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_7700820
_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, O1.69 S0.84'
_chemical_formula_sum            'C80 H144 Cr8 F8 O33.69 S0.84'
_chemical_formula_weight         2239.91
_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             2018-11-05
_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                 111.360(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.7957(14)
_cell_length_b                   16.4957(3)
_cell_length_c                   44.1262(15)
_cell_measurement_reflns_used    17794
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      27.4780
_cell_measurement_theta_min      1.5550
_cell_volume                     23587.8(15)
_computing_cell_refinement       'CrysAlisPro 1.171.40.20a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.20a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.20a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.842
_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    -67.00 108.00   1.00    6.00    --   19.90  60.00 -30.00  175
  2  \w    -53.00 -25.00   1.00    6.00    --   19.90  30.00 -60.00   28
  3  \w    -60.00   9.00   1.00    6.00    --   19.90  30.00 120.00   69
;
_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      -0.0213069000
_diffrn_orient_matrix_UB_12      0.0083538000
_diffrn_orient_matrix_UB_13      -0.0081734000
_diffrn_orient_matrix_UB_21      0.0022875000
_diffrn_orient_matrix_UB_22      0.0366806000
_diffrn_orient_matrix_UB_23      0.0088785000
_diffrn_orient_matrix_UB_31      0.0045464000
_diffrn_orient_matrix_UB_32      0.0207641000
_diffrn_orient_matrix_UB_33      -0.0123473000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0578
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.842
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            57205
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.842
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.197
_diffrn_reflns_theta_min         1.564
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Mo) X-ray DW Source'
_exptl_absorpt_coefficient_mu    0.801
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75894
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.20a (Rigaku Oxford Diffraction, 2018)
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    1.261
_exptl_crystal_description       block
_exptl_crystal_F_000             9368
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.972
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1446
_refine_ls_number_reflns         26876
_refine_ls_number_restraints     971
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0794
_refine_ls_R_factor_gt           0.0527
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0605P)^2^+45.0217P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1302
_refine_ls_wR_factor_ref         0.1426
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19294
_reflns_number_total             26876
