Flexible macrocycles as versatile supports for catalytically active metal clusters.
Ryan, Jason D.; Gagnon, Kevin J.; Teat, Simon J.; McIntosh, Ruaraidh D.; Chemical communications (Cambridge, England) 52 (2016) 9071–9073; doi:10.1039/c6cc00478d

data_7118743
_publ_section_title
;
 Flexible macrocycles as versatile supports for catalytically active metal
 clusters.
;
_journal_issue                   58
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              9071
_journal_page_last               9073
_journal_paper_doi               10.1039/c6cc00478d
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C116 H152 Na6 O15, 5(C4 H8 O)'
_chemical_formula_sum            'C136 H191 Na6 O20'
_chemical_formula_weight         2283.83
_chemical_name_systematic        Na6TBC[8](THF)7.(THF)5
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-11-05
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-01-15 deposited with the CCDC.
2016-02-12 downloaded from the CCDC.
;
_cell_angle_alpha                83.835(6)
_cell_angle_beta                 84.664(6)
_cell_angle_gamma                61.434(4)
_cell_formula_units_Z            2
_cell_length_a                   17.7793(7)
_cell_length_b                   18.0796(7)
_cell_length_c                   22.8488(16)
_cell_measurement_temperature    100(2)
_cell_volume                     6405.9(6)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0698
_diffrn_reflns_av_unetI/netI     0.0893
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            85135
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.03
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_T_max  0.9934
_exptl_absorpt_correction_T_min  0.9832
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2466
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.277
_refine_diff_density_min         -1.303
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1309
_refine_ls_number_reflns         29328
_refine_ls_number_restraints     238
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1634
_refine_ls_R_factor_gt           0.1120
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1773P)^2^+10.3703P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3012
_refine_ls_wR_factor_ref         0.3388
_reflns_number_gt                17840
_reflns_number_total             29328
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6cc00478d2.cif
_cod_data_source_block           sodiumrm
_cod_depositor_comments
'Adding full bibliography for 7118743--7118745.cif.'
_cod_database_code               7118743
_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
 C53-C51 = C52-C51 = C54-C51 = C63-C62 = C65-C62 = C64-C62 = C76-C73 = C75-C73
 = C74-C73 = C86-C84 = C85-C84 = C87-C84 = C9-C7 = C7-C10 = C8-C7 = C21-C18 =
 C20-C18 = C19-C18 = C43-C40 = C41-C40 = C42-C40 = C32-C29 = C30-C29 = C31-C29 =
  C119-C118 = C121-C120 = C120-C119 = C218-C217 = C219-C218 = C220-C219 = C224-
 C223 = C223-C222 = C124-C123 = C123-C122 = C125-C124 = C117-C116 = C115-C113 =
 C114-C113 = C116-C115 = C112-C111 = C111-C110 = C110-C109 = C204-C203 = C203-
 C202 = C202-C201 = C222-C221 = C108-C107 = C107-C106 = C106-C105 = C206-C205 =
 C208-C207 = C207-C206 = C215-C214 = C211-C210 = C210-C209 = C214-C213 = C212-
 C211 = C216-C215 = C127-C126 = C128-C127 = C129-C128 = C102-C101 = C103-C102 =
 C104-C103
 1.54 with sigma of 0.02
 O104-C113 = O104-C117 = O205-C217 = O205-C220 = O106-C125 = O106-C122 = O107-
 C126 = O107-C129 = O203-C209 = O203-C212 = O204-C216 = O204-C213 = O206-C224 =
