#------------------------------------------------------------------------------
#$Date: 2015-12-09 13:56:54 +0200 (Wed, 09 Dec 2015) $
#$Revision: 170985 $
#$URL: svn://www.crystallography.net/cod/cif/1/52/93/1529321.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_1529321
loop_
_publ_author_name
'Barker, Emily C.'
'Goh, Ching Yong'
'Jones, Franca'
'Mocerino, Mauro'
'Skelton, Brian W.'
'Becker, Thomas'
'Ogden, Mark I.'
_publ_section_title
;
 Investigating hydrogel formation using in situ variable-temperature
 scanning probe microscopy
;
_journal_issue                   11
_journal_name_full               'Chem. Sci.'
_journal_page_first              6133
_journal_paper_doi               10.1039/C5SC02196K
_journal_volume                  6
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C52 H60 N4 O12, C4 H8 O'
_chemical_formula_sum            'C56 H68 N4 O13'
_chemical_formula_weight         1005.14
_chemical_properties_physical    Efflorescent
_space_group_IT_number           209
_symmetry_cell_setting           cubic
_symmetry_Int_Tables_number      209
_symmetry_space_group_name_Hall  'F 4 2 3'
_symmetry_space_group_name_H-M   'F 4 3 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-06-12T08:07:09-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2015-06-12 deposited with the CCDC.
2015-08-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            24
_cell_length_a                   36.2659(2)
_cell_length_b                   36.2659(2)
_cell_length_c                   36.2659(2)
_cell_measurement_reflns_used    22874
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      67.1515
_cell_measurement_theta_min      3.4389
_cell_volume                     47697.5(5)
_computing_cell_refinement
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
        (compiled Jan 10 2008,16:37:18)
;
_computing_data_collection
;
        CrysAlis CCD, Oxford Diffraction Ltd.,
        Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
        (compiled Jan 10 2008,16:37:18)
;
_computing_data_reduction
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
        (compiled Jan 10 2008,16:37:18)
;
_computing_molecular_graphics    'Diamond (Brandenburg, K., (1999)'
_computing_publication_material  'WinGX Farrugia, L. J. (1999)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.4738
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
;
 Oxford Diffraction Gemini diffractometer
;
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0325850736
_diffrn_orient_matrix_UB_12      0.0181666536
_diffrn_orient_matrix_UB_13      -0.0205828603
_diffrn_orient_matrix_UB_21      -0.0220258864
_diffrn_orient_matrix_UB_22      0.0361848342
_diffrn_orient_matrix_UB_23      -0.0026870676
_diffrn_orient_matrix_UB_31      0.0164277526
_diffrn_orient_matrix_UB_32      0.0128559698
_diffrn_orient_matrix_UB_33      0.0369859983
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.058
_diffrn_reflns_av_unetI/netI     0.1585
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            144382
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.28
_diffrn_reflns_theta_max         67.28
_diffrn_reflns_theta_min         3.447
_exptl_absorpt_coefficient_mu    0.489
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.85908
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.84
_exptl_crystal_description       block
_exptl_crystal_F_000             12864
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: H2O/THF'
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.418
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details
;
 Flack x determined using 947 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.05(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.323
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         3613
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      1.37
_refine_ls_R_factor_all          0.1253
_refine_ls_R_factor_gt           0.1157
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3037
_refine_ls_wR_factor_ref         0.3188
_reflns_number_gt                2883
_reflns_number_total             3613
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5sc02196k2.cif
_cod_data_source_block           mmcy04
_cod_depositor_comments          'Adding full bibliography for 1529321.cif.'
