#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/36/7013621.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_7013621
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         'C51 H67 Cs O8 Ti,4(C H4 O)'
_chemical_formula_sum            'C55 H83 Cs O12 Ti'
_chemical_formula_weight         1117.1
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 105.12(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.622(5)
_cell_length_b                   22.248(7)
_cell_length_c                   21.168(7)
_cell_measurement_reflns_used    983
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.38
_cell_measurement_theta_min      2.97
_cell_volume                     6193(4)
_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      273(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  0.030
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            29958
_diffrn_reflns_theta_max         27
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.761
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.20
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2344.0
_refine_diff_density_max         1.14
_refine_diff_density_min         -0.97
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.94
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     171
_refine_ls_number_reflns         6178
_refine_ls_R_factor_gt           0.061
_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         0.093
_reflns_number_gt                6178
_reflns_number_total             7399
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b310635g.txt
_cod_data_source_block           4
_cod_original_cell_volume        6193(6)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7013621
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 x,-y,1/2+z
3 -x,-y,-z
4 -x,y,1/2-z
5 1/2+x,1/2+y,z
6 1/2+x,1/2-y,1/2+z
7 1/2-x,1/2-y,-z
8 1/2-x,1/2+y,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
Cs1 0.00000 0.08120(2) 0.25000 0.0425(2) Uani Cs 1.0
Ti1 0.00000 -0.10089(4) 0.25000 0.0263(2) Uani Ti 1.0
O1 0.0757(2) -0.0460(1) 0.2193(1) 0.0277(3) Uani O 1.0
O2 -0.1038(2) -0.0956(1) 0.1645(1) 0.0293(3) Uani O 1.0
C1 0.1461(2) -0.0292(1) 0.1911(1) 0.0297(3) Uani C 1.0
C2 0.2452(2) -0.0164(1) 0.2289(1) 0.0339(3) Uani C 1.0
C3 0.3153(2) 0.0063(1) 0.1975(1) 0.0392(5) Uani C 1.0
