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_7118745
_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         'C120 H176 O18 Ti4, 4(C4 H8 O)'
_chemical_formula_sum            'C140 H216 O23 Ti4'
_chemical_formula_weight         2458.73
_chemical_name_systematic        Ti4TBC[8](OC3H7)4(THF)2
_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             2015-11-04
_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                77.940(9)
_cell_angle_beta                 70.572(8)
_cell_angle_gamma                63.959(8)
_cell_formula_units_Z            1
_cell_length_a                   14.496(2)
_cell_length_b                   16.122(2)
_cell_length_c                   17.367(3)
_cell_measurement_temperature    100(2)
_cell_volume                     3429.6(9)
_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 0.980
_diffrn_measured_fraction_theta_max 0.980
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.1239
_diffrn_reflns_av_unetI/netI     0.1844
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            37038
_diffrn_reflns_theta_full        23.28
_diffrn_reflns_theta_max         23.28
_diffrn_reflns_theta_min         1.25
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.290
_exptl_absorpt_correction_T_max  0.9455
_exptl_absorpt_correction_T_min  0.9274
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Brucker-SADABS
_exptl_crystal_colour            'clear reddish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.191
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.489
_refine_diff_density_min         -1.218
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     668
_refine_ls_number_reflns         9666
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.1810
_refine_ls_R_factor_gt           0.0921
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1278P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2162
_refine_ls_wR_factor_ref         0.2501
_reflns_number_gt                4827
_reflns_number_total             9666
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6cc00478d2.cif
_cod_data_source_block           final
_cod_depositor_comments
'Adding full bibliography for 7118743--7118745.cif.'
_cod_original_cell_volume        3429.5(9)
_cod_database_code               7118745
_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. Uiso/Uaniso restraints and constraints
Uanis(O100) = Uanis(C103) = Uanis(C102) = Uanis(C101) = Uanis(C100)
Uanis(C109) = Uanis(C108) = Uanis(C107) = Uanis(C106) = Uanis(O102)
Uanis(C16) = Uanis(C17) = Uanis(C12) = Uanis(C13) = Uanis(C14) = Uanis(C15)
3.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C22(H22A,H22B), C33(H33A,H33B), C44(H44A,H44B), C45(H45A,
 H45B), C46(H46A,H46B), C48(H48A,H48B), C49(H49A,H49B), C51(H51A,H51B),
 C52(H52A,H52B), C54(H54A,H54B), C55(H55A,H55B), C56(H56A,H56B), C57(H57A,H57B),
  C58(H58A,H58B), C59(H59A,H59B), C100(H10D,H10E), C101(H10F,H10G), C102(H10H,
 H10I), C103(H10J,H10K), C106(H10L,H10M), C107(H10N,H10O), C108(H10P,H10Q),
 C109(H10R,H10S)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C13(H13), C15(H15), C24(H24), C26(H26), C35(H35), C37(H37)
3.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), 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), C47(H47A,H47B,H47C), C50(H50A,H50B,H50C), C53(H53A,H53B,H53C),
 C60(H60A,H60B,H60C)
;
_olex2_exptl_crystal_mounting_method
'Crystal was mounted on a loop using paratone oil. '
_olex2_submission_original_sample_id X8
_olex2_submission_special_instructions 'No special instructions were received'