 O206-C221 = O202-C205 = O202-C208 = O201-C204 = O201-C201 = O101-C104 = O101-
 C101 = O102-C105 = O102-C108 = O105-C118 = O105-C121
 1.45 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O201) = Uanis(C201) = Uanis(C202) = Uanis(C203) = Uanis(C204)
Uanis(O202) = Uanis(C205) = Uanis(C206) = Uanis(C207) = Uanis(C208)
Uanis(O203) = Uanis(C209) = Uanis(C210) = Uanis(C211) = Uanis(C212) =
Uanis(O204) = Uanis(C213) = Uanis(C214) = Uanis(C215) = Uanis(C216)
Uanis(O205) = Uanis(C217) = Uanis(C218) = Uanis(C219) = Uanis(C220)
Uanis(O206) = Uanis(C221) = Uanis(C222) = Uanis(C223) = Uanis(C224)
Uanis(O105) = Uanis(C118) = Uanis(C119) = Uanis(C120) = Uanis(C121)
Uanis(O104) = Uanis(C117) = Uanis(C113) = Uanis(C116) = Uanis(C114) =
Uanis(C115)
Uanis(O101) = Uanis(C104) = Uanis(C101) = Uanis(C102) = Uanis(C103)
4. Same fragment restrains
{O101, C101, C102, C103, C104} sigma for 1-2: 0.02, 1-3: 0.04
as
{O102, C105, C106, C107, C108}
{O101, C101, C103, C104, C102} sigma for 1-2: 0.02, 1-3: 0.04
as
{O104, C113, C116, C117, C115}
{O101, C101, C102, C103, C104} sigma for 1-2: 0.02, 1-3: 0.04
as
{O105, C118, C119, C120, C121}
{O101, C101, C102, C103, C104} sigma for 1-2: 0.02, 1-3: 0.04
as
{O106, C122, C123, C124, C125}
{O101, C101, C102, C103, C104} sigma for 1-2: 0.02, 1-3: 0.04
as
{O107, C126, C127, C128, C129}
5. Others
 Fixed Sof: C115(0.75) C114(0.25) O204(0.5) C216(0.5) H21D(0.5) H21E(0.5)
 C215(0.5) H21F(0.5) H21G(0.5) C214(0.5) H21H(0.5) H21I(0.5) C213(0.5)
 H21J(0.5) H21K(0.5) O203(0.5) C210(0.5) H21R(0.5) H21S(0.5) C212(0.5)
 H21T(0.5) H21U(0.5) C209(0.5) H20L(0.5) H20M(0.5) C211(0.5) H21V(0.5) H21W(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C101(H10A,H10B), C102(H10C,H10D), C103(H10E,H10F), C104(H10G,H10H), C105(H10I,
 H10J), C106(H10K,H10L), C107(H10M,H10N), C108(H10O,H10P), C118(H11A,H11B),
 C119(H11C,H11D), C120(H12A,H12B), C121(H12C,H12D), C122(H12E,H12F), C123(H12G,
 H12H), C124(H12I,H12J), C125(H12K,H12L), C126(H12M,H12N), C127(H12O,H12P),
 C128(H12Q,H12R), C129(H12S,H12T), C11(H11E,H11F), C22(H22A,H22B), C33(H33A,
 H33B), C44(H44A,H44B), C55(H55A,H55B), C66(H66A,H66B), C77(H77A,H77B),
 C88(H88A,H88B), C112(H11G,H11H), C111(H11I,H11J), C110(H11K,H11L), C109(H10Q,
 H10R), C206(H20N,H20O), C208(H20P,H20Q), C207(H20R,H20S), C222(H22C,H22D),
 C224(H22E,H22F), C221(H22G,H22H), C223(H22I,H22J), C216(H21D,H21E), C215(H21F,
 H21G), C214(H21H,H21I), C213(H21J,H21K), C203(H20D,H20E), C202(H20F,H20G),
 C201(H20H,H20I), C204(H20J,H20K), C217(H21L,H21M), C218(H21N,H21O), C219(H21P,
 H21Q), C220(H22K,H22L), C210(H21R,H21S), C212(H21T,H21U), C209(H20L,H20M),
 C211(H21V,H21W)
6.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C3(H3), C16(H16), C14(H14), C25(H25), C27(H27), C36(H36), C38(H38),
 C47(H47), C49(H49), C58(H58), C60(H60), C69(H69), C71(H71), C80(H80), C82(H82),
  C205(H205)
6.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C30(H30A,H30B,
 H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C41(H41A,H41B,H41C), C42(H42A,
 H42B,H42C), C43(H43A,H43B,H43C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C),
 C54(H54A,H54B,H54C), C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C65(H65A,H65B,
 H65C), C74(H74A,H74B,H74C), C75(H75A,H75B,H75C), C76(H76A,H76B,H76C), C85(H85A,
 H85B,H85C), C86(H86A,H86B,H86C), C87(H87A,H87B,H87C), C8(H8A,H8B,H8C), C9(H9A,
 H9B,H9C), C10(H10S,H10T,H10U)
;
_olex2_exptl_crystal_mounting_method 'Mounted on loop using paratone oil'
_olex2_submission_original_sample_id sodiumRM
_olex2_submission_special_instructions 'No special instructions were received'