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_7700819
_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'
_chemical_formula_sum            'C80 H144 Cr8 F8 O32'
_chemical_formula_weight         2185.94
_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             2018-01-25
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-06-04 deposited with the CCDC.    2019-08-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.279(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.7353(9)
_cell_length_b                   16.5967(4)
_cell_length_c                   44.7645(14)
_cell_measurement_reflns_used    19817
_cell_measurement_temperature    239.92(10)
_cell_measurement_theta_max      27.0690
_cell_measurement_theta_min      1.8320
_cell_volume                     24047.0(12)
_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)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      239.92(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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     66.00 106.00   1.00   12.00    --   19.30  43.00 -90.00   40
  2  \w    -70.00 107.00   1.00   12.00    --   19.30  57.00-120.00  177
  3  \w    -51.00 -17.00   1.00   12.00    --   19.30  60.00 120.00   34
  4  \w    -35.00  56.00   1.00   12.00    --   19.30  43.00 -90.00   91
;
_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      0.0084218000
_diffrn_orient_matrix_UB_12      -0.0120607000
_diffrn_orient_matrix_UB_13      0.0162936000
_diffrn_orient_matrix_UB_21      -0.0080154000
_diffrn_orient_matrix_UB_22      0.0353844000
_diffrn_orient_matrix_UB_23      0.0045045000
_diffrn_orient_matrix_UB_31      -0.0185893000
_diffrn_orient_matrix_UB_32      -0.0206777000
_diffrn_orient_matrix_UB_33      -0.0018501000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            68925
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         1.943
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.769
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55632
_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    1.208
_exptl_crystal_description       block
_exptl_crystal_F_000             9152
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.188
_refine_diff_density_min         -0.536
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1463
_refine_ls_number_reflns         24550
_refine_ls_number_restraints     801
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0748
_refine_ls_R_factor_gt           0.0515
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0861P)^2^+33.5767P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1466
_refine_ls_wR_factor_ref         0.1603
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17870
_reflns_number_total             24550
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02378j2.cif
_cod_data_source_block           lrepw134_2_240_00
_cod_depositor_comments
'Adding full bibliography for 7700801--7700822.cif.'
_cod_database_code               7700819
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         Cr8F8O32C80H146S
_shelx_estimated_absorpt_t_max   0.927
_shelx_estimated_absorpt_t_min   0.749
_reflns_odcompleteness_completeness 88.52
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.66
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C13-C11 \\sim C13-C15 \\sim C11-C15 \\sim C16-C14 \\sim C16-C12 \\sim C14-C12
 with sigma of 0.004
 C10-C9 \\sim C10-C13 \\sim C10-C11 \\sim C10-C15 \\sim C10-C16 \\sim C10-C14
\\sim C10-C12
 with sigma of 0.002
 C39-C37 \\sim C39-C41 \\sim C37-C41 \\sim C40-C42 \\sim C40-C38 \\sim C42-C38
 with sigma of 0.004
 C36-C35 \\sim C36-C39 \\sim C36-C37 \\sim C36-C41 \\sim C36-C40 \\sim C36-C42
