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_7241028
_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_formula_moiety         'C20 H34 N2, 2(Br), 2(H2 O)'
_chemical_formula_sum            'C20 H38 Br2 N2 O2'
_chemical_formula_weight         498.34
_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_method           SHELXL-2018/3
_audit_update_record
;
2020-02-17 deposited with the CCDC.	2020-07-31 downloaded from the CCDC.
;
_cell_angle_alpha                93.527(4)
_cell_angle_beta                 96.309(4)
_cell_angle_gamma                101.198(4)
_cell_formula_units_Z            2
_cell_length_a                   6.6197(3)
_cell_length_b                   12.7852(6)
_cell_length_c                   13.6584(6)
_cell_measurement_reflns_used    9079
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.495
_cell_measurement_theta_min      2.336
_cell_volume                     1123.02(9)
_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 16.0009
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur-S'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0290217
_diffrn_orient_matrix_UB_12      -0.0562404
_diffrn_orient_matrix_UB_13      -0.0109525
_diffrn_orient_matrix_UB_21      0.0988078
_diffrn_orient_matrix_UB_22      -0.0007034
_diffrn_orient_matrix_UB_23      -0.0152269
_diffrn_orient_matrix_UB_31      0.0389037
_diffrn_orient_matrix_UB_32      -0.0076322
_diffrn_orient_matrix_UB_33      0.0489681
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_av_unetI/netI     0.0582
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.914
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25169
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.809
_diffrn_reflns_theta_min         3.162
_exptl_absorpt_coefficient_mu    3.626
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.8753
_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    1.474
_exptl_crystal_description       block
_exptl_crystal_F_000             516
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.182
_exptl_crystal_size_min          0.160
_refine_diff_density_max         1.007
_refine_diff_density_min         -0.732
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         7631
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0404
_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^)+(0.0350P)^2^+0.9800P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0817
_refine_ls_wR_factor_ref         0.0944
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5796
_reflns_number_total             7631
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00747a2.cif
_cod_data_source_block           PME181031
_cod_database_code               7241028
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.419
_shelx_estimated_absorpt_t_max   0.595
_shelx_res_checksum              99183