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02378j2.cif
_cod_data_source_block           lrepw222
_cod_depositor_comments
'Adding full bibliography for 7700801--7700822.cif.'
_cod_database_code               7700820
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         Cr8F8O34C80H144S
_chemical_oxdiff_usercomment     'DS18_409 Cr8+SO2'
_shelx_estimated_absorpt_t_max   0.924
_shelx_estimated_absorpt_t_min   0.825
_diffrn_oxdiff_ac4_digest_frames
;
0132651e5b7a61ce5c86697d2ce0f9714100272af95
;
_reflns_odcompleteness_completeness 99.80
_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
 O5-O6
 2.4 with sigma of 0.02
 O1-O3 \\sim O1-O4 \\sim O2-O3 \\sim O2-O4
 with sigma of 0.04
 S1-O1 \\sim S1-O2 \\sim S1-O3 \\sim S1-O4
 with sigma of 0.02
 S1-O6 \\sim S1-O2 \\sim S1-O1 \\sim S1-O4 \\sim S1-O3 \\sim S1-O5
 with sigma of 0.002
 C10-C14 \\sim C10-C15
 with sigma of 0.02
 C10-C16 \\sim C10-C11
 with sigma of 0.02
 C10-C12 \\sim C10-C13
 with sigma of 0.02
 C14-C16 \\sim C14-C12 \\sim C16-C12 \\sim C11-C13 \\sim C11-C15 \\sim C13-C15
 with sigma of 0.004
 C10-C9 \\sim C10-C14 \\sim C10-C16 \\sim C10-C12 \\sim C10-C11 \\sim C10-C13
\\sim C10-C15
 with sigma of 0.002
 C2-C8 \\sim C2-C3
 with sigma of 0.02
 C2-C4 \\sim C2-C5
 with sigma of 0.02
 C2-C6 \\sim C2-C7
 with sigma of 0.02
 C8-C4 \\sim C8-C6 \\sim C4-C6 \\sim C5-C7 \\sim C5-C3 \\sim C7-C3
 with sigma of 0.004
 C2-C1 \\sim C2-C8 \\sim C2-C4 \\sim C2-C6 \\sim C2-C5 \\sim C2-C7 \\sim C2-C3
 with sigma of 0.002
 C67-C73 \\sim C67-C74
 with sigma of 0.02
 C67-C70 \\sim C67-C72
 with sigma of 0.02
 C67-C68 \\sim C67-C69
 with sigma of 0.02
 C73-C70 \\sim C73-C68 \\sim C70-C68 \\sim C69-C72 \\sim C69-C74 \\sim C72-C74
 with sigma of 0.004
 C67-C66 \\sim C67-C73 \\sim C67-C70 \\sim C67-C68 \\sim C67-C69 \\sim C67-C72
\\sim C67-C74
 with sigma of 0.002
 C76-C77 \\sim C76-C78
 with sigma of 0.02
 C76-C81 \\sim C76-C82
 with sigma of 0.02
 C76-C79 \\sim C76-C80
 with sigma of 0.02
 C77-C81 \\sim C77-C79 \\sim C81-C79 \\sim C82-C78 \\sim C82-C80 \\sim C78-C80
 with sigma of 0.004
 C76-C75 \\sim C76-C77 \\sim C76-C81 \\sim C76-C79 \\sim C76-C82 \\sim C76-C78
\\sim C76-C80
 with sigma of 0.002
 C51-C53 \\sim C51-C54
 with sigma of 0.02
 C51-C55 \\sim C51-C56
 with sigma of 0.02
 C51-C57 \\sim C51-C52
 with sigma of 0.02
 C53-C55 \\sim C53-C57 \\sim C55-C57 \\sim C54-C56 \\sim C54-C52 \\sim C56-C52
 with sigma of 0.004
 C51-C50 \\sim C51-C53 \\sim C51-C55 \\sim C51-C57 \\sim C51-C54 \\sim C51-C56
\\sim C51-C52
 with sigma of 0.002
 C84-C87 \\sim C84-C88
 with sigma of 0.02
 C84-C89 \\sim C84-C90
 with sigma of 0.02
 C84-C85 \\sim C84-C86
 with sigma of 0.02
 C87-C89 \\sim C87-C85 \\sim C89-C85 \\sim C86-C88 \\sim C86-C90 \\sim C88-C90
 with sigma of 0.004
 C84-C83 \\sim C84-C87 \\sim C84-C89 \\sim C84-C85 \\sim C84-C86 \\sim C84-C88
\\sim C84-C90
 with sigma of 0.002
 C38-C41 \\sim C38-C42
 with sigma of 0.02
 C38-C39 \\sim C38-C40
 with sigma of 0.02
 C38-C43 \\sim C38-C44
 with sigma of 0.02