_cod_original_cell_volume        47697.5(8)
_cod_database_code               1529321
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, -z'
'-y, -x, -z'
'y, -x, z'
'-y, x, z'
'x, z, -y'
'-x, z, y'
'-x, -z, -y'
'x, -z, y'
'z, y, -x'
'z, -y, x'
'-z, y, x'
'-z, -y, -x'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y+1/2, -z+1/2'
'z, x+1/2, y+1/2'
'z, -x+1/2, -y+1/2'
'-z, -x+1/2, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z+1/2, x+1/2'
'-y, z+1/2, -x+1/2'
'y, -z+1/2, -x+1/2'
'-y, -z+1/2, x+1/2'
'y, x+1/2, -z+1/2'
'-y, -x+1/2, -z+1/2'
'y, -x+1/2, z+1/2'
'-y, x+1/2, z+1/2'
'x, z+1/2, -y+1/2'
'-x, z+1/2, y+1/2'
'-x, -z+1/2, -y+1/2'
'x, -z+1/2, y+1/2'
'z, y+1/2, -x+1/2'
'z, -y+1/2, x+1/2'
'-z, y+1/2, x+1/2'
'-z, -y+1/2, -x+1/2'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'-x+1/2, y, -z+1/2'
'x+1/2, -y, -z+1/2'
'z+1/2, x, y+1/2'
'z+1/2, -x, -y+1/2'
'-z+1/2, -x, y+1/2'
'-z+1/2, x, -y+1/2'
'y+1/2, z, x+1/2'
'-y+1/2, z, -x+1/2'
'y+1/2, -z, -x+1/2'
'-y+1/2, -z, x+1/2'
'y+1/2, x, -z+1/2'
'-y+1/2, -x, -z+1/2'
'y+1/2, -x, z+1/2'
'-y+1/2, x, z+1/2'
'x+1/2, z, -y+1/2'
'-x+1/2, z, y+1/2'
'-x+1/2, -z, -y+1/2'
'x+1/2, -z, y+1/2'
'z+1/2, y, -x+1/2'
'z+1/2, -y, x+1/2'
'-z+1/2, y, x+1/2'
'-z+1/2, -y, -x+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
'z+1/2, x+1/2, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x+1/2, y'
'-z+1/2, x+1/2, -y'
'y+1/2, z+1/2, x'
'-y+1/2, z+1/2, -x'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z+1/2, x'
'y+1/2, x+1/2, -z'
'-y+1/2, -x+1/2, -z'
'y+1/2, -x+1/2, z'
'-y+1/2, x+1/2, z'
'x+1/2, z+1/2, -y'
'-x+1/2, z+1/2, y'
'-x+1/2, -z+1/2, -y'
'x+1/2, -z+1/2, y'
'z+1/2, y+1/2, -x'
'z+1/2, -y+1/2, x'
'-z+1/2, y+1/2, x'
'-z+1/2, -y+1/2, -x'
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.35830(11) 0.56940(10) 0.97982(11) 0.0736(10) Uani 1 d . .
O1 O 0.39037(7) 0.54991(7) 0.98372(7) 0.0705(8) Uani 1 d . .
H1 H 0.3968 0.55 1.006 0.106 Uiso 1 calc . .
C2 C 0.34303(12) 0.56998(10) 0.94500(11) 0.0794(11) Uani 1 d . .
C3 C 0.31040(14) 0.58981(14) 0.94009(17) 0.1028(15) Uani 1 d . .
H3 H 0.299 0.5903 0.9165 0.123 Uiso 1 calc . .
C4 C 0.29419(17) 0.60893(16) 0.9694(2) 0.1173(18) Uani 1 d . .
C41 C 0.2584(2) 0.6293(2) 0.9648(3) 0.148(3) Uani 1 d . .
H41A H 0.2425 0.6246 0.9865 0.177 Uiso 1 calc . .
H41B H 0.2454 0.6198 0.9428 0.177 Uiso 1 calc . .
N41 N 0.2640(2) 0.6709(2) 0.9606(3) 0.184(3) Uani 1 d . .
H41 H 0.2765 0.6796 0.9836 0.22 Uiso 1 calc . .
C42 C 0.2887(4) 0.6820(3) 0.9288(4) 0.204(4) Uani 1 d . .
H42 H 0.3021 0.6598 0.9194 0.245 Uiso 1 calc . .
C43 C 0.2586(5) 0.6945(4) 0.8992(5) 0.237(5) Uani 1 d . .
H43A H 0.2627 0.7203 0.8915 0.284 Uiso 1 calc . .
H43B H 0.2595 0.6784 0.8772 0.284 Uiso 1 calc . .
C44 C 0.2216(5) 0.6905(4) 0.9192(6) 0.258(7) Uani 1 d . .
H44A H 0.2051 0.7112 0.9124 0.309 Uiso 1 calc . .
H44B H 0.2095 0.6672 0.9117 0.309 Uiso 1 calc . .
C45 C 0.2279(4) 0.6905(5) 0.9586(6) 0.241(6) Uani 1 d . .
