Reversible uptake of sulfur-containing gases by single crystals of a Cr<sub>8</sub> metallacrown.
Vitórica-Yrezábal, Iñigo J; Sava, Daniel Florin; Reta, Daniel; Timco, Grigore A.; Winpenny, Richard E. P.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 13184–13189; doi:10.1039/c9dt02378j

data_7700802
_publ_section_title
;
 Reversible uptake of sulfur-containing gases by single crystals of a
 Cr<sub>8</sub> metallacrown.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13184
_journal_page_last               13189
_journal_paper_doi               10.1039/c9dt02378j
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C80 H144 Cr8 F8 O32, 0.85(O2 S)'
_chemical_formula_sum            'C80 H144 Cr8 F8 O33.73 S0.87'
_chemical_formula_weight         2241.44
_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             2019-02-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-06-04 deposited with the CCDC.    2019-08-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.428(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.8985(11)
_cell_length_b                   16.5023(4)
_cell_length_c                   44.0954(16)
_cell_measurement_reflns_used    12798
_cell_measurement_temperature    149.8(5)
_cell_measurement_theta_max      27.2120
_cell_measurement_theta_min      3.5680
_cell_volume                     23639.4(14)
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      149.8(5)
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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    -16.00  10.00   1.00   20.00    --  -18.77 -99.00  90.00   26
  2  \w     18.00  88.00   1.00   20.00    --   20.10  57.00  60.00   70
  3  \w     -7.00  81.00   1.00   20.00    --   20.10  37.00-150.00   88
  4  \w     24.00  61.00   1.00   20.00    --   20.10 -99.00   0.00   37
  5  \w    -49.00   6.00   1.00   20.00    --   20.10 -57.00 -90.00   55
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0604
_diffrn_reflns_av_unetI/netI     0.0937
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_number            59475
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.278
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.799
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55156
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.27b (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    1.260
_exptl_crystal_description       block
_exptl_crystal_F_000             9374
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.681
_refine_diff_density_min         -0.699
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1461
_refine_ls_number_reflns         24082
_refine_ls_number_restraints     729
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1036
_refine_ls_R_factor_gt           0.0596
_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^)+(0.0488P)^2^+31.9162P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1242
_refine_ls_wR_factor_ref         0.1478
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15604
_reflns_number_total             24082
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02378j2.cif
_cod_data_source_block           arepw1442_3_150_00
_cod_depositor_comments
'Adding full bibliography for 7700801--7700822.cif.'
_cod_database_code               7700802
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.924
_shelx_estimated_absorpt_t_min   0.691
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H53B-H47B_$1
 -2 with sigma of 0.001
 S1A-O1 = S1A-O2
 1.43 with sigma of 0.02
 S1-O3 = S1-O4
 1.43 with sigma of 0.02
 O74-O6
 2.4 with sigma of 0.02
 S4-O74 = S4-O6
 1.43 with sigma of 0.02
 C14-C16 \\sim C14-C18 \\sim C13-C15 \\sim C13-C17 \\sim C15-C17 \\sim C16-C18
 with sigma of 0.004
 C12-C14 \\sim C12-C13 \\sim C12-C15 \\sim C12-C16 \\sim C12-C11 \\sim C12-C18
\\sim C12-C17
 with sigma of 0.002
 C25-C23 \\sim C26-C24 \\sim C24-C22 \\sim C23-C21
 with sigma of 0.004
 C20-C25 \\sim C20-C26 \\sim C20-C24 \\sim C20-C23 \\sim C20-C22 \\sim C20-C21
\\sim C20-C19
 with sigma of 0.002
 C31-C29 \\sim C31-C33 \\sim C32-C30 \\sim C32-C34 \\sim C29-C33 \\sim C30-C34
 with sigma of 0.004
 C28-C31 \\sim C28-C32 \\sim C28-C29 \\sim C28-C30 \\sim C28-C27 \\sim C28-C33
\\sim C28-C34
 with sigma of 0.002
 C42-C38 \\sim C42-C40 \\sim C38-C40 \\sim C41-C37 \\sim C41-C39 \\sim C37-C39
 with sigma of 0.004
 C36-C35 \\sim C36-C42 \\sim C36-C38 \\sim C36-C40 \\sim C36-C41 \\sim C36-C37
\\sim C36-C39
 with sigma of 0.002
 C49-C47 \\sim C49-C45 \\sim C50-C48 \\sim C50-C46 \\sim C47-C45 \\sim C48-C46
 with sigma of 0.004
 C44-C49 \\sim C44-C50 \\sim C44-C43 \\sim C44-C47 \\sim C44-C48 \\sim C44-C46
\\sim C44-C45
 with sigma of 0.002
 C83-C79 \\sim C83-C81 \\sim C82-C78 \\sim C82-C80 \\sim C79-C81 \\sim C78-C80
 with sigma of 0.004
 C77-C83 \\sim C77-C82 \\sim C77-C79 \\sim C77-C78 \\sim C77-C76 \\sim C77-C80
\\sim C77-C81
 with sigma of 0.002
 C90-C88 \\sim C90-C86 \\sim C88-C86 \\sim C89-C91 \\sim C89-C87 \\sim C91-C87
 with sigma of 0.004
 C85-C84 \\sim C85-C90 \\sim C85-C88 \\sim C85-C86 \\sim C85-C89 \\sim C85-C91
\\sim C85-C87
 with sigma of 0.002
 O4-O3 \\sim O1-O2 \\sim O74-O6
 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
