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_7047614
_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, 0.38(I2)'
_chemical_formula_sum            'C80 H144 Cr8 F8 I0.76 O32'
_chemical_formula_weight         2282.23
_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                 111.2800(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.7598(3)
_cell_length_b                   16.47840(10)
_cell_length_c                   43.8863(4)
_cell_measurement_reflns_used    29681
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      69.9860
_cell_measurement_theta_min      2.7840
_cell_volume                     23423.5(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.21a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.21a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.21a (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      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_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    -26.00   0.00   0.50    0.63    --    5.00  44.00 -64.00   52
  2  \w    -43.00 -18.00   0.50    0.63    --  -45.10  44.00 -64.00   50
  3  \w   -128.00 -71.00   0.50    0.63    --  -45.10 -44.00 144.00  114
  4  \w   -158.00-133.00   0.50    2.52    -- -107.20 -44.00 144.00   50
  5  \w   -105.00 -80.00   0.50    2.52    -- -107.20  44.00 -64.00   50
  6  \w   -134.00 -38.00   0.50    0.63    --  -45.10 -64.00-128.70  192
  7  \w   -134.00 -11.00   0.50    0.63    --  -45.10 -60.00  88.66  246
  8  \w    -71.00 -44.00   0.50    0.63    --  -45.10 -57.00  30.00   54
  9  \w   -140.00-112.00   0.50    2.52    -- -107.20  76.00 -90.00   56
 10  \w   -133.00 -97.00   0.50    2.52    -- -107.20  57.00  90.00   72
 11  \w   -197.00 -81.00   0.50    2.52    -- -107.20 -43.00 166.82  232
 12  \w    -68.00 -20.00   0.50    2.52    -- -107.20  57.00  60.00   96
 13  \w   -118.00 -69.00   0.50    2.52    -- -107.20  76.00  60.00   98
 14  \w    -56.00 -18.00   0.50    2.52    -- -107.20  76.00  60.00   76
 15  \w   -150.00 -73.00   0.50    2.52    -- -107.20 -62.00 109.78  154
 16  \w   -134.00 -77.00   0.50    2.52    -- -107.20 -65.00  47.81  114
 17  \w   -105.00 -23.00   0.50    2.52    -- -107.20  76.00 -90.00  164
 18  \w    -46.00 -18.00   0.50    2.52    -- -107.20  57.00  90.00   56
 19  \w   -190.00-164.00   0.50    2.52    -- -107.20 -65.00  47.81   52
 20  \w    -73.00 -36.00   0.50    2.52    -- -107.20  38.00 150.00   74
 21  \w    -87.00 -20.00   0.50    2.52    -- -107.20  57.00 -90.00  134
 22  \w   -147.00-110.00   0.50    2.52    -- -107.20  38.00 150.00   74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0299266000
_diffrn_orient_matrix_UB_12      0.0393742000
_diffrn_orient_matrix_UB_13      -0.0143442000
_diffrn_orient_matrix_UB_21      -0.0369890000
_diffrn_orient_matrix_UB_22      0.0334361000
_diffrn_orient_matrix_UB_23      -0.0287952000
_diffrn_orient_matrix_UB_31      0.0007413000
_diffrn_orient_matrix_UB_32      0.0779016000
_diffrn_orient_matrix_UB_33      0.0195826000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            82510
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.075
_diffrn_reflns_theta_min         2.728
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.110
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.32778
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.21a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_description       block
_exptl_crystal_F_000             9474
_exptl_crystal_recrystallization_method
'The material was recrystallised from 1-bromodecane by slow cooling'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.526
_refine_diff_density_min         -1.015
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1322
_refine_ls_number_reflns         22150
_refine_ls_number_restraints     354
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0487
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0720P)^2^+62.2370P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1320
_refine_ls_wR_factor_ref         0.1369
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19248
_reflns_number_total             22150
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03172j2.cif
_cod_data_source_block           rrepw65
_cod_depositor_comments
'Adding full bibliography for 7047602--7047620.cif.'
