M8L12 cubic cages with all facial delta or facial lamda configuration: effects of surface anions on the occupancy of the cage and anion exchange
Jing Yang; Xiao-Yong Chang; Kiu-Chor Sham; Shek-Man Yiu; Hoi-Lun Kwong; Chi-Ming Che; Chem.Commun. 52 (2016) 5981–; doi:

data_7119036
_publ_section_title
;
 M8L12 cubic cages with all facial delta or facial lamda configuration:
 effects of surface anions on the occupancy of the cage and anion exchange
;
_journal_name_full               Chem.Commun.
_journal_page_first              5981
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C216 H240 Cd8 N72, 16(C F3 O3 S)'
_chemical_formula_sum            'C232 H240 Cd8 F48 N72 O48 S16'
_chemical_formula_weight         7129.11
_space_group_crystal_system      cubic
_space_group_IT_number           205
_space_group_name_Hall           '-P 2ac 2ab 3'
_space_group_name_H-M_alt        'P a -3'
_symmetry_space_group_name_Hall  '-P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P a -3'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-01-15
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2015.11.10 svn.r3248 for OlexSys, GUI svn.r5133)
;
_audit_update_record
;
2016-02-22 deposited with the CCDC.
2016-03-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   41.313(5)
_cell_length_b                   41.313(5)
_cell_length_c                   41.313(5)
_cell_measurement_reflns_used    2278
_cell_measurement_temperature    100
_cell_measurement_theta_max      20
_cell_measurement_theta_min      4
_cell_volume                     70512(15)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Mar CCD'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_wavelength     0.780
_diffrn_reflns_av_unetI/netI     0.1354
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_number            24838
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        27.905
_diffrn_reflns_theta_max         29.761
_diffrn_reflns_theta_min         0.937
_diffrn_source                   'synchrotron radiation'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.850
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_description       block
_exptl_crystal_F_000             28736
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.5
_refine_diff_density_max         1.581
_refine_diff_density_min         -0.888
_refine_diff_density_rms         0.152
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1380
_refine_ls_number_reflns         24838
_refine_ls_number_restraints     654
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.1477
_refine_ls_R_factor_gt           0.1226
_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^)+(0.2000P)^2^+90.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3474
_refine_ls_wR_factor_ref         0.3748
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                15830
_reflns_number_total             24838
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc01635a2.cif
_cod_data_source_block           cd2
_cod_original_cell_volume        70513(25)
_cod_database_code               7119036
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 S1-O1 = S1-O2 = S1-O3
 1.44 with sigma of 0.02
 F2-C1 = F1-C1 = F3-C1
 1.34 with sigma of 0.02
 S1-C1
 1.82 with sigma of 0.02
 F20-C7 = F21-C7 = F19-C7
 1.34 with sigma of 0.02
 S7-C7
 1.82 with sigma of 0.02
 O19-S7
 1.44 with sigma of 0.02
 S7-O20
 1.44 with sigma of 0.02
 N12-C45 = N12-C43
 1.38 with sigma of 0.02
 C45-C44
 1.41 with sigma of 0.02
 N11-C44 = N11-C43
 1.36 with sigma of 0.02
 N14-C50
 1.38 with sigma of 0.02
 C49-C48
 1.41 with sigma of 0.02