H45A H 0.2084 0.677 0.972 0.289 Uiso 1 calc . .
H45B H 0.2297 0.7159 0.9685 0.289 Uiso 1 calc . .
C46 C 0.3165(6) 0.7125(6) 0.9375(6) 0.263(7) Uani 1 d . .
O41 O 0.3386(5) 0.7157(5) 0.9121(5) 0.330(8) Uani 1 d . .
O42 O 0.3106(3) 0.7249(3) 0.9671(5) 0.249(5) Uani 1 d . .
C5 C 0.31110(14) 0.60844(14) 1.0033(2) 0.1048(15) Uani 1 d . .
H5 H 0.3007 0.6224 1.023 0.126 Uiso 1 calc . .
C6 C 0.34265(13) 0.58830(11) 1.00964(13) 0.0845(12) Uani 1 d . .
C0 C 0.35899(13) 0.54796(13) 0.91360(12) 0.0867(12) Uani 1 d . .
H0A H 0.386 0.5461 0.9168 0.104 Uiso 1 calc . .
H0B H 0.3542 0.561 0.8901 0.104 Uiso 1 calc . .
O01 O 0.2699(6) 0.5115(8) 1.0076(17) 0.182(12) Uiso 0.25 d A -1
C02 C 0.2404(7) 0.5338(7) 1.0172(8) 0.131(8) Uiso 0.25 d A -1
H02A H 0.2274 0.5428 0.9949 0.157 Uiso 0.25 calc A -1
H02B H 0.2489 0.5553 1.0317 0.157 Uiso 0.25 calc A -1
C03 C 0.2154(9) 0.5094(10) 1.0401(11) 0.175(14) Uiso 0.25 d A -1
H03A H 0.2238 0.5077 1.066 0.21 Uiso 0.25 calc A -1
H03B H 0.1895 0.518 1.0395 0.21 Uiso 0.25 calc A -1
C04 C 0.2203(13) 0.4731(11) 1.020(2) 0.35(6) Uiso 0.25 d A -1
H04A H 0.2054 0.4723 0.997 0.425 Uiso 0.25 calc A -1
H04B H 0.2139 0.4518 1.0357 0.425 Uiso 0.25 calc A -1
C05 C 0.2613(12) 0.4744(8) 1.0115(14) 0.174(15) Uiso 0.25 d A -1
H05A H 0.2756 0.4634 1.032 0.208 Uiso 0.25 calc A -1
H05B H 0.2668 0.4607 0.9886 0.208 Uiso 0.25 calc A -1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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
O1 C1 C2 116.3(3) . .
O1 C1 C6 121.2(4) . .
C2 C1 C6 122.5(4) . .
C1 O1 H1 109.5 . .
C1 C2 C3 117.7(4) . .
C1 C2 C0 122.0(4) . .
C3 C2 C0 120.2(4) . .
C4 C3 C2 120.9(6) . .
C4 C3 H3 119.5 . .
C2 C3 H3 119.5 . .
C5 C4 C3 119.1(5) . .
C5 C4 C41 119.4(6) . .
C3 C4 C41 121.4(7) . .
C4 C41 N41 112.4(7) . .
C4 C41 H41A 109.1 . .
N41 C41 H41A 109.1 . .
C4 C41 H41B 109.1 . .
N41 C41 H41B 109.1 . .
H41A C41 H41B 107.9 . .
C45 N41 C42 110.9(11) . .
C45 N41 C41 111.0(11) . .
C42 N41 C41 114.7(7) . .
C45 N41 H41 106.6 . .
C42 N41 H41 106.6 . .
C41 N41 H41 106.6 . .
N41 C42 C46 115.0(14) . .
N41 C42 C43 100.5(11) . .
C46 C42 C43 112.7(11) . .
N41 C42 H42 109.4 . .
C46 C42 H42 109.4 . .
C43 C42 H42 109.4 . .
C44 C43 C42 104.9(14) . .
C44 C43 H43A 110.8 . .
C42 C43 H43A 110.8 . .
C44 C43 H43B 110.8 . .
C42 C43 H43B 110.8 . .
H43A C43 H43B 108.8 . .
C45 C44 C43 109.1(17) . .
C45 C44 H44A 109.9 . .
C43 C44 H44A 109.9 . .
C45 C44 H44B 109.9 . .
