#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/36/7013622.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7013622
loop_
_publ_author_name
'Petrella, Antonella J.'
'Craig, Donald C.'
'Lamb, Robert N.'
'Raston, Colin L.'
'Roberts, Nicholas K.'
_publ_section_title
;
 A facile route to hetero-bimetallic Ti(iv)-alkali metal calix[4]arene
 complexes
;
_journal_issue                   24
_journal_name_full               'Dalton Transactions'
_journal_page_first              4590
_journal_paper_doi               10.1039/b310635g
_journal_year                    2003
_chemical_formula_moiety         'C44 H53 K O5 Ti,11(C H4 O)'
_chemical_formula_sum            'C55 H97 K O16 Ti'
_chemical_formula_weight         1101.4
_space_group_IT_number           97
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I 4 2'
_symmetry_space_group_name_H-M   'I 4 2 2'
_atom_type_scat_source
'International Tables for X-ray Crystallography, Vol. IV'
_audit_creation_method           'RAELSPUB and manual entry'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.558(3)
_cell_length_b                   15.558(3)
_cell_length_c                   26.922(8)
_cell_measurement_temperature    150
_cell_volume                     6517(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-II, (Johnson, 1976)'
_computing_publication_material  'Local programs'
_computing_structure_refinement  'RAELS, (Rae, 1989)'
_computing_structure_solution    'SIR92 (Altomare et al, 1994)'
_diffrn_ambient_temperature      150(2)
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.015
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2208
_diffrn_reflns_theta_max         22.6
_exptl_absorpt_coefficient_mu    0.248
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.12
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2384.0
_exptl_crystal_size_rad          0.1
_refine_diff_density_max         1.18
_refine_diff_density_min         -0.76
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.63
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     167
_refine_ls_number_reflns         1753
_refine_ls_R_factor_gt           0.125
_refine_ls_shift/su_max          0.004
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[σ²(F) + 0.0004F²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.176
_reflns_number_gt                1753
_reflns_number_total             2163
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b310635g.txt
_cod_data_source_block           AJP5
_cod_original_cell_volume        6517(4)
_cod_database_code               7013622
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,-y,z
3 -x,y,-z
4 x,-y,-z
5 y,x,-z
6 -y,-x,-z
7 -y,x,z
8 y,-x,z