C4 0.2911(2) 0.0170(1) 0.1302(1) 0.0389(6) Uani C 1.0
C5 0.1920(2) 0.0037(1) 0.0944(1) 0.0333(5) Uani C 1.0
C6 0.1188(2) -0.0191(1) 0.1231(1) 0.0296(3) Uani C 1.0
C7 0.2730(3) -0.0370(2) 0.3008(2) 0.0350(4) Uani C 1.0
C8 0.3728(6) 0.0365(5) 0.0969(5) 0.062(1) Uani C 0.5
C9 0.4361(11) -0.0177(10) 0.0869(13) 0.107(5) Uani C 0.5
C10 0.4436(14) 0.0828(9) 0.1389(11) 0.076(3) Uani C 0.5
C11 0.3241(17) 0.0645(14) 0.0302(8) 0.130(2) Uani C 0.5
C8' 0.3733(6) 0.0402(5) 0.0993(5) 0.061(1) Uani C 0.5
C9' 0.4520(10) -0.0089(10) 0.0999(13) 0.097(4) Uani C 0.5
C10' 0.4274(15) 0.0944(8) 0.1373(13) 0.085(3) Uani C 0.5
C11' 0.3267(17) 0.0592(14) 0.0285(7) 0.129(2) Uani C 0.5
C12 -0.1298(2) -0.0387(1) 0.1413(1) 0.0287(3) Uani C 1.0
C13 -0.0739(2) -0.0108(1) 0.1021(1) 0.0279(3) Uani C 1.0
C14 -0.1019(2) 0.0468(1) 0.0785(1) 0.0299(4) Uani C 1.0
C15 -0.1830(2) 0.0779(1) 0.0921(1) 0.0335(6) Uani C 1.0
C16 -0.2366(2) 0.0488(1) 0.1312(1) 0.0342(6) Uani C 1.0
C17 -0.2120(2) -0.0088(1) 0.1561(1) 0.0316(3) Uani C 1.0
C18 0.0150(3) -0.0417(2) 0.0853(2) 0.0281(3) Uani C 1.0
C19 -0.2129(3) 0.1414(2) 0.0632(2) 0.048(1) Uani C 1.0
C20 -0.1542(4) 0.1883(2) 0.1112(3) 0.090(2) Uani C 1.0
C21 -0.3267(3) 0.1529(3) 0.0527(3) 0.096(3) Uani C 1.0
C22 -0.1865(6) 0.1490(3) -0.0021(3) 0.137(5) Uani C 1.0
O1Ac 0.0754(4) -0.1664(3) 0.2208(2) 0.107(7) Uani O 1.0
C1Ac 0.0785(9) -0.2194(4) 0.2216(5) 0.191(9) Uani C 1.0
C2Ac 0.0000 -0.2481(5) 0.2500 0.222(9) Uani C 1.0
C3Ac 0.1563(11) -0.2526(6) 0.1967(7) 0.340(9) Uani C 1.0
O1Me1 0.1158(4) 0.1796(3) 0.2031(3) 0.103(2) Uani O 1.0
C1Me1 0.1696(8) 0.1524(5) 0.1616(5) 0.130(4) Uani C 1.0
O1Me2 0.2986(7) 0.3101(4) 0.1083(6) 0.199(5) Uani O 1.0
C1Me2 0.3610(10) 0.2866(7) 0.0699(6) 0.308(9) Uani C 1.0
O1Me3 0.1131(8) 0.2934(5) 0.1484(8) 0.192(7) Uani O 0.67
C1Me3 0.0522(15) 0.3207(8) 0.0913(8) 0.149(6) Uani C 0.67
O1Me3' 0.1088(19) 0.3011(6) 0.2520(14) 0.192(7) Uani O 0.33
C1Me3' 0.0741(26) 0.3598(9) 0.2593(19) 0.149(6) Uani C 0.33
HC3 0.3857 0.0155 0.2243 0.045 Uani H 1.0
HC5 0.1728 0.0109 0.0461 0.034 Uani H 1.0
H1C7 0.3463 -0.0272 0.3203 0.040 Uani H 1.0
H2C7 0.2631 -0.0815 0.3013 0.035 Uani H 1.0
H1C9 0.4893 -0.0044 0.0651 0.133 Uani H 0.5
H2C9 0.4696 -0.0360 0.1303 0.125 Uani H 0.5
H3C9 0.3909 -0.0481 0.0588 0.150 Uani H 0.5
H1C10 0.4966 0.0951 0.1165 0.092 Uani H 0.5
