#------------------------------------------------------------------------------
#$Date: 2020-04-05 13:01:50 +0300 (Sun, 05 Apr 2020) $
#$Revision: 250166 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/59/7125966.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_7125966
loop_
_publ_author_name
'Pramanik, Subhamay'
'Day, Victor W.'
'Bowman-James, Kristin'
_publ_section_title
;
 Supramolecular traps for highly phosphorylated inositol sources of
 phosphorus.
;
_journal_issue                   22
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3269
_journal_page_last               3272
_journal_paper_doi               10.1039/c9cc09321d
_journal_volume                  56
_journal_year                    2020
_chemical_formula_sum            'C82 H171.4 N26 O59.6 P6'
_chemical_formula_weight         2661.26
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2020-01-20 deposited with the CCDC.	2020-02-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   18.3819(8)
_cell_length_b                   18.3819(8)
_cell_length_c                   35.5789(18)
_cell_measurement_reflns_used    3885
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      53.17
_cell_measurement_theta_min      3.04
_cell_volume                     10411.3(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker Platinum 135 CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0721
_diffrn_reflns_av_unetI/netI     0.0747
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            12128
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        62.631
_diffrn_reflns_theta_max         62.631
_diffrn_reflns_theta_min         3.726
_diffrn_source                   'Bruker MicroStar microfocus rotating anode'
_exptl_absorpt_coefficient_mu    1.538
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.711
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_description       Rhomboid
_exptl_crystal_F_000             4237
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.930
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         3641
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.2191
_refine_ls_R_factor_gt           0.1584
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0900P)²+180.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3512
_refine_ls_wR_factor_ref         0.3915
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2001
_reflns_number_total             3641
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9cc09321d2.cif
_cod_data_source_block           v99d
_cod_depositor_comments
'Adding full bibliography for 7125965--7125967.cif.'
_cod_original_cell_volume        10411.3(10)
_cod_original_formula_sum        'C82 H171.40 N26 O59.60 P6'
_cod_database_code               7125966
_shelx_shelxl_version_number     2017/1
_shelx_space_group_comment
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;
_shelx_estimated_absorpt_t_min   0.769
_shelx_estimated_absorpt_t_max   0.887
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
P P 0.5770(2) 0.7524(3) 0.19572(9) 0.1162(13) Uani 1 1 d . . .
O11 O 0.5060(5) 0.7354(5) 0.16633(19) 0.100(2) Uani 1 1 d . . .
O12 O 0.6408(8) 0.8486(10) 0.1858(4) 0.280(11) Uani 1 1 d . . .
H12O H 0.614545 0.869461 0.175201 0.420 Uiso 1 1 calc R U .
O13 O 0.6105(9) 0.6998(10) 0.1825(3) 0.197(6) Uani 1 1 d . . .
O14 O 0.5501(4) 0.7425(5) 0.2347(2) 0.104(2) Uani 1 1 d . . .
C21 C 0.4219(6) 0.7007(7) 0.1767(4) 0.108(4) Uani 1 1 d . . .
H21 H 0.413766 0.697588 0.204605 0.130 Uiso 1 1 calc R U .
O1 O 0.6289(5) 0.6275(6) 0.3515(3) 0.119(3) Uani 1 1 d . . .
O2 O 0.4778(4) 0.9065(4) 0.32825(17) 0.088(2) Uani 1 1 d . . .
N1 N 0.6179(5) 0.6786(6) 0.2948(3) 0.095(3) Uani 1 1 d . . .
H1N H 0.599803 0.708293 0.282737 0.115 Uiso 1 1 calc R U .
N2 N 0.5577(5) 0.7674(5) 0.3286(2) 0.082(2) Uani 1 1 d . . .
N3 N 0.5215(6) 0.8555(6) 0.2810(2) 0.097(3) Uani 1 1 d . . .
H3N H 0.544318 0.824934 0.274965 0.116 Uiso 1 1 calc R U .
N4 N 0.5005(6) 1.0222(6) 0.2749(3) 0.099(3) Uani 1 1 d . . .