_cod_database_code               7047614
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         Cr8F8O32C80H144I2
_chemical_oxdiff_usercomment     DS17_282
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C78-C76 = C82-C76 = C80-C76
 1.54 with sigma of 0.02
 C74-C70 \\sim C74-C72 \\sim C70-C72 \\sim C71-C69 \\sim C71-C73 \\sim C69-C73
 with sigma of 0.04
 C68-C67 \\sim C68-C74 \\sim C68-C70 \\sim C68-C72 \\sim C68-C71 \\sim C68-C69
\\sim C68-C73
 with sigma of 0.02
 C43-C41 \\sim C43-C45 \\sim C41-C45 \\sim C42-C44 \\sim C42-C46 \\sim C44-C46
 with sigma of 0.04
 C40-C39 \\sim C40-C43 \\sim C40-C41 \\sim C40-C45 \\sim C40-C42 \\sim C40-C44
\\sim C40-C46
 with sigma of 0.02
 C37-C35 \\sim C37-C33 \\sim C35-C33 \\sim C36-C34 \\sim C36-C38 \\sim C34-C38
 with sigma of 0.04
 C32-C31 \\sim C32-C37 \\sim C32-C35 \\sim C32-C33 \\sim C32-C36 \\sim C32-C34
\\sim C32-C38
 with sigma of 0.02
 C75-C82 \\sim C75-C80 \\sim C75-C78 \\sim C82-C80 \\sim C82-C78 \\sim C80-C78
 with sigma of 0.004
 C76-C75 \\sim C76-C82 \\sim C76-C80 \\sim C76-C78
 with sigma of 0.002
 C82-C80 \\sim C82-C78 \\sim C80-C78 \\sim C79-C81 \\sim C79-C77 \\sim C81-C77
 with sigma of 0.004
 C76-C75 \\sim C76-C82 \\sim C76-C80 \\sim C76-C78 \\sim C76-C79 \\sim C76-C81
\\sim C76-C77
 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
Uanis(C82) \\sim Ueq, Uanis(C77) \\sim Ueq, Uanis(C78) \\sim Ueq, Uanis(C79)
\\sim Ueq, Uanis(C80) \\sim Ueq, Uanis(C81) \\sim Ueq, Uanis(C76) \\sim Ueq:
with sigma of 0.004 and sigma for terminal atoms of 0.004
4. Rigid body (RIGU) restrains
 C68, C70, C72, C74
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C68, C69, C71, C73
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C40, C41, C43, C45
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C40, C42, C44, C46
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C32, C33, C35, C37
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C32, C34, C36, C38
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C76, C78, C80, C82, C77, C79, C81
 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(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(4)
 Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(H70C)=Sof(C72)=Sof(H72A)=Sof(H72B)=Sof(H72C)=
 Sof(C74)=Sof(H74A)=Sof(H74B)=Sof(H74C)=FVAR(4)
 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(5)
 Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(H43C)=
 Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(H45C)=FVAR(5)
 Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=
 Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=1-FVAR(6)
 Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=
 Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(H37C)=FVAR(6)
 Sof(C77)=Sof(H77A)=Sof(H77B)=Sof(H77C)=Sof(C79)=Sof(H79A)=Sof(H79B)=Sof(H79C)=
 Sof(C81)=Sof(H81A)=Sof(H81B)=Sof(H81C)=1-FVAR(7)
 Sof(C78)=Sof(H78A)=Sof(H78B)=Sof(H78C)=Sof(C80)=Sof(H80A)=Sof(H80B)=Sof(H80C)=
 Sof(C82)=Sof(H82A)=Sof(H82B)=Sof(H82C)=FVAR(7)
6.a 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), C49(H49A,H49B,H49C),
 C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C54(H54A,H54B,H54C), C55(H55A,H55B,
 H55C), C56(H56A,H56B,H56C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C61(H61A,
 H61B,H61C), C64(H64A,H64B,H64C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C),
 C85(H85A,H85B,H85C), C86(H86A,H86B,H86C), C87(H87A,H87B,H87C), C90(H90A,H90B,
 H90C), C91(H91A,H91B,H91C), C92(H92A,H92B,H92C), C33(H33A,H33B,H33C), C35(H35A,
 H35B,H35C), C37(H37A,H37B,H37C), C41(H41A,H41B,H41C), C43(H43A,H43B,H43C),
 C45(H45A,H45B,H45C), C70(H70A,H70B,H70C), C72(H72A,H72B,H72C), C74(H74A,H74B,
 H74C), C78(H78A,H78B,H78C), C80(H80A,H80B,H80C), C82(H82A,H82B,H82C), C34(H34A,
 H34B,H34C), C36(H36A,H36B,H36C), C38(H38A,H38B,H38C), C42(H42A,H42B,H42C),
 C44(H44A,H44B,H44C), C46(H46A,H46B,H46C), C69(H69A,H69B,H69C), C71(H71A,H71B,
 H71C), C73(H73A,H73B,H73C), C77(H77A,H77B,H77C), C79(H79A,H79B,H79C), C81(H81A,
 H81B,H81C)
;
_shelx_res_checksum              65197
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a mylar loop with fomblin 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 3.084
_oxdiff_exptl_absorpt_empirical_full_min 0.545