H2C10 0.4034 0.1188 0.1453 0.115 Uani H 0.5
H3C10 0.4773 0.0647 0.1824 0.086 Uani H 0.5
H1C11 0.3786 0.0770 0.0091 0.170 Uani H 0.5
H2C11 0.2786 0.0344 0.0018 0.160 Uani H 0.5
H3C11 0.2834 0.1005 0.0360 0.164 Uani H 0.5
H1C9' 0.5054 0.0068 0.0796 0.117 Uani H 0.5
H2C9' 0.4843 -0.0212 0.1461 0.112 Uani H 0.5
H3C9' 0.4179 -0.0444 0.0745 0.141 Uani H 0.5
H1C10' 0.4810 0.1091 0.1165 0.102 Uani H 0.5
H2C10' 0.3770 0.1272 0.1367 0.130 Uani H 0.5
H3C10' 0.4598 0.0823 0.1836 0.093 Uani H 0.5
H1C11' 0.3815 0.0743 0.0090 0.168 Uani H 0.5
H2C11' 0.2922 0.0240 0.0027 0.157 Uani H 0.5
H3C11' 0.2758 0.0919 0.0273 0.165 Uani H 0.5
HC14 -0.0623 0.0667 0.0507 0.031 Uani H 1.0
HC16 -0.2950 0.0702 0.1416 0.038 Uani H 1.0
H1C18 0.0086 -0.0356 0.0376 0.029 Uani H 1.0
H2C18 0.0111 -0.0856 0.0945 0.029 Uani H 1.0
H1C20 -0.1730 0.2294 0.0930 0.097 Uani H 1.0
H2C20 -0.1717 0.1842 0.1540 0.128 Uani H 1.0
H3C20 -0.0796 0.1818 0.1178 0.161 Uani H 1.0
H1C21 -0.3437 0.1940 0.0340 0.103 Uani H 1.0
H2C21 -0.3662 0.1223 0.0216 0.169 Uani H 1.0
H3C21 -0.3446 0.1498 0.0954 0.135 Uani H 1.0
H1C22 -0.2065 0.1902 -0.0197 0.164 Uani H 1.0
H2C22 -0.1116 0.1436 0.0044 0.197 Uani H 1.0
H3C22 -0.2239 0.1184 -0.0339 0.196 Uani H 1.0
HC2Ac 0.0000 -0.2924 0.2500 0.335 Uani H 1.0
H1C3Ac 0.1470 -0.2968 0.2012 0.439 Uani H 1.0
H2C3Ac 0.1479 -0.2425 0.1495 0.365 Uani H 1.0
H3C3Ac 0.2259 -0.2407 0.2226 0.364 Uani H 1.0
H1O1Me1 0.1149 0.2205 0.1834 0.103 Uani H 1.0
H1C1Me1 0.2444 0.1567 0.1814 0.130 Uani H 1.0
H2C1Me1 0.1517 0.1088 0.1563 0.130 Uani H 1.0
H3C1Me1 0.1507 0.1725 0.1178 0.130 Uani H 1.0
H1O1Me2 0.3362 0.3464 0.1299 0.199 Uani H 1.0
H1C1Me2 0.4290 0.3067 0.0825 0.308 Uani H 1.0
H2C1Me2 0.3697 0.2424 0.0775 0.308 Uani H 1.0
H3C1Me2 0.3281 0.2943 0.0225 0.308 Uani H 1.0
H1O1Me3 0.1773 0.2992 0.1346 0.192 Uani H 1.0
H1C1Me3 0.0548 0.3653 0.0967 0.149 Uani H 1.0
H2C1Me3 0.0783 0.3094 0.0529 0.149 Uani H 1.0
H3C1Me3 -0.0197 0.3066 0.0838 0.149 Uani H 1.0
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 Cs1 O1 51.12(9) 1_555 1_555 4_555 no
O1 Cs1 O1Me1 111.0(1) 1_555 1_555 1_555 no
O1 Cs1 O1Me1 162.1(1) 1_555 1_555 4_555 no
O1 Cs1 O1Me1 162.1(1) 4_555 1_555 1_555 no
O1 Cs1 O1Me1 111.0(1) 4_555 1_555 4_555 no
O1Me1 Cs1 O1Me1 86.8(2) 1_555 1_555 4_555 no
O1 Ti1 O1 95.9(2) 1_555 1_555 4_555 no
O1 Ti1 O2 88.3(1) 1_555 1_555 1_555 no