H4N H 0.472425 0.981528 0.295942 0.119 Uiso 1 1 calc R U .
C1 C 0.5883(8) 0.5693(8) 0.2515(4) 0.114(4) Uani 1 1 d . . .
H1A H 0.614163 0.545361 0.234926 0.137 Uiso 1 1 calc R U .
H1B H 0.560820 0.592242 0.235250 0.137 Uiso 1 1 calc R U .
C2 C 0.6550(8) 0.6386(8) 0.2728(4) 0.121(4) Uani 1 1 d . . .
H2A H 0.682816 0.617156 0.289692 0.145 Uiso 1 1 calc R U .
H2B H 0.697714 0.679907 0.255404 0.145 Uiso 1 1 calc R U .
C3 C 0.6097(7) 0.6727(7) 0.3324(4) 0.094(3) Uani 1 1 d . . .
C4 C 0.5790(7) 0.7230(7) 0.3508(3) 0.090(3) Uani 1 1 d . . .
C5 C 0.5734(8) 0.7237(8) 0.3884(4) 0.110(4) Uani 1 1 d . . .
H5 H 0.589362 0.691594 0.403719 0.132 Uiso 1 1 calc R U .
C6 C 0.5437(9) 0.7722(9) 0.4042(3) 0.121(5) Uani 1 1 d . . .
H6 H 0.539386 0.774081 0.430769 0.146 Uiso 1 1 calc R U .
C7 C 0.5200(8) 0.8186(7) 0.3816(3) 0.101(3) Uani 1 1 d . . .
H7 H 0.498790 0.851862 0.391987 0.121 Uiso 1 1 calc R U .
C8 C 0.5287(6) 0.8139(6) 0.3435(2) 0.075(2) Uani 1 1 d . . .
C9 C 0.5072(6) 0.8623(7) 0.3165(3) 0.084(3) Uani 1 1 d . . .
C10 C 0.5010(9) 0.8969(9) 0.2511(3) 0.111(4) Uani 1 1 d . . .
H10A H 0.440079 0.877119 0.251948 0.134 Uiso 1 1 calc R U .
H10B H 0.513309 0.880230 0.226497 0.134 Uiso 1 1 calc R U .
C11 C 0.5491(8) 0.9914(10) 0.2541(3) 0.114(4) Uani 1 1 d . . .
H11A H 0.603108 1.009558 0.267110 0.137 Uiso 1 1 calc R U .
H11B H 0.561791 1.016157 0.228537 0.137 Uiso 1 1 calc R U .
C12 C 0.5548(9) 1.1050(9) 0.2930(5) 0.142(5) Uani 1 1 d . . .
H12A H 0.519531 1.123878 0.305407 0.214 Uiso 1 1 calc R U .
H12B H 0.589566 1.146052 0.273829 0.214 Uiso 1 1 calc R U .
H12C H 0.591052 1.099658 0.311639 0.214 Uiso 1 1 calc R U .
N1S N 0.333333 0.666667 0.3518(5) 0.111(6) Uani 1 3 d S T P
C1S C 0.333333 0.666667 0.3202(7) 0.102(6) Uani 1 3 d S T P
C2S C 0.333333 0.666667 0.2792(6) 0.134(8) Uani 1 3 d S T P
H2S H 0.381670 0.665400 0.268280 0.201 Uiso 1 1 d . U .
O1W O 0.333333 0.666667 0.4337(5) 0.200(9) Uani 1 3 d S T P
O2W O 0.5381(9) 0.5040(12) 0.4044(6) 0.263(11) Uani 0.8 1 d . . P
O3W O 0.5992(15) 0.4112(14) 0.4271(8) 0.253(11) Uani 0.7 1 d . . P
O4W O 0.7621(17) 0.734(3) 0.1662(7) 0.24(2) Uani 0.4 1 d . . P
O5W O 0.8141(18) 0.886(2) 0.1545(8) 0.223(11) Uani 0.5 1 d . U P
O6W O 0.666667 1.333333 0.2782(18) 0.28(3) Uani 0.6 3 d S T P
O7W O 0.481(2) 0.5506(16) 0.4608(6) 0.32(3) Uani 0.5 1 d . . P
O7W' O 0.508(3) 0.674(3) 0.5063(11) 0.125(13) Uani 0.2 1 d . U P
O7W" O 0.415(2) 0.617(2) 0.4769(9) 0.144(11) Uani 0.3 1 d . U P
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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 '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'
P P 0.2955 0.4335 '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
O14 P O13 117.0(6) . .