9 1/2+x,1/2+y,1/2+z
10 1/2-x,1/2-y,1/2+z
11 1/2-x,1/2+y,1/2-z
12 1/2+x,1/2-y,1/2-z
13 1/2+y,1/2+x,1/2-z
14 1/2-y,1/2-x,1/2-z
15 1/2-y,1/2+x,1/2+z
16 1/2+y,1/2-x,1/2+z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_type_symbol
_atom_site_occupancy
Ti1 0.50000 0.50000 0.12663(8) 0.062(1) Uani Ti 1.0
O1 0.6233(3) 0.4992(5) 0.1421(2) 0.063(1) Uani O 1.0
O2 0.5000 0.5000 0.0651(3) 0.097(4) Uani O 1.0
C1 0.6679(3) 0.5020(6) 0.1853(2) 0.057(2) Uani C 1.0
C2 0.6905(5) 0.5793(5) 0.2076(2) 0.060(3) Uani C 1.0
C3 0.7361(4) 0.5786(6) 0.2521(3) 0.075(4) Uani C 1.0
C4 0.7596(3) 0.5018(6) 0.2748(2) 0.065(2) Uani C 1.0
C5 0.7364(4) 0.4251(4) 0.2519(3) 0.059(3) Uani C 1.0
C6 0.6908(4) 0.4246(5) 0.2073(3) 0.058(3) Uani C 1.0
C7 0.6623(7) 0.6620(7) 0.1857(3) 0.065(2) Uani C 1.0
C8 0.8091(5) 0.4937(7) 0.3242(3) 0.087(4) Uani C 1.0
C9 0.8857(9) 0.4395(12) 0.3184(7) 0.230(6) Uani C 1.0
C10 0.7542(10) 0.4552(12) 0.3625(5) 0.242(9) Uani C 1.0
C11 0.8367(11) 0.5787(8) 0.3416(6) 0.224(6) Uani C 1.0
K1 0.6085(3) 0.6085(3) 0.0000 0.094(2) Uani K 0.5
O1Me1 0.4090(9) 0.5911(9) 0.0000 0.094(2) Uani O 0.5
C1Me1 0.3519(21) 0.6392(23) 0.0262(10) 0.094(2) Uani C 0.5
O1Me2 0.2088(4) 0.0050(9) 0.4407(2) 0.156(4) Uani O 1.0
C1Me2 0.2956(5) 0.0118(27) 0.4284(4) 0.308(4) Uani C 1.0
O1Me3 0.4316(12) 0.5117(36) 0.3194(9) 0.170(7) Uani O 0.25
C1Me3 0.5000 0.5000 0.2871(6) 0.099(5) Uani C 1.0
O1Me4 0.7244(25) 0.7244(25) 0.0000 0.608(9) Uani O 1.0
C1Me4 0.7314(39) 0.7691(35) -0.0455(16) 0.321(9) Uani C 0.5
O1Me5 0.3909(14) 0.0000 0.0000 0.298(9) Uani O 1.0
C1Me5 0.3177(17) 0.0516(18) 0.0012(14) 0.237(9) Uani C 0.5
O1Me6 -0.0469(12) 0.1657(25) 0.0012(29) 0.343(9) Uani O 0.125
C1Me6 0.0469(12) 0.1657(25) -0.0012(29) 0.343(9) Uani C 0.125
O1Me7 0.5257(39) 0.5371(25) 0.4213(9) 0.265(9) Uani O 0.125
C1Me7 0.4743(39) 0.4629(25) 0.4213(9) 0.265(9) Uani C 0.125
HC3 0.7522 0.6343 0.2681 0.075 Uani H 1.0
HC5 0.7528 0.3693 0.2677 0.059 Uani H 1.0
H1C7 0.6564 0.6550 0.1490 0.065 Uani H 1.0
H2C7 0.7064 0.7069 0.1931 0.065 Uani H 1.0
H1C9 0.9166 0.4354 0.3509 0.249 Uani H 1.0
H2C9 0.8681 0.3808 0.3073 0.384 Uani H 1.0
H3C9 0.9247 0.4656 0.2930 0.383 Uani H 1.0
H1C10 0.7872 0.4504 0.3943 0.271 Uani H 1.0
H2C10 0.7025 0.4922 0.3679 0.398 Uani H 1.0
H3C10 0.7355 0.3967 0.3516 0.390 Uani H 1.0
H1C11 0.8687 0.5725 0.3736 0.248 Uani H 1.0
H2C11 0.8751 0.6056 0.3162 0.368 Uani H 1.0
H3C11 0.7852 0.6160 0.3469 0.377 Uani H 1.0
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
? ? ? ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ti1 O1 155.6(3) 1_555 1_555 2_665 no
O1 Ti1 O1 87.43(5) 1_555 1_555 7_655 no
O1 Ti1 O1 87.43(5) 1_555 1_555 8_565 no
O1 Ti1 O2 102.2(1) 1_555 1_555 1_555 no