O1 Ti1 O2 87.2(1) 1_555 1_555 4_555 no
O1 Ti1 O1Ac 89.7(2) 1_555 1_555 1_555 no
O1 Ti1 O1Ac 174.4(2) 1_555 1_555 4_555 no
O1 Ti1 O2 87.2(1) 4_555 1_555 1_555 no
O1 Ti1 O2 88.3(1) 4_555 1_555 4_555 no
O1 Ti1 O1Ac 174.4(2) 4_555 1_555 1_555 no
O1 Ti1 O1Ac 89.7(2) 4_555 1_555 4_555 no
O2 Ti1 O2 173.2(2) 1_555 1_555 4_555 no
O2 Ti1 O1Ac 93.6(1) 1_555 1_555 1_555 no
O2 Ti1 O1Ac 91.4(1) 1_555 1_555 4_555 no
O2 Ti1 O1Ac 91.4(1) 4_555 1_555 1_555 no
O2 Ti1 O1Ac 93.6(1) 4_555 1_555 4_555 no
O1Ac Ti1 O1Ac 84.7(4) 1_555 1_555 4_555 no
Cs1 O1 Ti1 106.5(1) 1_555 1_555 1_555 no
Cs1 O1 C1 99.0(2) 1_555 1_555 1_555 no
Ti1 O1 C1 154.5(2) 1_555 1_555 1_555 no
Ti1 O2 C12 115.9(2) 1_555 1_555 1_555 no
O1 C1 C2 120.4(2) 1_555 1_555 1_555 no
O1 C1 C6 118.8(2) 1_555 1_555 1_555 no
C2 C1 C6 120.5(2) 1_555 1_555 1_555 no
C1 C2 C3 118.5(2) 1_555 1_555 1_555 no
C1 C2 C7 117.1(3) 1_555 1_555 1_555 no
C3 C2 C7 123.9(2) 1_555 1_555 1_555 no
C2 C3 C4 122.7(2) 1_555 1_555 1_555 no
C3 C4 C5 117.1(2) 1_555 1_555 1_555 no
C3 C4 C8 120.9(4) 1_555 1_555 1_555 no
C3 C4 C8' 119.4(4) 1_555 1_555 1_555 no
C5 C4 C8 121.8(4) 1_555 1_555 1_555 no
C5 C4 C8' 123.5(4) 1_555 1_555 1_555 no
C4 C5 C6 122.7(2) 1_555 1_555 1_555 no
C1 C6 C5 118.5(2) 1_555 1_555 1_555 no
C1 C6 C18 116.6(2) 1_555 1_555 1_555 no
C5 C6 C18 124.4(2) 1_555 1_555 1_555 no
C2 C7 C17 116.0(3) 1_555 1_555 4_555 no
C4 C8 C9 110.2(5) 1_555 1_555 1_555 no
C4 C8 C10 110.4(3) 1_555 1_555 1_555 no
C4 C8 C11 110.5(3) 1_555 1_555 1_555 no
C9 C8 C10 108.6(2) 1_555 1_555 1_555 no
C9 C8 C11 108.6(2) 1_555 1_555 1_555 no
C10 C8 C11 108.6(2) 1_555 1_555 1_555 no
C4 C8' C9' 110.2(5) 1_555 1_555 1_555 no
C4 C8' C10' 110.4(3) 1_555 1_555 1_555 no
C4 C8' C11' 110.5(4) 1_555 1_555 1_555 no
C9' C8' C10' 108.6(2) 1_555 1_555 1_555 no
C9' C8' C11' 108.6(2) 1_555 1_555 1_555 no
C10' C8' C11' 108.6(2) 1_555 1_555 1_555 no
O2 C12 C13 119.2(2) 1_555 1_555 1_555 no
O2 C12 C17 120.2(2) 1_555 1_555 1_555 no
C13 C12 C17 120.5(2) 1_555 1_555 1_555 no
C12 C13 C14 118.5(2) 1_555 1_555 1_555 no
C12 C13 C18 121.9(2) 1_555 1_555 1_555 no
C14 C13 C18 119.6(2) 1_555 1_555 1_555 no
C13 C14 C15 122.7(2) 1_555 1_555 1_555 no
C14 C15 C16 117.1(2) 1_555 1_555 1_555 no
C14 C15 C19 120.8(2) 1_555 1_555 1_555 no
C16 C15 C19 122.1(2) 1_555 1_555 1_555 no
C15 C16 C17 122.7(2) 1_555 1_555 1_555 no