O14 P O11 114.3(5) . .
O13 P O11 103.7(6) . .
O14 P O12 111.5(7) . .
O13 P O12 110.1(10) . .
O11 P O12 98.6(5) . .
C21 O11 P 122.2(8) . .
P O12 H12O 109.5 . .
O11 C21 C21 109.5(10) . 14_455
O11 C21 C21 106.7(11) . 15
C21 C21 C21 101.3(11) 14_455 15
O11 C21 H21 112.8 . .
C21 C21 H21 112.8 14_455 .
C21 C21 H21 112.8 15 .
C3 N1 C2 123.8(11) . .
C3 N1 H1N 118.1 . .
C2 N1 H1N 118.1 . .
C8 N2 C4 119.9(9) . .
C9 N3 C10 122.4(10) . .
C9 N3 H3N 118.8 . .
C10 N3 H3N 118.8 . .
C11 N4 C12 112.6(11) . .
C11 N4 C1 112.0(10) . 2_665
C12 N4 C1 113.8(10) . 2_665
C11 N4 H4N 105.9 . .
C12 N4 H4N 105.9 . .
C1 N4 H4N 105.9 2_665 .
C2 C1 N4 115.3(11) . 3_565
C2 C1 H1A 108.5 . .
N4 C1 H1A 108.5 3_565 .
C2 C1 H1B 108.5 . .
N4 C1 H1B 108.5 3_565 .
H1A C1 H1B 107.5 . .
N1 C2 C1 108.5(10) . .
N1 C2 H2A 110.0 . .
C1 C2 H2A 110.0 . .
N1 C2 H2B 110.0 . .
C1 C2 H2B 110.0 . .
H2A C2 H2B 108.4 . .
O1 C3 N1 122.3(12) . .
O1 C3 C4 120.3(12) . .
N1 C3 C4 117.4(11) . .
N2 C4 C5 122.6(12) . .
N2 C4 C3 116.8(10) . .
C5 C4 C3 120.6(12) . .
C4 C5 C6 118.0(12) . .
C4 C5 H5 121.0 . .
C6 C5 H5 121.0 . .
C5 C6 C7 120.5(11) . .
C5 C6 H6 119.7 . .
C7 C6 H6 119.7 . .
C8 C7 C6 116.8(12) . .
C8 C7 H7 121.6 . .
C6 C7 H7 121.6 . .
N2 C8 C7 122.2(10) . .
N2 C8 C9 116.2(8) . .
C7 C8 C9 121.6(10) . .
O2 C9 N3 124.0(10) . .
O2 C9 C8 120.1(9) . .
N3 C9 C8 116.0(10) . .
N3 C10 C11 113.1(10) . .
N3 C10 H10A 109.0 . .
C11 C10 H10A 109.0 . .
N3 C10 H10B 109.0 . .
C11 C10 H10B 109.0 . .
H10A C10 H10B 107.8 . .
N4 C11 C10 111.0(10) . .
N4 C11 H11A 109.4 . .
C10 C11 H11A 109.4 . .
N4 C11 H11B 109.4 . .
C10 C11 H11B 109.4 . .
H11A C11 H11B 108.0 . .
N4 C12 H12A 109.5 . .
N4 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
N4 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
N1S C1S C2S 180.0 . .
C1S C2S H2S 113.3 . .