 N19-C66 = N19-C68
 1.38 with sigma of 0.02
 C67-C66
 1.41 with sigma of 0.02
 N20-C68 = N20-C67
 1.36 with sigma of 0.02
 N17-C62 = N17-C61
 1.36 with sigma of 0.02
 N18-C61 = N18-C63
 1.38 with sigma of 0.02
 N12-C46 = N1-C11 = N7-C29 = N13-C47 = N6-C28 = N19-C65 = N24-C82 = N18-C64
 1.48 with sigma of 0.02
 O2-C1
 2.56 with sigma of 0.03
 C1-O3
 2.56 with sigma of 0.03
 O1-C1
 2.56 with sigma of 0.03
 F2-S1
 2.6 with sigma of 0.03
 F3-S1
 2.6 with sigma of 0.03
 F1-S1
 2.6 with sigma of 0.03
 F2-F1
 2.18 with sigma of 0.03
 F1-F3
 2.18 with sigma of 0.03
 F2-F3
 2.18 with sigma of 0.03
 O1-O2
 2.45 with sigma of 0.03
 O2-O3
 2.45 with sigma of 0.03
 O1-O3
 2.45 with sigma of 0.03
 F20-F21
 2.18 with sigma of 0.04
 F19-F21
 2.18 with sigma of 0.04
 F19-F20
 2.18 with sigma of 0.04
 F21-S7
 2.6 with sigma of 0.04
 S7-F19
 2.6 with sigma of 0.04
 F20-S7
 2.6 with sigma of 0.04
 O20-O19
 2.45 with sigma of 0.04
 C2-O5
 2.5 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
S2 \\sim O4 \\sim O5 \\sim O6 \\sim C2 \\sim F4 \\sim F5 \\sim F6: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02
F18 \\sim S6 \\sim O16 \\sim O17 \\sim O18 \\sim C6 \\sim F16 \\sim F17: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02
S1 \\sim O1 \\sim O2 \\sim O3 \\sim C1 \\sim F1 \\sim F2 \\sim F3: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02
S3 \\sim O7 \\sim O8 \\sim O9 \\sim C3 \\sim F7 \\sim F8 \\sim F9: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02
S5 \\sim O13 \\sim O14 \\sim O15 \\sim C5 \\sim F13 \\sim F14 \\sim F15: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02
S4 \\sim O12 \\sim O11 \\sim O10 \\sim F11 \\sim C4 \\sim F12 \\sim F10: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02
S7 \\sim O19 \\sim C7 \\sim F21 \\sim F20 \\sim F19 \\sim O20: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
4. Same fragment restrains
{S1, O1, O2, O3, C1, F1, F2, F3} sigma for 1-2: 0.02, 1-3: 0.04
as
{S2, O4, O5, O6, C2, F4, F5, F6}
{S1, O1, O2, O3, C1, F1, F2, F3} sigma for 1-2: 0.02, 1-3: 0.04
as
{S3, O7, O8, O9, C3, F7, F8, F9}
{S1, O1, O2, O3, C1, F1, F2, F3} sigma for 1-2: 0.02, 1-3: 0.04
as
{S4, O10, O11, O12, C4, F10, F11, F12}
{S1, O1, O2, O3, C1, F1, F2, F3} sigma for 1-2: 0.02, 1-3: 0.04
as
{S5, O13, O14, O15, C5, F13, F14, F15}
{S1, O1, O2, O3, C1, F1, F2, F3} sigma for 1-2: 0.02, 1-3: 0.04
as
{S6, O16, O17, O18, C6, F16, F17, F18}
5. Others
 Fixed Sof: S3(0.5) O7(0.5) O8(0.5) O9(0.5) C3(0.5) F7(0.5) F8(0.5) F9(0.5)
 S6(0.5) O16(0.5) O17(0.5) O18(0.5) C6(0.5) F16(0.5) F17(0.5) F18(0.5)
 C7(0.33333) F21(0.33333) F20(0.33333) F19(0.33333) O20(0.66667)
6.a Secondary CH2 refined with riding coordinates:
 C52(H52A,H52B), C59(H59A,H59B), C23(H23A,H23B), C70(H70A,H70B), C41(H41A,
 H41B), C34(H34A,H34B), C77(H77A,H77B), C16(H16A,H16B)
6.b Aromatic/amide H refined with riding coordinates:
 C37(H37), C31(H31), C40(H40), C30(H30), C42(H42), C24(H24), C54(H54),
 C33(H33), C13(H13), C73(H73), C15(H15), C19(H19), C76(H76), C49(H49), C74(H74),
  C26(H26), C78(H78), C36(H36), C72(H72), C48(H48), C51(H51), C63(H63),
 C62(H62), C66(H66), C45(H45), C58(H58), C69(H69), C57(H57), C22(H22), C60(H60),
  C38(H38), C56(H56), C12(H12), C18(H18), C81(H81), C20(H20), C27(H27),
 C67(H67), C44(H44), C80(H80)
6.c Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C11(H11A,H11B,H11C), C47(H47A,H47B,H47C), C46(H46A,H46B,
 H46C), C29(H29A,H29B,H29C), C82(H82A,H82B,H82C), C64(H64A,H64B,H64C), C65(H65A,
 H65B,H65C)
;
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              74799
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'