About the relevance of anion-π interactions in water.
Pitarch-Jarque, Javier; Zaragozá, Ramón J; Ballesteros, Rafael; Abarca, Belen; Garcia-España, Enrique; Verdejo, Begoña; Ballesteros-Garrido, Rafael; Dalton transactions (Cambridge, England : 2003) 50 (2021) 6834–6839; doi:10.1039/d1dt00771h

data_7707137
_publ_section_title
;
 About the relevance of anion-\p interactions in water.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6834
_journal_page_last               6839
_journal_paper_doi               10.1039/d1dt00771h
_journal_volume                  50
_journal_year                    2021
_chemical_absolute_configuration unk
_chemical_formula_moiety         '9(Br), 3(C30 H30 N9), 4(H2 O)'
_chemical_formula_sum            'C90 H98 Br9 N27 O4'
_chemical_formula_weight         2341.14
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2019-10-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-10-28 deposited with the CCDC.	2021-04-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.7951(4)
_cell_length_b                   30.5457(6)
_cell_length_c                   14.9217(3)
_cell_measurement_reflns_used    9615
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      28.5680
_cell_measurement_theta_min      3.6010
_cell_volume                     9478.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -96.00 -35.00   1.00   30.46    --  -19.87-178.00  60.00   61
  2  \w    -81.00  15.00   1.00   30.46    --  -19.87   0.00   0.00   96
  3  \w     -5.00  83.00   1.00   30.46    --   20.73  38.00  30.00   88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0118789000
_diffrn_orient_matrix_UB_12      -0.0035546000
_diffrn_orient_matrix_UB_13      0.0405544000
_diffrn_orient_matrix_UB_21      -0.0090907000
_diffrn_orient_matrix_UB_22      0.0291477000
_diffrn_orient_matrix_UB_23      0.0161722000
_diffrn_orient_matrix_UB_31      -0.0177531000
_diffrn_orient_matrix_UB_32      -0.0173187000
_diffrn_orient_matrix_UB_33      0.0188957000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_unetI/netI     0.0577
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            43674
_diffrn_reflns_point_group_measured_fraction_full 0.761
_diffrn_reflns_point_group_measured_fraction_max 0.754
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         3.309
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.872
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52044
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_description       block
_exptl_crystal_F_000             4696
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.897
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.099
_refine_ls_abs_structure_details
;
 Flack x determined using 2760 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.007(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1208
_refine_ls_number_reflns         14073
_refine_ls_number_restraints     135
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0450
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0527P)^2^+8.9994P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1010
_refine_ls_wR_factor_ref         0.1128
_reflns_Friedel_coverage         0.453
_reflns_Friedel_fraction_full    0.505
_reflns_Friedel_fraction_max     0.491
_reflns_number_gt                11106
_reflns_number_total             14073
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00771h2.cif
_cod_data_source_block           rafaiodo2(1)
_cod_depositor_comments
'Adding full bibliography for 7707136--7707138.cif.'
_cod_database_code               7707137
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.654
_shelx_estimated_absorpt_t_min   0.390
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.979(12)
 0.021(12)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H2a,H2b} of O2, {H1a,H1b} of O1, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, {H4a,H4b} of O4, {H3a,H3b} of O3
3. Restrained distances
 H1a-O1
 0.82 with sigma of 0.01
 O1-H1b
 0.82 with sigma of 0.01
 H1b-H1a
 1.39 with sigma of 0.01
 O2-H2a
 0.82 with sigma of 0.01
 H3b-Br5
 2.6 with sigma of 0.01
 H4a-C55_$1
 2.893 with sigma of 0.01
 H4b-Br9A
 1.5 with sigma of 0.01
 H4b-H44
 2.2 with sigma of 0.01
4. Rigid bond restraints
 C70, N20
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N11, C40
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C8, C10
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C68, N19
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C76, C78
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C38, C39
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C16, C18
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C46, C47
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C54, C56
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C76, C77
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C84, C86
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C68, C69
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C24, C26
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C14 \\sim N2 \\sim N3: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02
N27 \\sim N26 \\sim C78: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02
N2 \\sim N3 \\sim C14: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02
N8 \\sim C30 \\sim C26 \\sim C24: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C70) \\sim Ueq, Uanis(C72) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(O4) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(N14) \\sim Ueq, Uanis(N11)
\\sim Ueq, Uanis(N20) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.001
Uanis(N5) \\sim Ueq, Uanis(N21) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.001
Uanis(C74) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(N27) \\sim Ueq, Uanis(C61) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
6. Others
 Fixed Sof: Br8B(0.6) Br9B(0.7) Br9A(0.3) Br8A(0.4)
7.a Free rotating group:
 O3(H3a,H3b), O4(H4a,H4b)
7.b Rotating group with stretchable bonds:
 O1(H1a,H1b), O2(H2a,H2b)
7.c Secondary CH2 refined with riding coordinates:
 C7(H7a,H7b), C23(H23a,H23b), C37(H37a,H37b), C83(H83a,H83b), C15(H15a,H15b),
 C53(H53a,H53b), C75(H75a,H75b), C67(H67a,H67b), C45(H45a,H45b)
7.d Me refined with riding coordinates:
 C55(H55a,H55b,H55c)
7.e Aromatic/amide H refined with riding coordinates:
 C6(H6), C2(H2), C64(H64), C36(H36), C4(H4), C14(H14), C32(H32), C13(H13),
 C42(H42), C34(H34), C12(H12), C66(H66), C11(H11), C19(H19), C90(H90), C49(H49),
  C30(H30), C82(H82), C22(H22), C80(H80), C52(H52), C79(H79), C41(H41),
 C88(H88), C27(H27), C81(H81), C60(H60), C62(H62), C89(H89), C44(H44), C58(H58),
  C87(H87), C57(H57), C20(H20), C28(H28), C51(H51), C50(H50), C21(H21),
 C43(H43), C59(H59), C29(H29), C71(H71), C72(H72), C73(H73), C74(H74)
7.f Idealised Me refined as rotating group:
 C17(H17a,H17b,H17c), C9(H9a,H9b,H9c), C39(H39a,H39b,H39c), C77(H77a,H77b,
 H77c), C47(H47a,H47b,H47c), C69(H69a,H69b,H69c), C85(H85a,H85b,H85c), C25(H25a,
 H25b,H25c)
;
_shelx_res_checksum              91488
_shelx_hkl_checksum              29812
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.622
_oxdiff_exptl_absorpt_empirical_full_min 0.756