C1S C2S H2S 113.3(11) . 2_665
H2S C2S H2S 105.4 . 2_665
C1S C2S H2S 113.3(11) . 3_565
H2S C2S H2S 105.4 . 3_565
H2S C2S H2S 105.4 2_665 3_565
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
P O14 1.455(8) .
P O13 1.458(11) .
P O11 1.577(8) .
P O12 1.598(14) .
O11 C21 1.397(11) .
O12 H12O 0.8400 .
C21 C21 1.592(17) 14_455
C21 C21 1.592(17) 15
C21 H21 1.0000 .
O1 C3 1.254(13) .
O2 C9 1.251(11) .
N1 C3 1.346(14) .
N1 C2 1.453(13) .
N1 H1N 0.8800 .
N2 C8 1.323(12) .
N2 C4 1.327(13) .
N3 C9 1.306(11) .
N3 C10 1.464(13) .
N3 H3N 0.8800 .
N4 C11 1.476(14) .
N4 C12 1.485(16) .
N4 C1 1.505(14) 2_665
N4 H4N 1.0000 .
C1 C2 1.462(16) .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 C4 1.456(16) .
C4 C5 1.345(15) .
C5 C6 1.377(17) .
C5 H5 0.9500 .
C6 C7 1.391(17) .
C6 H6 0.9500 .
C7 C8 1.372(13) .
C7 H7 0.9500 .
C8 C9 1.493(14) .
C10 C11 1.509(17) .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
C11 H11A 0.9900 .
C11 H11B 0.9900 .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
N1S C1S 1.12(2) .
C1S C2S 1.46(3) .
C2S H2S 0.9801 .
C2S H2S 0.980(8) 2_665
C2S H2S 0.980(8) 3_565
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
_geom_hbond_publ_flag
O12 H12O O13 0.84 2.01 2.83(2) 166.8 15 yes
N1 H1N O14 0.88 2.17 2.994(13) 155.0 . yes
N3 H3N O14 0.88 2.13 2.898(11) 146.2 . yes
N4 H4N O2 1.00 1.84 2.723(11) 146.1 . yes
C1 H1B O13 0.99 2.54 3.311(18) 134.6 . yes
C10 H10B O11 0.99 2.44 3.194(12) 132.7 15 yes
C11 H11A O1 0.99 2.38 3.337(15) 162.0 16_665 yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O14 P O11 C21 -9.8(10) . .
O13 P O11 C21 118.7(10) . .
O12 P O11 C21 -128.1(10) . .
P O11 C21 C21 -116.8(12) . 14_455
P O11 C21 C21 134.4(10) . 15
C3 N1 C2 C1 109.0(13) . .
N4 C1 C2 N1 -63.1(15) 3_565 .
C2 N1 C3 O1 -4.6(17) . .
C2 N1 C3 C4 174.0(10) . .
C8 N2 C4 C5 -0.8(16) . .
C8 N2 C4 C3 179.5(9) . .
O1 C3 C4 N2 -178.1(10) . .
N1 C3 C4 N2 3.3(14) . .
O1 C3 C4 C5 2.1(17) . .
N1 C3 C4 C5 -176.5(10) . .
N2 C4 C5 C6 0.4(18) . .
C3 C4 C5 C6 -179.8(11) . .
C4 C5 C6 C7 0(2) . .
C5 C6 C7 C8 -0.7(19) . .
C4 N2 C8 C7 0.3(15) . .
C4 N2 C8 C9 179.4(9) . .
C6 C7 C8 N2 0.4(16) . .
C6 C7 C8 C9 -178.6(10) . .
C10 N3 C9 O2 -2.6(17) . .
C10 N3 C9 C8 177.9(10) . .
N2 C8 C9 O2 178.6(9) . .
C7 C8 C9 O2 -2.4(15) . .
N2 C8 C9 N3 -1.9(13) . .
C7 C8 C9 N3 177.2(10) . .
C9 N3 C10 C11 62.5(15) . .
C12 N4 C11 C10 154.7(10) . .
C1 N4 C11 C10 -75.5(12) 2_665 .
N3 C10 C11 N4 -93.7(12) . .
