#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:47:12 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180155 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/51/7105128.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_7105128
loop_
_publ_author_name
'Massera, Chiara'
'Melegari, Monica'
'Ugozzoli, Franco'
'Dalcanale, Enrico'
_publ_section_title
;
 Formation of tetrameric water clusters driven by a cavitand template.
;
_journal_issue                   1
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              88
_journal_page_last               90
_journal_paper_doi               10.1039/b917931c
_journal_volume                  46
_journal_year                    2009
_chemical_formula_sum            'C37 H48 O17 P4'
_chemical_formula_weight         888.63
_chemical_name_systematic
;
?
;
_space_group_IT_number           85
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.352(2)
_cell_length_b                   14.352(2)
_cell_length_c                   9.8218(17)
_cell_measurement_reflns_used    2045
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.03
_cell_measurement_theta_min      2.01
_cell_volume                     2023.2(6)
_computing_data_collection       SMART
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Giacovazzo et al., 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean '8.192 pixels/mm'
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'BRUKER AXS SMART 1000'
_diffrn_measurement_method       omega-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_sigmaI/netI    0.0236
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            12598
_diffrn_reflns_theta_full        29.03
_diffrn_reflns_theta_max         29.03
_diffrn_reflns_theta_min         2.01
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.262
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.782580
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker AXS SADABS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             932
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.549
_refine_diff_density_min         -0.228
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     144
_refine_ls_number_reflns         2626
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0467
_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/[σ²(Fo²)+(0.1008P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1417
_refine_ls_wR_factor_ref         0.1509
_reflns_number_gt                1836
_reflns_number_total             2626
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b917931c.txt
_cod_data_source_block           tpometaq
_cod_original_sg_symbol_H-M      P4/n
_cod_database_code               7105128
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y+1/2, x, z'
'y, -x+1/2, z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y-1/2, -x, -z'
'-y, x-1/2, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.43165(3) -0.16861(3) 0.71664(6) 0.0448(2) Uani 1 1 d . . .
O1 O 0.45877(9) -0.08494(9) 0.81278(15) 0.0472(3) Uani 1 1 d . . .
O2 O 0.41318(9) -0.25606(9) 0.81200(16) 0.0472(3) Uani 1 1 d . . .
O3 O 0.49896(12) -0.18675(12) 0.60892(17) 0.0666(5) Uani 1 1 d . . .
C1 C 0.65755(13) -0.09328(13) 1.0433(2) 0.0434(4) Uani 1 1 d . . .
H1 H 0.6758 -0.1232 1.1230 0.050(6) Uiso 1 1 calc R . .
C2 C 0.57193(13) -0.11510(12) 0.9863(2) 0.0416(4) Uani 1 1 d . . .
C3 C 0.54816(12) -0.06912(12) 0.8670(2) 0.0415(4) Uani 1 1 d . . .
C4 C 0.60366(13) -0.00350(12) 0.8032(2) 0.0423(4) Uani 1 1 d . . .
C5 C 0.68829(13) 0.01501(12) 0.8667(2) 0.0413(4) Uani 1 1 d . . .
C6 C 0.71681(13) -0.02825(13) 0.98542(19) 0.0425(4) Uani 1 1 d . . .
C7 C 0.57420(15) 0.04328(15) 0.6736(2) 0.0550(5) Uani 1 1 d . . .
H7A H 0.5908 0.0048 0.5975 0.103(4) Uiso 1 1 calc R . .
H7B H 0.6050 0.1024 0.6659 0.103(4) Uiso 1 1 calc R . .
H7C H 0.5080 0.0526 0.6745 0.103(4) Uiso 1 1 calc R . .
C8 C 0.51020(13) -0.18863(13) 1.0484(2) 0.0458(4) Uani 1 1 d . . .
H8A H 0.4454 -0.1717 1.0346 0.048(4) Uiso 1 1 calc R . .
H8B H 0.5215 -0.1918 1.1456 0.048(4) Uiso 1 1 calc R . .
C9 C 0.31783(16) -0.13599(17) 0.6698(3) 0.0665(7) Uani 1 1 d . . .
H9A H 0.3179 -0.0724 0.6393 0.103(4) Uiso 1 1 calc R . .