O1 Ti1 O1 87.43(5) 2_665 1_555 7_655 no
O1 Ti1 O1 87.43(5) 2_665 1_555 8_565 no
O1 Ti1 O2 102.2(1) 2_665 1_555 1_555 no
O1 Ti1 O1 155.6(3) 7_655 1_555 8_565 no
O1 Ti1 O2 102.2(1) 7_655 1_555 1_555 no
O1 Ti1 O2 102.2(1) 8_565 1_555 1_555 no
Ti1 O1 C1 133.0(3) 1_555 1_555 1_555 no
Ti1 O2 K1 126.3(2) 1_555 1_555 1_555 no
Ti1 O2 K1 126.3(2) 1_555 1_555 2_665 no
K1 O2 K1 107.5(3) 1_555 1_555 2_665 no
O1 C1 C2 121.9(7) 1_555 1_555 1_555 no
O1 C1 C6 118.1(8) 1_555 1_555 1_555 no
C2 C1 C6 120.0(6) 1_555 1_555 1_555 no
C1 C2 C3 119.6(4) 1_555 1_555 1_555 no
C1 C2 C7 120.4(7) 1_555 1_555 1_555 no
C3 C2 C7 120.0(7) 1_555 1_555 1_555 no
C2 C3 C4 121.2(5) 1_555 1_555 1_555 no
C3 C4 C5 118.3(7) 1_555 1_555 1_555 no
C3 C4 C8 125.4(7) 1_555 1_555 1_555 no
C5 C4 C8 116.2(8) 1_555 1_555 1_555 no
C4 C5 C6 121.2(5) 1_555 1_555 1_555 no
C1 C6 C5 119.6(4) 1_555 1_555 1_555 no
C1 C6 C7 121.7(8) 1_555 1_555 8_565 no
C5 C6 C7 118.6(7) 1_555 1_555 8_565 no
C2 C7 C6 111.3(5) 1_555 1_555 7_655 no
C4 C8 C9 111.1(9) 1_555 1_555 1_555 no
C4 C8 C10 110.5(8) 1_555 1_555 1_555 no
C4 C8 C11 110.4(9) 1_555 1_555 1_555 no
C9 C8 C10 108.3(5) 1_555 1_555 1_555 no
C9 C8 C11 108.3(5) 1_555 1_555 1_555 no
C10 C8 C11 108.3(5) 1_555 1_555 1_555 no
O2 K1 O2 72.5(3) 1_555 1_555 3_655 no
O2 K1 O1Me1 51.8(3) 1_555 1_555 1_555 no
O2 K1 O1Me1 51.8(3) 1_555 1_555 2_665 no
O2 K1 O1Me1 36.3(2) 1_555 1_555 3_655 no
O2 K1 O1Me2 109.4(3) 1_555 1_555 9_554 no
O2 K1 O1Me2 68.1(2) 1_555 1_555 12_555 no
O2 K1 O1Me2 69.3(2) 1_555 1_555 13_555 no
O2 K1 O1Me2 106.9(3) 1_555 1_555 15_554 no
O2 K1 O1Me4 143.7(2) 1_555 1_555 1_555 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 O1 1.963(4) 1_555 1_555 no
Ti1 O1 1.963(4) 1_555 2_665 no
Ti1 O1 1.963(4) 1_555 7_655 no
Ti1 O1 1.963(4) 1_555 8_565 no
Ti1 O2 1.657(9) 1_555 1_555 no
O1 C1 1.355(8) 1_555 1_555 no
O2 K1 2.962(8) 1_555 1_555 no
O2 K1 2.962(8) 1_555 2_665 no
C1 C2 1.390(6) 1_555 1_555 no
C1 C6 1.390(6) 1_555 1_555 no
C2 C3 1.393(7) 1_555 1_555 no
C2 C7 1.481(14) 1_555 1_555 no
C3 C4 1.390(6) 1_555 1_555 no
C4 C5 1.390(6) 1_555 1_555 no
C4 C8 1.542(10) 1_555 1_555 no
C5 C6 1.393(7) 1_555 1_555 no
C6 C7 1.537(14) 1_555 8_565 no
C7 C6 1.537(14) 1_555 7_655 no
C8 C9 1.468(8) 1_555 1_555 no
C8 C10 1.468(8) 1_555 1_555 no
C8 C11 1.468(8) 1_555 1_555 no
K1 O1Me1 3.117(11) 1_555 1_555 no
K1 O1Me1 3.117(11) 1_555 2_665 no
K1 O1Me2 2.752(9) 1_555 9_554 no
K1 O1Me2 2.846(10) 1_555 12_555 no
K1 O1Me2 2.752(9) 1_555 13_555 no
K1 O1Me2 2.846(10) 1_555 15_554 no
K1 O1Me4 2.548(55) 1_555 1_555 no
O1Me1 C1Me1 1.358(12) 1_555 1_555 no
O1Me2 C1Me2 1.395(5) 1_555 1_555 no
O1Me3 C1Me3 1.386(10) 1_555 1_555 no
O1Me4 C1Me4 1.414(24) 1_555 1_555 no
O1Me5 C1Me5 1.393(15) 1_555 1_555 no