C81 \\sim C82 \\sim C83 \\sim C78 \\sim C79 \\sim C80: within 2A with sigma of
0.002 and sigma for terminal atoms of 0.004
C86 \\sim C50 \\sim C49 \\sim C48 \\sim C47 \\sim C46 \\sim C45: within 2A with
sigma of 0.002 and sigma for terminal atoms of 0.004
C89 \\sim C88 \\sim C85 \\sim C90 \\sim C91 \\sim C86 \\sim C87: within 2A with
sigma of 0.002 and sigma for terminal atoms of 0.004
S1 \\sim O1 \\sim O2 \\sim O6 \\sim O74: within 2A with sigma of 0.002 and
sigma for terminal atoms of 0.004
S1 \\sim O3 \\sim O4 \\sim O1 \\sim O2 \\sim O6 \\sim O74: within 2A with sigma
of 0.002 and sigma for terminal atoms of 0.004
S1 \\sim S4 \\sim S1A: within 2A with sigma of 0.002 and sigma for terminal
atoms of 0.004
4. Rigid body (RIGU) restrains
 C85, C86, C88, C90
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C77, C78, C80, C82
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C12, C13, C15, C17
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C12, C14, C16, C18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C20, C21, C23, C25
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C20, C22, C24, C26
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C28, C29, C31, C33
 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 0.004 and sigma for 1-3 distances of 0.004
 C36, C38, C40, C42
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C36, C37, C39, C41
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C44, C46, C48, C50
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C3, C4, C5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C44, C45, C47, C49
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C77, C79, C81, C83
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C85, C87, C89, C91
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(S1)=Sof(O3)=Sof(O4)=FVAR(1)
 Sof(O1)=Sof(O2)=Sof(S1A)=FVAR(2)
 Sof(O6)=Sof(O74)=Sof(S4)=FVAR(3)
 Sof(C87)=Sof(H87A)=Sof(H87B)=Sof(H87C)=Sof(C89)=Sof(H89A)=Sof(H89B)=Sof(H89C)=
 Sof(C91)=Sof(H91A)=Sof(H91B)=Sof(H91C)=1-FVAR(4)
 Sof(C86)=Sof(H86A)=Sof(H86B)=Sof(H86C)=Sof(C88)=Sof(H88A)=Sof(H88B)=Sof(H88C)=
 Sof(C90)=Sof(H90A)=Sof(H90B)=Sof(H90C)=FVAR(4)
 Sof(C79)=Sof(H79A)=Sof(H79B)=Sof(H79C)=Sof(C81)=Sof(H81A)=Sof(H81B)=Sof(H81C)=
 Sof(C83)=Sof(H83A)=Sof(H83B)=Sof(H83C)=1-FVAR(5)
 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(5)
 Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=
 Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=1-FVAR(6)
 Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=
 Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=FVAR(6)
 Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=
 Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=1-FVAR(7)
 Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=
 Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=FVAR(7)
 Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=
 Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=1-FVAR(8)
 Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H31C)=
 Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=FVAR(8)
 Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(H37C)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=
 Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=1-FVAR(9)
 Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=
 Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(H42C)=FVAR(9)
 Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(H46C)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(H48C)=
 Sof(C50)=Sof(H50A)=Sof(H50B)=Sof(H50C)=1-FVAR(10)
 Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(H45C)=Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(H47C)=
 Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(H49C)=FVAR(10)
6.a Me refined with riding coordinates:
 C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C21(H21A,H21B,
 H21C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C29(H29A,H29B,H29C), C31(H31A,
 H31B,H31C), C33(H33A,H33B,H33C), C38(H38A,H38B,H38C), C40(H40A,H40B,H40C),
 C42(H42A,H42B,H42C), C45(H45A,H45B,H45C), C47(H47A,H47B,H47C), C49(H49A,H49B,
 H49C), C78(H78A,H78B,H78C), C80(H80A,H80B,H80C), C82(H82A,H82B,H82C), C86(H86A,
 H86B,H86C), C88(H88A,H88B,H88C), C90(H90A,H90B,H90C), C14(H14A,H14B,H14C),
 C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C22(H22A,H22B,H22C), C24(H24A,H24B,
 H24C), C26(H26A,H26B,H26C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C34(H34A,
 H34B,H34C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C46(H46A,H46B,H46C),
 C48(H48A,H48B,H48C), C50(H50A,H50B,H50C), C79(H79A,H79B,H79C), C81(H81A,H81B,
 H81C), C83(H83A,H83B,H83C), C87(H87A,H87B,H87C), C89(H89A,H89B,H89C), C91(H91A,
 H91B,H91C)
6.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C8(H8A,H8B,H8C), C9(H9A,
 H9B,H9C), C10(H10A,H10B,H10C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C),
 C55(H55A,H55B,H55C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C60(H60A,H60B,
 H60C), 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), C94(H94A,H94B,H94C), C95(H95A,H95B,
 H95C), C96(H96A,H96B,H96C), C99(H99A,H99B,H99C), C100(H10D,H10E,H10F),
 C101(H10G,H10H,H10I), C37(H37A,H37B,H37C)
;
_shelx_res_checksum              48788
_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
;