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_7047603
_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, 0.8(Br2)'
_chemical_formula_sum            'C80 H144 Br1.6 Cr8 F8 O32'
_chemical_formula_weight         2314.00
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2018-02-21
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-08-02 deposited with the CCDC.
2018-09-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.369(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   44.1693(11)
_cell_length_b                   16.5140(3)
_cell_length_c                   34.8521(10)
_cell_measurement_reflns_used    18225
_cell_measurement_temperature    150.02(11)
_cell_measurement_theta_max      25.5390
_cell_measurement_theta_min      3.3840
_cell_volume                     23673.9(11)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41q (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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.02(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -81.00  17.25   0.75   20.00    --  -22.82  19.00-120.00  131
  2  \w   -110.00 -35.00   0.75   20.00    --  -22.82 178.00  30.00  100
  3  \w    -17.00  10.00   0.75   20.00    --  -22.82 -99.00  30.00   36
  4  \w     -8.00  22.00   0.75   20.00    --  -22.82 -99.00-150.00   40
  5  \w     -6.00  96.00   0.75   20.00    --   23.91  57.00  60.00  136
  6  \w     36.00 100.50   0.75   20.00    --   23.91 178.00 -30.00   86
  7  \w    -42.00  42.00   0.75   20.00    --   23.91 -57.00 -90.00  112
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0026022000
_diffrn_orient_matrix_UB_12      0.0165212000
_diffrn_orient_matrix_UB_13      -0.0197297000
_diffrn_orient_matrix_UB_21      0.0097839000
_diffrn_orient_matrix_UB_22      -0.0309592000
_diffrn_orient_matrix_UB_23      -0.0036076000
_diffrn_orient_matrix_UB_31      -0.0139551000
_diffrn_orient_matrix_UB_32      -0.0247774000
_diffrn_orient_matrix_UB_33      -0.0086650000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0579
_diffrn_reflns_av_unetI/netI     0.0564
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       53
_diffrn_reflns_limit_h_min       -53
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            83715
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         3.281
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.322
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52037
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41q (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    1.298
_exptl_crystal_description       block
_exptl_crystal_F_000             9601
_exptl_crystal_recrystallization_method
'The material was recrystallised from 1-bromodecane by slow cooling'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.752
_refine_diff_density_min         -0.449
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1425
_refine_ls_number_reflns         21611
_refine_ls_number_restraints     612
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0472
_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^)+(0.0464P)^2^+51.6718P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1054
_refine_ls_wR_factor_ref         0.1194
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15651
_reflns_number_total             21611
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03172j2.cif
_cod_data_source_block           arepw1281
_cod_depositor_comments
'Adding full bibliography for 7047602--7047620.cif.'
_cod_original_formula_sum        'C80 H144 Br1.60 Cr8 F8 O32'
_cod_database_code               7047603
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         Cr8F8O32C80H144Br2
_chemical_oxdiff_usercomment     'Cr8 + Br2'
_reflns_odcompleteness_completeness 89.40
_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
2. Restrained distances
 C42-C41 = C44-C41 = C46-C41
 1.54 with sigma of 0.02
 C67-C65 \\sim C67-C63 \\sim C65-C63 \\sim C64-C66
 with sigma of 0.04
 C62-C61 \\sim C62-C67 \\sim C62-C65 \\sim C62-C63 \\sim C62-C64 \\sim C62-C68
\\sim C62-C66
 with sigma of 0.02
 C73-C71 \\sim C73-C75 \\sim C71-C75
 with sigma of 0.04
 C70-C69 \\sim C70-C73 \\sim C70-C71 \\sim C70-C75 \\sim C70-C74 \\sim C70-C72
\\sim C70-C76
 with sigma of 0.02
 C13-C15 \\sim C13-C11 \\sim C15-C11 \\sim C12-C16 \\sim C12-C14 \\sim C16-C14
 with sigma of 0.04
 C10-C9 \\sim C10-C13 \\sim C10-C15 \\sim C10-C11 \\sim C10-C12 \\sim C10-C16
\\sim C10-C14
 with sigma of 0.02
 C40-C47 \\sim C40-C43 \\sim C40-C45 \\sim C47-C43 \\sim C47-C45 \\sim C43-C45
 with sigma of 0.04
 C41-C40 \\sim C41-C47 \\sim C41-C43 \\sim C41-C45
 with sigma of 0.02
 C48-C54 \\sim C48-C52 \\sim C48-C50 \\sim C54-C52 \\sim C54-C50 \\sim C52-C50
 with sigma of 0.04
 C49-C48 \\sim C49-C54 \\sim C49-C52 \\sim C49-C50
 with sigma of 0.02
 C5-C7 \\sim C5-C3 \\sim C7-C3 \\sim C6-C4 \\sim C6-C8 \\sim C4-C8
 with sigma of 0.04
 C2-C1 \\sim C2-C5 \\sim C2-C7 \\sim C2-C3 \\sim C2-C6 \\sim C2-C4 \\sim C2-C8
 with sigma of 0.02
 Br2-Br1 \\sim Br7-Br8 \\sim Br4-Br3 \\sim Br6-Br5
 with sigma of 0.02