C43 C44 H44B 109.9 . .
H44A C44 H44B 108.3 . .
C44 C45 N41 100.7(14) . .
C44 C45 H45A 111.6 . .
N41 C45 H45A 111.6 . .
C44 C45 H45B 111.6 . .
N41 C45 H45B 111.6 . .
H45A C45 H45B 109.4 . .
O42 C46 O41 140(3) . .
O42 C46 C42 110(2) . .
O41 C46 C42 110(2) . .
C4 C5 C6 121.8(5) . .
C4 C5 H5 119.1 . .
C6 C5 H5 119.1 . .
C5 C6 C1 117.9(5) . .
C5 C6 C0 120.2(4) . 44_565
C1 C6 C0 121.9(4) . 44_565
C2 C0 C6 111.8(3) . 41_546
C2 C0 H0A 109.3 . .
C6 C0 H0A 109.3 41_546 .
C2 C0 H0B 109.3 . .
C6 C0 H0B 109.3 41_546 .
H0A C0 H0B 107.9 . .
C05 O01 C02 111.6(15) . .
O01 C02 C03 104.9(18) . .
O01 C02 H02A 110.8 . .
C03 C02 H02A 110.8 . .
O01 C02 H02B 110.8 . .
C03 C02 H02B 110.8 . .
H02A C02 H02B 108.8 . .
C04 C03 C02 99.9(19) . .
C04 C03 H03A 111.8 . .
C02 C03 H03A 111.8 . .
C04 C03 H03B 111.8 . .
C02 C03 H03B 111.8 . .
H03A C03 H03B 109.5 . .
C03 C04 C05 101(2) . .
C03 C04 H04A 111.6 . .
C05 C04 H04A 111.6 . .
C03 C04 H04B 111.6 . .
C05 C04 H04B 111.6 . .
H04A C04 H04B 109.4 . .
O01 C05 C04 105.7(17) . .
O01 C05 H05A 110.6 . .
C04 C05 H05A 110.6 . .
O01 C05 H05B 110.6 . .
C04 C05 H05B 110.6 . .
H05A C05 H05B 108.7 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O1 1.368(5) .
C1 C2 1.379(6) .
C1 C6 1.401(6) .
O1 H1 0.84 .
C2 C3 1.396(6) .
C2 C0 1.506(6) .
C3 C4 1.400(9) .
C3 H3 0.95 .
C4 C5 1.374(10) .
C4 C41 1.504(8) .
C41 N41 1.529(13) .
C41 H41A 0.99 .
C41 H41B 0.99 .
N41 C45 1.493(12) .
N41 C42 1.515(16) .
N41 H41 1 .
C42 C46 1.53(3) .
C42 C43 1.60(2) .
C42 H42 1 .
C43 C44 1.53(2) .
C43 H43A 0.99 .
C43 H43B 0.99 .
C44 C45 1.45(2) .
C44 H44A 0.99 .
C44 H44B 0.99 .
C45 H45A 0.99 .
C45 H45B 0.99 .
C46 O42 1.183(19) .
C46 O41 1.228(19) .
C5 C6 1.377(7) .
C5 H5 0.95 .
C6 C0 1.512(7) 44_565
C0 C6 1.512(7) 41_546
C0 H0A 0.99 .
C0 H0B 0.99 .
O01 C05 1.39(2) .
O01 C02 1.39(2) .
C02 C03 1.52(2) .
C02 H02A 0.99 .
C02 H02B 0.99 .
C03 C04 1.52(3) .
C03 H03A 0.99 .
C03 H03B 0.99 .
C04 C05 1.52(2) .
C04 H04A 0.99 .
C04 H04B 0.99 .
C05 H05A 0.99 .
C05 H05B 0.99 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 O1 0.84 2.02 2.693(4) 136.4 44_565
O1 H1 O1 0.84 2.02 2.693(4) 136.4 44_565
N41 H41 O42 1.00 1.82 2.735(18) 150.2 14_667
C45 H45B O42 0.99 2.6 3.383(15) 136.4 74_565
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.000 0.000 0.000 125.2 113.4
2 0.428 -0.005 -0.004 16483.0 3981.0
3 0.500 0.000 0.500 125.3 113.4
4 0.500 0.500 0.000 125.3 113.4
5 0.000 0.500 0.500 125.3 113.4
