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_7047602
_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, 0.74(Cl2)'
_chemical_formula_sum            'C80 H144 Cl1.5 Cr8 F8 O32'
_chemical_formula_weight         2238.99
_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                 111.359(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.8424(9)
_cell_length_b                   16.5213(3)
_cell_length_c                   44.0605(19)
_cell_measurement_reflns_used    17520
_cell_measurement_temperature    149.9(5)
_cell_measurement_theta_max      26.3070
_cell_measurement_theta_min      3.6570
_cell_volume                     23621.0(14)
_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      149.9(5)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1428
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_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     21.00  53.00   1.00   27.50    --  -18.62  37.00-120.00   32
  2  \w    -18.00  23.00   1.00   27.50    --  -18.62 -99.00-180.00   41
  3  \w      3.00  69.00   1.00   27.50    --   20.18  57.00  60.00   66
  4  \w    -11.00  87.00   1.00   27.50    --   20.18  77.00 -60.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0165533000
_diffrn_orient_matrix_UB_12      0.0074086000
_diffrn_orient_matrix_UB_13      0.0053747000
_diffrn_orient_matrix_UB_21      -0.0142251000
_diffrn_orient_matrix_UB_22      -0.0116724000
_diffrn_orient_matrix_UB_23      -0.0154943000
_diffrn_orient_matrix_UB_31      0.0010652000
_diffrn_orient_matrix_UB_32      -0.0406692000
_diffrn_orient_matrix_UB_33      0.0054340000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_number            49902
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.392
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.817
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60357
_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            'clear dark green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_description       block
_exptl_crystal_F_000             9355
_exptl_crystal_preparation       'Product put into Cl2 atmosphere.'
_exptl_crystal_recrystallization_method
'Product crystallized from 1Br-Decane.'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.342
_refine_diff_density_min         -0.619
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1331
_refine_ls_number_reflns         24024
_refine_ls_number_restraints     397
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0471
_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^)+(0.0608P)^2^+64.3815P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1231
_refine_ls_wR_factor_ref         0.1324
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19747
_reflns_number_total             24024
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03172j2.cif
_cod_data_source_block           arepw1378
_cod_depositor_comments
'Adding full bibliography for 7047602--7047620.cif.'
_cod_original_formula_sum        'C80 H144 Cl1.50 Cr8 F8 O32'
_cod_database_code               7047602
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         Cr8F8O32C80H144Cl2
_chemical_oxdiff_usercomment     DS17_275
_reflns_odcompleteness_completeness 99.43
_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
 C44-C40 \\sim C44-C42 \\sim C40-C42 \\sim C43-C39 \\sim C43-C41 \\sim C39-C41
 with sigma of 0.04
 C38-C37 \\sim C38-C44 \\sim C38-C40 \\sim C38-C42 \\sim C38-C43 \\sim C38-C39
\\sim C38-C41
 with sigma of 0.02
 C14-C12 \\sim C14-C16 \\sim C12-C16 \\sim C15-C13 \\sim C15-C11 \\sim C13-C11
 with sigma of 0.04
 C10-C9 \\sim C10-C14 \\sim C10-C12 \\sim C10-C16 \\sim C10-C15 \\sim C10-C13
\\sim C10-C11
 with sigma of 0.02
 C58-C60 \\sim C58-C56 \\sim C60-C56 \\sim C57-C59 \\sim C57-C55 \\sim C59-C55
 with sigma of 0.04
 C54-C53 \\sim C54-C58 \\sim C54-C60 \\sim C54-C56 \\sim C54-C57 \\sim C54-C59
\\sim C54-C55
 with sigma of 0.02
 C7-C5 \\sim C7-C3 \\sim C5-C3 \\sim C8-C6 \\sim C8-C4 \\sim C6-C4
 with sigma of 0.04
 C2-C1 \\sim C2-C7 \\sim C2-C5 \\sim C2-C3 \\sim C2-C8 \\sim C2-C6 \\sim C2-C4
 with sigma of 0.02
 C47-C49 \\sim C47-C51 \\sim C49-C51 \\sim C48-C50 \\sim C48-C52 \\sim C50-C52
 with sigma of 0.004
 C46-C45 \\sim C46-C47 \\sim C46-C49 \\sim C46-C51 \\sim C46-C48 \\sim C46-C50
\\sim C46-C52
 with sigma of 0.02
 Cl4-Cl3 \\sim Cl2-Cl1
 with sigma of 0.02
 Cl2-Cl1 \\sim Cl4-Cl3
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C38, C40, C42, C44
 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
 C10, C11, C13, C15
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C54, C56, C58, C60
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C54, C55, C57, C59
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C38, C39, C41, C43
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C67, C68, C69, C70
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C62, C63, C64, C65
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C2, C3, C5, C7
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C2, C4, C6, C8
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C46, C47, C49, C51
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C46, C48, C50, C52
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Others
 Sof(Cl3)=Sof(Cl4)=FVAR(1)
 Sof(Cl1)=Sof(Cl2)=FVAR(2)
 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(3)
 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(3)
 Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(H48C)=Sof(C50)=Sof(H50A)=Sof(H50B)=Sof(H50C)=
 Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(H52C)=1-FVAR(4)
 Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(H47C)=Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(H49C)=
 Sof(C51)=Sof(H51A)=Sof(H51B)=Sof(H51C)=FVAR(4)
 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(5)
 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(5)
 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(6)
 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(6)
 Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(H55C)=Sof(C57)=Sof(H57A)=Sof(H57B)=Sof(H57C)=
 Sof(C59)=Sof(H59A)=Sof(H59B)=Sof(H59C)=1-FVAR(7)
 Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(H56C)=Sof(C58)=Sof(H58A)=Sof(H58B)=Sof(H58C)=
 Sof(C60)=Sof(H60A)=Sof(H60B)=Sof(H60C)=FVAR(7)
5.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), C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C65(H65A,H65B,
 H65C), C68(H68A,H68B,H68C), C69(H69A,H69B,H69C), C70(H70A,H70B,H70C), C73(H73A,
 H73B,H73C), C74(H74A,H74B,H74C), C75(H75A,H75B,H75C), C78(H78A,H78B,H78C),
 C79(H79A,H79B,H79C), C80(H80A,H80B,H80C), C83(H83A,H83B,H83C), C84(H84A,H84B,
 H84C), C85(H85A,H85B,H85C), C88(H88A,H88B,H88C), C89(H89A,H89B,H89C), C90(H90A,
 H90B,H90C), C93(H93A,H93B,H93C), C94(H94A,H94B,H94C), C95(H95A,H95B,H95C),
 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), C47(H47A,H47B,H47C), C49(H49A,H49B,H49C), C51(H51A,
 H51B,H51C), C56(H56A,H56B,H56C), C58(H58A,H58B,H58C), C60(H60A,H60B,H60C),
 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), C48(H48A,H48B,H48C), C50(H50A,H50B,H50C), C52(H52A,
 H52B,H52C), C55(H55A,H55B,H55C), C57(H57A,H57B,H57C), C59(H59A,H59B,H59C)
;
_shelx_res_checksum              67688
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a 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 1.351
_oxdiff_exptl_absorpt_empirical_full_min 0.722