sof(H57B)=Sof(H57C)=1-FVAR(8)
 Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(H52C)=Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(H54C)=
 Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(H56C)=FVAR(8)
 Sof(C69)=Sof(H69A)=Sof(H69B)=Sof(H69C)=Sof(C71)=Sof(H71A)=Sof(H71B)=Sof(H71C)=
 Sof(C73)=Sof(H73A)=Sof(H73B)=Sof(H73C)=1-FVAR(9)
 Sof(C68)=Sof(H68A)=Sof(H68B)=Sof(H68C)=Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(H70C)=
 Sof(C72)=Sof(H72A)=Sof(H72B)=Sof(H72C)=FVAR(9)
 Sof(C85)=Sof(H85A)=Sof(H85B)=Sof(H85C)=Sof(C87)=Sof(H87A)=Sof(H87B)=Sof(H87C)=
 Sof(C89)=Sof(H89A)=Sof(H89B)=Sof(H89C)=1-FVAR(10)
 Sof(C84)=Sof(H84A)=Sof(H84B)=Sof(H84C)=Sof(C86)=Sof(H86A)=Sof(H86B)=Sof(H86C)=
 Sof(C88)=Sof(H88A)=Sof(H88B)=Sof(H88C)=FVAR(10)
 Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=Sof(C8)=
 Sof(H8A)=Sof(H8B)=Sof(H8C)=1-FVAR(11)
 Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=Sof(C7)=
 Sof(H7A)=Sof(H7B)=Sof(H7C)=FVAR(11)
 Sof(C76)=Sof(H76A)=Sof(H76B)=Sof(H76C)=Sof(C78)=Sof(H78A)=Sof(H78B)=Sof(H78C)=
 Sof(C80)=Sof(H80A)=Sof(H80B)=Sof(H80C)=1-FVAR(12)
 Sof(C77)=Sof(H77A)=Sof(H77B)=Sof(H77C)=Sof(C79)=Sof(H79A)=Sof(H79B)=Sof(H79C)=
 Sof(C81)=Sof(H81A)=Sof(H81B)=Sof(H81C)=FVAR(12)
6.a Me refined with riding coordinates:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C29(H29A,H29B,H29C), C30(H30A,
 H30B,H30C), C31(H31A,H31B,H31C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C),
 C36(H36A,H36B,H36C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C49(H49A,H49B,
 H49C), C100(H10A,H10B,H10C), C101(H10D,H10E,H10F), C102(H10G,H10H,H10I),
 C105(H10J,H10K,H10L), C106(H10M,H10N,H10O), C107(H10P,H10Q,H10R), C3(H3A,H3B,
 H3C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C12(H12A,H12B,H12C), C14(H14A,H14B,
 H14C), C16(H16A,H16B,H16C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C44(H44A,
 H44B,H44C), C52(H52A,H52B,H52C), C54(H54A,H54B,H54C), C56(H56A,H56B,H56C),
 C61(H61A,H61B,H61C), C63(H63A,H63B,H63C), C65(H65A,H65B,H65C), C68(H68A,H68B,
 H68C), C70(H70A,H70B,H70C), C72(H72A,H72B,H72C), C77(H77A,H77B,H77C), C79(H79A,
 H79B,H79C), C81(H81A,H81B,H81C), C84(H84A,H84B,H84C), C86(H86A,H86B,H86C),
 C88(H88A,H88B,H88C), C92(H92A,H92B,H92C), C94(H94A,H94B,H94C), C96(H96A,H96B,
 H96C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C11(H11A,H11B,H11C),
 C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C39(H39A,H39B,H39C), C41(H41A,H41B,
 H41C), C43(H43A,H43B,H43C), C53(H53A,H53B,H53C), C55(H55A,H55B,H55C), C57(H57A,
 H57B,H57C), C60(H60A,H60B,H60C), C62(H62A,H62B,H62C), C64(H64A,H64B,H64C),
 C69(H69A,H69B,H69C), C71(H71A,H71B,H71C), C73(H73A,H73B,H73C), C76(H76A,H76B,
 H76C), C78(H78A,H78B,H78C), C80(H80A,H80B,H80C), C85(H85A,H85B,H85C), C87(H87A,
 H87B,H87C), C89(H89A,H89B,H89C), C93(H93A,H93B,H93C), C95(H95A,H95B,H95C),
 C97(H97A,H97B,H97C)
;
_shelx_res_checksum              49612
_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 1.305
_oxdiff_exptl_absorpt_empirical_full_min 0.395