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_7700812
_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, 0.79(H2 S)'
_chemical_formula_sum            'C80 H145.57 Cr8 F8 O32 S0.78'
_chemical_formula_weight         2212.69
_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   mixed
_audit_creation_date             2019-06-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-06-05 deposited with the CCDC.    2019-08-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.3334(15)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.8280(4)
_cell_length_b                   16.46848(17)
_cell_length_c                   43.7202(6)
_cell_measurement_reflns_used    56834
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      44.1420
_cell_measurement_theta_min      2.2350
_cell_volume                     23358.1(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14d (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14d (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14d (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)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.998
_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    -28.00  14.50   0.50    2.00    --    0.00  57.00 -90.00   85
  2  \w     34.00  86.50   0.50    2.00    --    0.00  57.00   0.00  105
  3  \w     53.00  81.50   0.50    2.00    --    0.00  57.00 -90.00   57
  4  \w    -27.00   3.50   0.50    2.00    --    0.00  57.00   0.00   61
  5  \w    -64.00  24.50   0.50   10.00    --  -63.70  57.00-180.00  177
  6  \w   -150.00 -52.50   0.50   10.00    --  -63.70 -57.00  90.00  195
  7  \w   -153.00 -43.50   0.50   10.00    --  -63.70 -57.00  60.00  219
  8  \w    -52.00 -27.50   0.50   10.00    --  -63.70  57.00  60.00   49
  9  \w   -100.00  18.50   0.50   10.00    --  -63.70  76.00 -60.00  237
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_av_unetI/netI     0.0540
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       69
_diffrn_reflns_limit_h_min       -69
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       86
_diffrn_reflns_limit_l_min       -87
_diffrn_reflns_number            322797
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         45.294
_diffrn_reflns_theta_min         2.239
_exptl_absorpt_coefficient_mu    0.806
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66379
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14d (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_description       plank
_exptl_crystal_F_000             9265
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.304
_refine_diff_density_min         -0.836
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1339
_refine_ls_number_reflns         97655
_refine_ls_number_restraints     363
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0901
_refine_ls_R_factor_gt           0.0460
_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^)+(0.0558P)^2^+7.7954P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1067
_refine_ls_wR_factor_ref         0.1232
_reflns_Friedel_coverage         0.000
_reflns_number_gt                62047
_reflns_number_total             97655
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02378j2.cif
_cod_data_source_block           rrepw124
_cod_depositor_comments
'Adding full bibliography for 7700801--7700822.cif.'
_cod_database_code               7700812
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.924
_shelx_estimated_absorpt_t_min   0.855
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All S(H,H) groups
2. Restrained distances
 S1-H1B = S1-H1A
 1.3 with sigma of 0.02
 H1A-H1B
 1.95 with sigma of 0.002
 C78-C76 = C82-C76
 1.54 with sigma of 0.02
 C74-C70 \\sim C74-C72 \\sim C70-C72 \\sim C73-C71 \\sim C73-C69 \\sim C71-C69
 with sigma of 0.004
 C68-C67 \\sim C68-C74 \\sim C68-C70 \\sim C68-C72 \\sim C68-C73 \\sim C68-C71
\\sim C68-C69
 with sigma of 0.002
 C15-C13 \\sim C15-C17 \\sim C13-C17 \\sim C16-C14 \\sim C16-C18 \\sim C14-C18
 with sigma of 0.004
 C12-C11 \\sim C12-C15 \\sim C12-C13 \\sim C12-C17 \\sim C12-C16 \\sim C12-C14
\\sim C12-C18
 with sigma of 0.002
 C24-C26 \\sim C24-C22 \\sim C26-C22 \\sim C23-C21 \\sim C23-C25 \\sim C21-C25
 with sigma of 0.004
 C20-C19 \\sim C20-C24 \\sim C20-C26 \\sim C20-C22 \\sim C20-C23 \\sim C20-C21
\\sim C20-C25
 with sigma of 0.002
 S1-H1A \\sim H1AA-S1A
 with sigma of 0.02
 S1-H1B \\sim H1AA-H1AB
 with sigma of 0.02
 H1A-H1B \\sim S1A-H1AB
 with sigma of 0.04
 C78-C76 \\sim C77-C76A \\sim C82-C76 \\sim C81-C76A \\sim C79-C76A \\sim
C80-C76
 with sigma of 0.002
 C76A-C75A \\sim C76-C75
 with sigma of 0.002
 O27-C75 \\sim O27-C75A \\sim O28-C75A \\sim O28-C75
 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
C81 \\sim C82 \\sim C77 \\sim C78 \\sim C80 \\sim C79: within 2A with sigma of
0.002 and sigma for terminal atoms of 0.004
S1 \\sim S1A: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
C75 \\sim O27 \\sim O28: within 2A with sigma of 0.002 and sigma for terminal
atoms of 0.004
C76A \\sim C76: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
C75 \\sim C75A: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
4. Rigid body (RIGU) restrains
 C68, C70, C72, C74, C69, C71, C73
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C12, C13, C15, C17, C14, C16, C18
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C20, C22, C24, C26, C21, C23, C25
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C76, C78, C80, C82, C77, C79, C81
 with sigma for 1-2 distances of 0.0005 and sigma for 1-3 distances of 0.0005
 S1, O27, O28, C75, C76, C76A, C77, C78, C82, C81, C79, C80
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Sof(C77)=Sof(H77A)=Sof(H77B)=Sof(H77C)=Sof(C79)=Sof(H79A)=Sof(H79B)=Sof(H79C)=
 Sof(C81)=Sof(H81A)=Sof(H81B)=Sof(H81C)=Sof(C76A)=Sof(C75A)=1-FVAR(1)
 Sof(C75)=Sof(C76)=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(1)
 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(2)
 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(2)
 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(3)
 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(3)
 Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=
 Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=1-FVAR(4)
 Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=
 Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=FVAR(4)
 Sof(S1)=Sof(H1A)=Sof(H1B)=FVAR(5)
 Sof(S1A)=Sof(H1AA)=Sof(H1AB)=FVAR(6)
6.a Riding coordinates:
 S1(H1A,H1B), S1A(H1AA,H1AB)
6.b Me refined with riding coordinates:
 C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C22(H22A,H22B,
 H22C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C70(H70A,H70B,H70C), C72(H72A,
 H72B,H72C), C74(H74A,H74B,H74C), C78(H78A,H78B,H78C), C80(H80A,H80B,H80C),
 C82(H82A,H82B,H82C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C18(H18A,H18B,
 H18C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C69(H69A,
 H69B,H69C), C71(H71A,H71B,H71C), C73(H73A,H73B,H73C), C77(H77A,H77B,H77C),
 C79(H79A,H79B,H79C), C81(H81A,H81B,H81C)
6.c 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), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C),
 C31(H31A,H31B,H31C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,
 H36C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C44(H44A,
 H44B,H44C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), 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)
;
_shelx_res_checksum              56034
_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
;