 C32-C30 \\sim C32-C34 \\sim C30-C34 \\sim C33-C31 \\sim C33-C29 \\sim C31-C29
 with sigma of 0.04
 C28-C27 \\sim C28-C32 \\sim C28-C30 \\sim C28-C34 \\sim C28-C33 \\sim C28-C31
\\sim C28-C29
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Br1 \\sim Br2 \\sim Br3 \\sim Br4 \\sim Br5 \\sim Br6 \\sim Br7 \\sim Br8:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 C62, C63, C65, C67
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C62, C64, C66, C68
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C70, C71, C73, C75
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C70, C72, C74, C76
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C28, C30, C32, C34
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C10, C11, C13, C15
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C10, C12, C14, C16
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C41, C43, C45, C47
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C49, C50, C52, C54
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C41, C42, C44, C46
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C49, C51, C53, C55
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C2, C3, C5, C7
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C2, C4, C6, C8
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C28, C29, C31, C33
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C57, C58, C59, C60
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Sof(Br1)=Sof(Br2)=FVAR(1)
 Sof(Br3)=Sof(Br4)=FVAR(2)
 Sof(Br7)=Sof(Br8)=FVAR(3)
 Sof(Br5)=Sof(Br6)=FVAR(4)
 Sof(C64)=Sof(H64A)=Sof(H64B)=Sof(H64C)=Sof(C66)=Sof(H66A)=Sof(H66B)=Sof(H66C)=
 Sof(C68)=Sof(H68A)=Sof(H68B)=Sof(H68C)=1-FVAR(5)
 Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(H63C)=Sof(C65)=Sof(H65A)=Sof(H65B)=Sof(H65C)=
 Sof(C67)=Sof(H67A)=Sof(H67B)=Sof(H67C)=FVAR(5)
 Sof(C72)=Sof(H72A)=Sof(H72B)=Sof(H72C)=Sof(C74)=Sof(H74A)=Sof(H74B)=Sof(H74C)=
 Sof(C76)=Sof(H76A)=Sof(H76B)=Sof(H76C)=1-FVAR(6)
 Sof(C71)=Sof(H71A)=Sof(H71B)=Sof(H71C)=Sof(C73)=Sof(H73A)=Sof(H73B)=Sof(H73C)=
 Sof(C75)=Sof(H75A)=Sof(H75B)=Sof(H75C)=FVAR(6)
 Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=
 Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=1-FVAR(7)
 Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=
 Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=FVAR(7)
 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(8)
 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(8)
 Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(H42C)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(H44C)=
 Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(H46C)=1-FVAR(9)
 Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(H43C)=Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(H45C)=
 Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(H47C)=FVAR(9)
 Sof(C51)=Sof(H51A)=Sof(H51B)=Sof(H51C)=Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(H53C)=
 Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(H55C)=1-FVAR(10)
 Sof(C50)=Sof(H50A)=Sof(H50B)=Sof(H50C)=Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(H52C)=
 Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(H54C)=FVAR(10)
 Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H31C)=
 Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=1-FVAR(11)
 Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=
 Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=FVAR(11)
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), C37(H37A,H37B,H37C), C38(H38A,
 H38B,H38C), C39(H39A,H39B,H39C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C),
 C60(H60A,H60B,H60C), C79(H79A,H79B,H79C), C80(H80A,H80B,H80C), C81(H81A,H81B,
 H81C), C84(H84A,H84B,H84C), C85(H85A,H85B,H85C), C86(H86A,H86B,H86C), C89(H89A,
 H89B,H89C), C90(H90A,H90B,H90C), C91(H91A,H91B,H91C), C94(H94A,H94B,H94C),
 C95(H95A,H95B,H95C), C96(H96A,H96B,H96C), C99(H99A,H99B,H99C), C100(H10A,H10B,
 H10C), C101(H10D,H10E,H10F), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C),
  C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C30(H30A,H30B,
 H30C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C43(H43A,H43B,H43C), C45(H45A,
 H45B,H45C), C47(H47A,H47B,H47C), C50(H50A,H50B,H50C), C52(H52A,H52B,H52C),
 C54(H54A,H54B,H54C), C63(H63A,H63B,H63C), C65(H65A,H65B,H65C), C67(H67A,H67B,
 H67C), C71(H71A,H71B,H71C), C73(H73A,H73B,H73C), C75(H75A,H75B,H75C), C4(H4A,
 H4B,H4C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C12(H12A,H12B,H12C), C14(H14A,H14B,
 H14C), C16(H16A,H16B,H16C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C33(H33A,
 H33B,H33C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C), C46(H46A,H46B,H46C),
 C51(H51A,H51B,H51C), C53(H53A,H53B,H53C), C55(H55A,H55B,H55C), C64(H64A,H64B,
 H64C), C66(H66A,H66B,H66C), C68(H68A,H68B,H68C), C72(H72A,H72B,H72C), C74(H74A,
 H74B,H74C), C76(H76A,H76B,H76C)
;
_shelx_res_checksum              57672
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder oil'
_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 1.790
_oxdiff_exptl_absorpt_empirical_full_min 0.526