\\sim C36-C38
 with sigma of 0.002
 C68-C70 \\sim C68-C66 \\sim C70-C66 \\sim C71-C67 \\sim C71-C69 \\sim C67-C69
 with sigma of 0.004
 C65-C64 \\sim C65-C68 \\sim C65-C70 \\sim C65-C66 \\sim C65-C71 \\sim C65-C67
\\sim C65-C69
 with sigma of 0.002
 C104-C100 \\sim C100-C102 \\sim C103-C99 \\sim C101-C99
 with sigma of 0.004
 C98-C97 \\sim C98-C104 \\sim C98-C100 \\sim C98-C102 \\sim C98-C103 \\sim
C98-C101 \\sim C98-C99
 with sigma of 0.002
 C6-C8 \\sim C6-C4 \\sim C8-C4 \\sim C3-C7 \\sim C3-C5 \\sim C7-C5
 with sigma of 0.004
 C2-C1 \\sim C2-C6 \\sim C2-C8 \\sim C2-C4 \\sim C2-C3 \\sim C2-C7 \\sim C2-C5
 with sigma of 0.002
 C31-C33 \\sim C31-C29 \\sim C33-C29 \\sim C34-C32 \\sim C34-C30 \\sim C32-C30
 with sigma of 0.004
 C28-C27 \\sim C28-C31 \\sim C28-C33 \\sim C28-C29 \\sim C28-C34 \\sim C28-C32
\\sim C28-C30
 with sigma of 0.002
 C47-C49 \\sim C47-C45 \\sim C49-C45 \\sim C50-C48 \\sim C50-C46 \\sim C48-C46
 with sigma of 0.004
 C44-C43 \\sim C44-C47 \\sim C44-C49 \\sim C44-C45 \\sim C44-C50 \\sim C44-C48
\\sim C44-C46
 with sigma of 0.002
 C61-C59 \\sim C61-C63 \\sim C59-C63 \\sim C58-C60 \\sim C58-C62 \\sim C60-C62
 with sigma of 0.004
 C57-C56 \\sim C57-C61 \\sim C57-C59 \\sim C57-C63 \\sim C57-C58 \\sim C57-C60
\\sim C57-C62
 with sigma of 0.002
 C75-C77 \\sim C75-C79 \\sim C77-C79 \\sim C74-C78 \\sim C74-C76 \\sim C78-C76
 with sigma of 0.004
 C73-C72 \\sim C73-C75 \\sim C73-C77 \\sim C73-C79 \\sim C73-C74 \\sim C73-C78
\\sim C73-C76
 with sigma of 0.002
 C92-C93 \\sim C92-C96 \\sim C93-C96 \\sim C94-C91 \\sim C94-C95 \\sim C91-C95
 with sigma of 0.004
 C90-C89 \\sim C90-C92 \\sim C90-C93 \\sim C90-C96 \\sim C90-C94 \\sim C90-C91
\\sim C90-C95
 with sigma of 0.002
 C86-C88 \\sim C86-C84 \\sim C88-C84 \\sim C85-C83 \\sim C85-C87 \\sim C83-C87
 with sigma of 0.004
 C81-C80 \\sim C81-C86 \\sim C81-C88 \\sim C81-C84 \\sim C81-C85 \\sim C81-C83
\\sim C81-C87
 with sigma of 0.002
3. Rigid body (RIGU) restrains
 C10, C11, C13, C15, C12, C14, C16
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C36, C37, C39, C41, C38, C40, C42
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C65, C66, C68, C70, C67, C69, C71
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C98, C100, C102, C104, C99, C101, C103
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C2, C4, C6, C8, C3, C5, C7
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C28, C29, C31, C33, C30, C32, C34
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C44, C45, C47, C49, C46, C48, C50
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C57, C59, C61, C63, C58, C60, C62
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C73, C75, C77, C79, C74, C76, C78
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C90, C92, C93, C96, C91, C94, C95
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C81, C84, C86, C88, C83, C85, C87
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C26, C23, C24, C25
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Others
 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(1)
 Sof(C11)=Sof(H11J)=Sof(H11K)=Sof(H11L)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=
 Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=FVAR(1)
 Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=
 Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(H42C)=1-FVAR(2)
 Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(H37C)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=
 Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=FVAR(2)
 Sof(C67)=Sof(H67A)=Sof(H67B)=Sof(H67C)=Sof(C69)=Sof(H69A)=Sof(H69B)=Sof(H69C)=
 Sof(C71)=Sof(H71A)=Sof(H71B)=Sof(H71C)=1-FVAR(3)
 Sof(C66)=Sof(H66A)=Sof(H66B)=Sof(H66C)=Sof(C68)=Sof(H68A)=Sof(H68B)=Sof(H68C)=
 Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(H70C)=FVAR(3)
 Sof(C99)=Sof(H99A)=Sof(H99B)=Sof(H99C)=Sof(C101)=Sof(H10S)=Sof(H10T)=
 Sof(H10U)=Sof(C103)=Sof(H10V)=Sof(H10W)=Sof(H10X)=1-FVAR(4)
 Sof(C100)=Sof(H10J)=Sof(H10K)=Sof(H10L)=Sof(C102)=Sof(H10M)=Sof(H10N)=
 Sof(H10O)=Sof(C104)=Sof(H10P)=Sof(H10Q)=Sof(H10R)=FVAR(4)
 Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=Sof(C7)=
 Sof(H7A)=Sof(H7B)=Sof(H7C)=1-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)=FVAR(5)
 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(6)
 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(6)
 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(7)
 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(7)
 Sof(C58)=Sof(H58A)=Sof(H58B)=Sof(H58C)=Sof(C60)=Sof(H60A)=Sof(H60B)=Sof(H60C)=
 Sof(C62)=Sof(H62A)=Sof(H62B)=Sof(H62C)=1-FVAR(8)
 Sof(C59)=Sof(H59A)=Sof(H59B)=Sof(H59C)=Sof(C61)=Sof(H61A)=Sof(H61B)=Sof(H61C)=
 Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(H63C)=FVAR(8)
 Sof(C74)=Sof(H74A)=Sof(H74B)=Sof(H74C)=Sof(C76)=Sof(H76A)=Sof(H76B)=Sof(H76C)=
 Sof(C78)=Sof(H78A)=Sof(H78B)=Sof(H78C)=1-FVAR(9)
 Sof(C75)=Sof(H75A)=Sof(H75B)=Sof(H75C)=Sof(C77)=Sof(H77A)=Sof(H77B)=Sof(H77C)=
 Sof(C79)=Sof(H79A)=Sof(H79B)=Sof(H79C)=FVAR(9)
 Sof(C91)=Sof(H91A)=Sof(H91B)=Sof(H91C)=Sof(C94)=Sof(H94A)=Sof(H94B)=Sof(H94C)=
 Sof(C95)=Sof(H95A)=Sof(H95B)=Sof(H95C)=1-FVAR(10)
 Sof(C92)=Sof(H92A)=Sof(H92B)=Sof(H92C)=Sof(C93)=Sof(H93A)=Sof(H93B)=Sof(H93C)=
 Sof(C96)=Sof(H96A)=Sof(H96B)=Sof(H96C)=FVAR(10)
 Sof(C83)=Sof(H83A)=Sof(H83B)=Sof(H83C)=Sof(C85)=Sof(H85A)=Sof(H85B)=Sof(H85C)=
 Sof(C87)=Sof(H87A)=Sof(H87B)=Sof(H87C)=1-FVAR(11)
 Sof(C84)=Sof(H84A)=Sof(H84B)=Sof(H84C)=Sof(C86)=Sof(H86A)=Sof(H86B)=Sof(H86C)=
 Sof(C88)=Sof(H88A)=Sof(H88B)=Sof(H88C)=FVAR(11)
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), C53(H53A,H53B,H53C), C55(H55A,
 H55B,H55C), C107(H10A,H10B,H10C), C108(H10D,H10E,H10F), C109(H10G,H10H,H10I),
 C112(H11A,H11B,H11C), C113(H11D,H11E,H11F), C114(H11G,H11H,H11I), C4(H4A,H4B,
 H4C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C11(H11J,H11K,H11L), C13(H13A,H13B,
 H13C), C15(H15A,H15B,H15C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C33(H33A,
 H33B,H33C), C37(H37A,H37B,H37C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C),
 C45(H45A,H45B,H45C), C47(H47A,H47B,H47C), C49(H49A,H49B,H49C), C59(H59A,H59B,
 H59C), C61(H61A,H61B,H61C), C63(H63A,H63B,H63C), C66(H66A,H66B,H66C), C68(H68A,
 H68B,H68C), C70(H70A,H70B,H70C), C75(H75A,H75B,H75C), C77(H77A,H77B,H77C),
 C79(H79A,H79B,H79C), C84(H84A,H84B,H84C), C86(H86A,H86B,H86C), C88(H88A,H88B,
 H88C), C92(H92A,H92B,H92C), C93(H93A,H93B,H93C), C96(H96A,H96B,H96C),
 C100(H10J,H10K,H10L), C102(H10M,H10N,H10O), C104(H10P,H10Q,H10R), C3(H3A,H3B,
 H3C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C12(H12A,H12B,H12C), C14(H14A,H14B,
 H14C), C16(H16A,H16B,H16C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C34(H34A,
 H34B,H34C), C38(H38A,H38B,H38C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C),
 C46(H46A,H46B,H46C), C50(H50A,H50B,H50C), C58(H58A,H58B,H58C), C60(H60A,H60B,
 H60C), C62(H62A,H62B,H62C), C67(H67A,H67B,H67C), C69(H69A,H69B,H69C), C71(H71A,
 H71B,H71C), C74(H74A,H74B,H74C), C76(H76A,H76B,H76C), C78(H78A,H78B,H78C),
 C83(H83A,H83B,H83C), C85(H85A,H85B,H85C), C87(H87A,H87B,H87C), C91(H91A,H91B,
 H91C), C94(H94A,H94B,H94C), C95(H95A,H95B,H95C), C99(H99A,H99B,H99C),
 C101(H10S,H10T,H10U), C103(H10V,H10W,H10X)
5.b Idealised Me refined as rotating group:
 C54(H54A,H54B,H54C), C48(H48A,H48B,H48C)
;
_shelx_res_checksum              89102
_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 1.426
_oxdiff_exptl_absorpt_empirical_full_min 0.559