H9B H 0.2772 -0.1421 0.7468 0.103(4) Uiso 1 1 calc R . .
H9C H 0.2964 -0.1756 0.5975 0.103(4) Uiso 1 1 calc R . .
O1W O 0.60799(19) -0.2282(2) 0.3796(3) 0.1259(10) Uani 1 1 d . . .
C1S C 0.7500 -0.2500 0.7423(9) 0.111(2) Uani 1 4 d SD . .
O1S O 0.7025(13) -0.216(2) 0.6279(9) 0.158(6) Uani 0.25 1 d PD . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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_3
_geom_angle_publ_flag
O3 P1 O1 114.06(9) . . ?
O3 P1 O2 113.45(9) . . ?
O1 P1 O2 106.86(8) . . ?
O3 P1 C9 118.23(13) . . ?
O1 P1 C9 100.55(10) . . ?
O2 P1 C9 102.09(10) . . ?
C3 O1 P1 125.07(11) . . ?
C5 O2 P1 123.39(11) 3_545 . ?
C6 C1 C2 122.05(19) . . ?
C6 C1 H1 119.0 . . ?
C2 C1 H1 119.0 . . ?
C1 C2 C3 116.86(18) . . ?
C1 C2 C8 121.08(18) . . ?
C3 C2 C8 122.01(17) . . ?
C4 C3 C2 124.37(18) . . ?
C4 C3 O1 117.59(17) . . ?
C2 C3 O1 117.85(17) . . ?
C3 C4 C5 115.46(18) . . ?
C3 C4 C7 121.78(18) . . ?
C5 C4 C7 122.75(18) . . ?
C6 C5 C4 123.41(18) . . ?
C6 C5 O2 118.80(17) . 4_655 ?
C4 C5 O2 117.61(17) . 4_655 ?
C5 C6 C1 117.85(18) . . ?
C5 C6 C8 122.20(18) . 4_655 ?
C1 C6 C8 119.88(18) . 4_655 ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C2 C8 C6 111.24(15) . 3_545 ?
C2 C8 H8A 109.4 . . ?
C6 C8 H8A 109.4 3_545 . ?
C2 C8 H8B 109.4 . . ?
C6 C8 H8B 109.4 3_545 . ?
H8A C8 H8B 108.0 . . ?
P1 C9 H9A 109.5 . . ?
P1 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
P1 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O1S C1S O1S 49.9(6) 3_545 . ?
O1S C1S O1S 73.2(10) 3_545 4_655 ?
O1S C1S O1S 49.9(6) . 4_655 ?
O1S C1S O1S 49.9(6) 3_545 2_645 ?
O1S C1S O1S 73.2(10) . 2_645 ?
O1S C1S O1S 49.9(6) 4_655 2_645 ?
O1S O1S O1S 90.000(3) 3_545 4_655 ?
O1S O1S C1S 65.1(3) 3_545 . ?
O1S O1S C1S 65.1(3) 4_655 . ?
O1S O1S O1S 45.000(2) 3_545 2_645 ?
O1S O1S O1S 45.000(2) 4_655 2_645 ?
C1S O1S O1S 53.4(5) . 2_645 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 O3 1.4562(16) . ?
P1 O1 1.5765(14) . ?
P1 O2 1.5883(15) . ?
P1 C9 1.761(2) . ?
O1 C3 1.408(2) . ?
O2 C5 1.410(2) 3_545 ?
C1 C6 1.385(3) . ?
C1 C2 1.386(3) . ?
C1 H1 0.9300 . ?
C2 C3 1.387(3) . ?
C2 C8 1.507(3) . ?
C3 C4 1.383(3) . ?
C4 C5 1.391(3) . ?
C4 C7 1.500(3) . ?
C5 C6 1.383(3) . ?
C5 O2 1.410(2) 4_655 ?
C6 C8 1.514(3) 4_655 ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 C6 1.514(3) 3_545 ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C1S O1S 1.3994(10) 3_545 ?
C1S O1S 1.3994(10) . ?
C1S O1S 1.3994(10) 4_655 ?
C1S O1S 1.3994(10) 2_645 ?
O1S O1S 1.180(14) 3_545 ?
O1S O1S 1.180(14) 4_655 ?
O1S O1S 1.669(19) 2_645 ?
