Structural investigation of bromide complexation with bipodal, tripodal and tetrapodal cationic molecules
Ling, Irene; Sobolev, Alexandre N.; Loh, Sze Le; Turner, Gemma F.; Moggach, Stephen A.; CrystEngComm  (2020) –; doi:10.1039/D0CE00747A

data_7241034
_publ_section_title
;
 Structural investigation of bromide complexation with bipodal, tripodal
 and tetrapodal cationic molecules
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00747A
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C27 H48 N3, 3(Br), 4(H2 O)'
_chemical_formula_sum            'C27 H56 Br3 N3 O4'
_chemical_formula_weight         726.47
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-06-16 deposited with the CCDC.	2020-07-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.582(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.2861(5)
_cell_length_b                   13.4278(3)
_cell_length_c                   12.7119(3)
_cell_measurement_reflns_used    9984
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.399
_cell_measurement_theta_min      2.285
_cell_volume                     3277.20(14)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'X-Seed v. 4.0 (Barbour, 2001)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2015/1 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4738
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Gemini-R Ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.931
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19064
_diffrn_reflns_point_group_measured_fraction_full 0.744
_diffrn_reflns_point_group_measured_fraction_max 0.631
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.654
_diffrn_reflns_theta_min         2.226
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.727
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.54673
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_description       block
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.419
_exptl_crystal_size_mid          0.306
_exptl_crystal_size_min          0.167
_refine_diff_density_max         0.471
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
;
 Flack x determined using 1792 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.012(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         7579
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0240
_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^)+(0.0295P)^2^+0.2950P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0536
_refine_ls_wR_factor_ref         0.0551
_reflns_Friedel_coverage         0.354
_reflns_Friedel_fraction_full    0.487
_reflns_Friedel_fraction_max     0.331
_reflns_number_gt                7123
_reflns_number_total             7579
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00747a2.cif
_cod_data_source_block           3ME181101
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               7241034
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.304
_shelx_estimated_absorpt_t_max   0.575
_shelx_res_checksum              41731