C7 C17 C12 122.0(3) 4_555 1_555 1_555 no
C7 C17 C16 119.5(3) 4_555 1_555 1_555 no
C12 C17 C16 118.5(2) 1_555 1_555 1_555 no
C6 C18 C13 114.7(3) 1_555 1_555 1_555 no
C15 C19 C20 108.8(3) 1_555 1_555 1_555 no
C15 C19 C21 111.3(3) 1_555 1_555 1_555 no
C15 C19 C22 111.1(3) 1_555 1_555 1_555 no
C20 C19 C21 108.6(2) 1_555 1_555 1_555 no
C20 C19 C22 108.6(2) 1_555 1_555 1_555 no
C21 C19 C22 108.6(2) 1_555 1_555 1_555 no
Ti1 O1Ac C1Ac 138.9(9) 1_555 1_555 1_555 no
O1Ac C1Ac C2Ac 113.8(10) 1_555 1_555 1_555 no
O1Ac C1Ac C3Ac 121.0(10) 1_555 1_555 1_555 no
C2Ac C1Ac C3Ac 125.2(7) 1_555 1_555 1_555 no
C1Ac C2Ac C1Ac 129.6(9) 1_555 1_555 4_555 no
Cs1 O1Me1 C1Me1 107.1(6) 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
Cs1 O1 3.137(3) 1_555 1_555 no
Cs1 O1 3.137(3) 1_555 4_555 no
Cs1 O1Me1 3.014(5) 1_555 1_555 no
Cs1 O1Me1 3.014(5) 1_555 4_555 no
Ti1 O1 1.823(3) 1_555 1_555 no
Ti1 O1 1.823(3) 1_555 4_555 no
Ti1 O2 1.989(2) 1_555 1_555 no
Ti1 O2 1.989(2) 1_555 4_555 no
Ti1 O1Ac 1.973(4) 1_555 1_555 no
Ti1 O1Ac 1.973(4) 1_555 4_555 no
O1 C1 1.311(4) 1_555 1_555 no
O2 C12 1.371(4) 1_555 1_555 no
C1 C2 1.407(2) 1_555 1_555 no
C1 C6 1.407(2) 1_555 1_555 no
C2 C3 1.393(3) 1_555 1_555 no
C2 C7 1.539(4) 1_555 1_555 no
C3 C4 1.397(2) 1_555 1_555 no
C4 C5 1.397(2) 1_555 1_555 no
C4 C8 1.527(4) 1_555 1_555 no
C4 C8' 1.527(4) 1_555 1_555 no
C5 C6 1.393(3) 1_555 1_555 no
C6 C18 1.517(4) 1_555 1_555 no
C7 C17 1.520(4) 1_555 4_555 no
C8 C9 1.528(3) 1_555 1_555 no
C8 C10 1.528(3) 1_555 1_555 no
C8 C11 1.528(3) 1_555 1_555 no
C8' C9' 1.528(3) 1_555 1_555 no
C8' C10' 1.528(3) 1_555 1_555 no
C8' C11' 1.528(3) 1_555 1_555 no
C12 C13 1.407(2) 1_555 1_555 no
C12 C17 1.407(2) 1_555 1_555 no
C13 C14 1.393(3) 1_555 1_555 no
C13 C18 1.513(4) 1_555 1_555 no
C14 C15 1.397(2) 1_555 1_555 no
C15 C16 1.397(2) 1_555 1_555 no
C15 C19 1.549(5) 1_555 1_555 no
C16 C17 1.393(3) 1_555 1_555 no
C17 C7 1.520(4) 1_555 4_555 no
C19 C20 1.528(3) 1_555 1_555 no
C19 C21 1.528(3) 1_555 1_555 no
C19 C22 1.528(3) 1_555 1_555 no
O1Ac C1Ac 1.180(10) 1_555 1_555 no
C1Ac C2Ac 1.500(15) 1_555 1_555 no
C1Ac C3Ac 1.495(4) 1_555 1_555 no
C2Ac C1Ac 1.500(15) 1_555 4_555 no
O1Me1 C1Me1 1.418(3) 1_555 1_555 no
O1Me2 C1Me2 1.420(4) 1_555 1_555 no
O1Me3 C1Me3 1.413(6) 1_555 1_555 no
O1Me3' C1Me3' 1.412(12) 1_555 1_555 no