 C41-C39 \\sim C41-C43 \\sim C39-C43 \\sim C44-C40 \\sim C44-C42 \\sim C40-C42
 with sigma of 0.004
 C38-C37 \\sim C38-C41 \\sim C38-C39 \\sim C38-C43 \\sim C38-C44 \\sim C38-C40
\\sim C38-C42
 with sigma of 0.002
 C59-C60 \\sim C59-C61
 with sigma of 0.02
 C59-C62 \\sim C59-C63
 with sigma of 0.02
 C59-C64 \\sim C59-C65
 with sigma of 0.02
 C60-C62 \\sim C60-C64 \\sim C62-C64 \\sim C63-C65 \\sim C63-C61 \\sim C65-C61
 with sigma of 0.004
 C59-C58 \\sim C59-C60 \\sim C59-C62 \\sim C59-C64 \\sim C59-C63 \\sim C59-C65
\\sim C59-C61
 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
S1 \\sim O1 \\sim O2 \\sim O3 \\sim O4: within 2A with sigma of 0.002 and sigma
for terminal atoms of 0.004
O5 \\sim S1 \\sim O1 \\sim O3 \\sim O4 \\sim O6 \\sim O2: within 2A with sigma
of 0.002 and sigma for terminal atoms of 0.004
C15 \\sim C16 \\sim C11 \\sim C12 \\sim C10 \\sim C13 \\sim C14: within 2A with
sigma of 0.002 and sigma for terminal atoms of 0.004
C3 \\sim C4 \\sim C5 \\sim C2 \\sim C6 \\sim C7 \\sim C8: within 2A with sigma
of 0.002 and sigma for terminal atoms of 0.004
C72 \\sim C67 \\sim C69 \\sim C70 \\sim C68 \\sim C74 \\sim C73: within 2A with
sigma of 0.002 and sigma for terminal atoms of 0.004
C81 \\sim C82 \\sim C77 \\sim C78 \\sim C79 \\sim C80 \\sim C76: within 2A with
sigma of 0.002 and sigma for terminal atoms of 0.004
C53 \\sim C54 \\sim C55 \\sim C51 \\sim C56 \\sim C52 \\sim C57: within 2A with
sigma of 0.002 and sigma for terminal atoms of 0.004
C86 \\sim C85 \\sim C84 \\sim C87 \\sim C88 \\sim C89 \\sim C90: within 2A with
sigma of 0.002 and sigma for terminal atoms of 0.004
C39 \\sim C40 \\sim C38 \\sim C41 \\sim C42 \\sim C43 \\sim C44: within 2A with
sigma of 0.002 and sigma for terminal atoms of 0.004
C62 \\sim C63 \\sim C64 \\sim C65 \\sim C59 \\sim C61 \\sim C60: within 2A with
sigma of 0.002 and sigma for terminal atoms of 0.004
4. Rigid body (RIGU) restrains
 C15, C16, C10, C14, C13, C12, C11
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 1*[Sof(O1)+Sof(O2)]+1*[Sof(O3)+Sof(O4)]+1*[Sof(O6)+Sof(O5)]=0.84318 with esd
 of 0.001
 Sof(O1)=Sof(O2)=FVAR(1)
 Sof(O3)=Sof(O4)=FVAR(2)
 Sof(O6)=Sof(O5)=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(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=
 Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=FVAR(4)
 Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=Sof(C3)=
 Sof(H3A)=Sof(H3B)=Sof(H3C)=1-FVAR(5)
 Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=Sof(C6)=
 Sof(H6A)=Sof(H6B)=Sof(H6C)=FVAR(5)
 Sof(C69)=Sof(H69A)=Sof(H69B)=Sof(H69C)=Sof(C72)=Sof(H72A)=Sof(H72B)=Sof(H72C)=
 Sof(C74)=Sof(H74A)=Sof(H74B)=Sof(H74C)=1-FVAR(6)
 Sof(C73)=Sof(H73A)=Sof(H73B)=Sof(H73C)=Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(H70C)=
 Sof(C68)=Sof(H68A)=Sof(H68B)=Sof(H68C)=FVAR(6)
 Sof(C82)=Sof(H82A)=Sof(H82B)=Sof(H82C)=Sof(C78)=Sof(H78A)=Sof(H78B)=Sof(H78C)=
 Sof(C80)=Sof(H80A)=Sof(H80B)=Sof(H80C)=1-FVAR(7)
 Sof(C77)=Sof(H77A)=Sof(H77B)=Sof(H77C)=Sof(C81)=Sof(H81A)=Sof(H81B)=Sof(H81C)=
