Tritopic ion-pair receptors based on anion-π interactions for selective CaX<sub>2</sub> binding.
Luo, Jian; Ao, Yu-Fei; Malm, Christian; Hunger, Johannes; Wang, Qi-Qiang; Wang, De-Xian; Dalton transactions (Cambridge, England : 2003) 47 (2018) 7883–7887; doi:10.1039/c8dt01727a

data_7046409
_publ_section_title
;
 Tritopic ion-pair receptors based on anion-\p interactions for selective
 CaX<sub>2</sub> binding.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7883
_journal_page_last               7887
_journal_paper_doi               10.1039/c8dt01727a
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C23 H28 Br2 Ca Cl2 N6 O9, H2 O'
_chemical_formula_sum            'C23 H30 Br2 Ca Cl2 N6 O10'
_chemical_formula_weight         821.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-09-14
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-03-28 deposited with the CCDC.
2018-05-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.521(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.081(4)
_cell_length_b                   7.8133(15)
_cell_length_c                   23.448(5)
_cell_measurement_reflns_used    9821
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.4838
_cell_measurement_theta_min      1.1583
_cell_volume                     3220.7(12)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'CIFTAB (Sheldrick, 2013)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'MM007-HF CCD(Saturn 724+)'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            21205
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         1.888
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    2.903
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7606
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.694
_exptl_crystal_description       block
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.232
_exptl_crystal_size_mid          0.166
_exptl_crystal_size_min          0.147
_refine_diff_density_max         1.189
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         7261
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0411P)^2^+2.8904P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.0903
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6680
_reflns_number_total             7261
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01727a2.cif
_cod_data_source_block           mx6282e
_cod_depositor_comments
'Adding full bibliography for 7046407--7046410.cif.'
_cod_original_cell_volume        3220.7(11)
_cod_database_code               7046409
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.675
_shelx_estimated_absorpt_t_min   0.552
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O9-H9
 0.85 with sigma of 0.01
 C23-H9
 1.891852 with sigma of 0.02
 Ca1-H9
 2.823801 with sigma of 0.02
3.a Free rotating group:
 O10(H10C,H10D)
3.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B),
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B)
3.c Aromatic/amide H refined with riding coordinates:
 C18(H18), C19(H19), C20(H20), C22(H22)
3.d Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C)
;
_shelx_res_checksum              41370
_olex2_submission_special_instructions 'No special instructions were received'