Molecular clips with spatially proximal urea residues for efficient transmembrane co-transport of H<sup>+</sup>/Cl<sup>-</sup> ions.
Pradhan, Nyaya Prakash; Namdev, Kavthekar Rupesh; Srivastava, Aasheesh; Organic & biomolecular chemistry 22 (2023) 74–79; doi:10.1039/d3ob01431b

data_7159708
_publ_section_title
;
 Molecular clips with spatially proximal urea residues for efficient
 transmembrane co-transport of H<sup>+</sup>/Cl<sup>-</sup> ions.
;
_journal_issue                   1
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              74
_journal_page_last               79
_journal_paper_doi               10.1039/d3ob01431b
_journal_volume                  22
_journal_year                    2023
_chemical_formula_moiety         'C37 H23 F12 N7 O4, H2 O, [+ solvents]'
_chemical_formula_sum            'C37 H25 F12 N7 O5'
_chemical_formula_weight         875.64
_chemical_name_systematic        'Compound 1a'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2023-04-19
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-04-25 deposited with the CCDC.	2023-12-05 downloaded from the CCDC.
;
_cell_angle_alpha                107.182(12)
_cell_angle_beta                 102.520(13)
_cell_angle_gamma                106.296(11)
_cell_formula_units_Z            2
_cell_length_a                   10.587(2)
_cell_length_b                   15.112(3)
_cell_length_c                   16.143(3)
_cell_measurement_reflns_used    3856
_cell_measurement_temperature    140.00
_cell_measurement_theta_max      21.91
_cell_measurement_theta_min      2.42
_cell_volume                     2238.3(8)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      140.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1556
_diffrn_reflns_av_unetI/netI     0.1228
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            60369
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.885
_diffrn_reflns_theta_min         2.423
_exptl_absorpt_coefficient_mu    0.121
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4787
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1286 before and 0.0789 after correction.
The Ratio of minimum to maximum transmission is 0.6420.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic light yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_description       plate
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.427
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     643
_refine_ls_number_reflns         10655
_refine_ls_number_restraints     832
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.1494
_refine_ls_R_factor_gt           0.0719
_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/[\s^2^(Fo^2^)+(0.0948P)^2^+0.1501P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1872
_refine_ls_wR_factor_ref         0.2267
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4866
_reflns_number_total             10655
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ob01431b2.cif
_cod_data_source_block           f1_a
_cod_depositor_comments          'Adding full bibliography for 7159708.cif.'
_cod_original_cell_volume        2238.2(8)
_cod_database_code               7159708
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 F6-F4 \\sim F6A-F4A
 with sigma of 0.04
 C01I-C1 \\sim C01I-C1A
 with sigma of 0.02
 C1-F6 \\sim C1A-F6A
 with sigma of 0.02
 F5-F4 \\sim F5A-F4A
 with sigma of 0.04
 C1-F5 \\sim C1A-F5A
 with sigma of 0.02
 C1-F4 \\sim C1A-F4A
 with sigma of 0.02
 F6-F5 \\sim F6A-F5A
 with sigma of 0.04
 C01I-F6 \\sim C01I-F6A
 with sigma of 0.04
 C01I-F5 \\sim C01I-F5A
 with sigma of 0.04
 C01I-F4 \\sim C01I-F4A
 with sigma of 0.04
 F1-C6 \\sim F1A-C6
 with sigma of 0.02
 F3-C6 \\sim F3A-C6
 with sigma of 0.02
 F2-C6 \\sim F2A-C6
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1 \\sim F6 \\sim F5 \\sim F4 \\sim F4A \\sim C1A \\sim F6A \\sim F5A: within
2A with sigma of 0.002 and sigma for terminal atoms of 0.004 within 2A
F1 \\sim F2 \\sim F3 \\sim C6 \\sim F3A \\sim F2A \\sim F1A: within 2A with
sigma of 0.002 and sigma for terminal atoms of 0.004 within 2A
Uanis(F4) \\sim Ueq, Uanis(F4A) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(F6) \\sim
Ueq, Uanis(F6A) \\sim Ueq, Uanis(C1A) \\sim Ueq, Uanis(F5) \\sim Ueq,
Uanis(F5A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(F1) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(C6) \\sim
Ueq, Uanis(F3A) \\sim Ueq, Uanis(F2A) \\sim Ueq, Uanis(F1A) \\sim Ueq: with
sigma of 0.1 and sigma for terminal atoms of 0.2
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F3A)=Sof(F2A)=Sof(F1A)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(1)
 Fixed Sof: C1(0.6) F6(0.6) F5(0.6) F4(0.6) F4A(0.4) C1A(0.4) F6A(0.4) F5A(0.4)
6.a Free rotating group:
 O1(H1A,H1B)
6.b Aromatic/amide H refined with riding coordinates:
 C00T(H00T), C00W(H00W), C00X(H00X), C00Z(H00Z), C010(H010), C012(H012),
 C013(H013), C014(H014), C015(H015), C018(H018), C019(H019), C01A(H01A),
 C01B(H01B), C01C(H01C), C01F(H01F), C01G(H01G), C01P(H01P)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 102 electrons were 
found in a volume of 514\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
[+ solvents] per Asymmetric Unit 
which account for 104 electrons 
per unit cell.
;
_shelx_res_checksum              55844
_shelx_fab_checksum              80557
_olex2_submission_special_instructions 'No special instructions were received'