 Sof(C79)=Sof(H79A)=Sof(H79B)=Sof(H79C)=FVAR(7)
 Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(H54C)=Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(H56C)=
 Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(H52C)=1-FVAR(8)
 Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(H53C)=Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(H55C)=
 Sof(C57)=Sof(H57A)=Sof(H57B)=Sof(H57C)=FVAR(8)
 Sof(C86)=Sof(H86A)=Sof(H86B)=Sof(H86C)=Sof(C88)=Sof(H88A)=Sof(H88B)=Sof(H88C)=
 Sof(C90)=Sof(H90A)=Sof(H90B)=Sof(H90C)=1-FVAR(9)
 Sof(C87)=Sof(H87A)=Sof(H87B)=Sof(H87C)=Sof(C89)=Sof(H89A)=Sof(H89B)=Sof(H89C)=
 Sof(C85)=Sof(H85A)=Sof(H85B)=Sof(H85C)=FVAR(9)
 Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(H44C)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=
 Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(H42C)=1-FVAR(10)
 Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=
 Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(H43C)=FVAR(10)
 Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(H63C)=Sof(C65)=Sof(H65A)=Sof(H65B)=Sof(H65C)=
 Sof(C61)=Sof(H61A)=Sof(H61B)=Sof(H61C)=1-FVAR(11)
 Sof(C60)=Sof(H60A)=Sof(H60B)=Sof(H60C)=Sof(C62)=Sof(H62A)=Sof(H62B)=Sof(H62C)=
 Sof(C64)=Sof(H64A)=Sof(H64B)=Sof(H64C)=FVAR(11)
6.a Me refined with riding coordinates:
 C105(H10A,H10B,H10C), C98(H98A,H98B,H98C), C103(H10D,H10E,H10F), C34(H34A,
 H34B,H34C), C104(H10G,H10H,H10I), C99(H99A,H99B,H99C), C41(H41A,H41B,H41C),
 C25(H25A,H25B,H25C), C100(H10J,H10K,H10L), C19(H19A,H19B,H19C), C47(H47A,H47B,
 H47C), C21(H21A,H21B,H21C), C49(H49A,H49B,H49C), C87(H87A,H87B,H87C), C89(H89A,
 H89B,H89C), C36(H36A,H36B,H36C), C24(H24A,H24B,H24C), C95(H95A,H95B,H95C),
 C26(H26A,H26B,H26C), C20(H20A,H20B,H20C), C39(H39A,H39B,H39C), C29(H29A,H29B,
 H29C), C94(H94A,H94B,H94C), C30(H30A,H30B,H30C), C93(H93A,H93B,H93C), C35(H35A,
 H35B,H35C), C53(H53A,H53B,H53C), C85(H85A,H85B,H85C), C60(H60A,H60B,H60C),
 C62(H62A,H62B,H62C), C43(H43A,H43B,H43C), C73(H73A,H73B,H73C), C31(H31A,H31B,
 H31C), C55(H55A,H55B,H55C), C64(H64A,H64B,H64C), C70(H70A,H70B,H70C), C8(H8A,
 H8B,H8C), C14(H14A,H14B,H14C), C57(H57A,H57B,H57C), C4(H4A,H4B,H4C), C77(H77A,
 H77B,H77C), C68(H68A,H68B,H68C), C6(H6A,H6B,H6C), C81(H81A,H81B,H81C),
 C16(H16A,H16B,H16C), C12(H12A,H12B,H12C), C79(H79A,H79B,H79C), C11(H11A,H11B,
 H11C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C5(H5A,H5B,H5C), C7(H7A,H7B,
 H7C), C3(H3A,H3B,H3C), C69(H69A,H69B,H69C), C72(H72A,H72B,H72C), C74(H74A,H74B,
 H74C), C82(H82A,H82B,H82C), C78(H78A,H78B,H78C), C80(H80A,H80B,H80C), C54(H54A,
 H54B,H54C), C56(H56A,H56B,H56C), C52(H52A,H52B,H52C), C86(H86A,H86B,H86C),
 C88(H88A,H88B,H88C), C90(H90A,H90B,H90C), C44(H44A,H44B,H44C), C42(H42A,H42B,
 H42C), C63(H63A,H63B,H63C), C65(H65A,H65B,H65C), C61(H61A,H61B,H61C)
6.b Idealised Me refined as rotating group:
 C48(H48A,H48B,H48C), C40(H40A,H40B,H40C)
;
_shelx_res_checksum              22206
_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 1.698
_oxdiff_exptl_absorpt_empirical_full_min 0.663