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_7241035
_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         'C33 H60 N3, 3(Br), 4(H2 O)'
_chemical_formula_sum            'C33 H68 Br3 N3 O4'
_chemical_formula_weight         810.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2020-07-23 deposited with the CCDC.	2020-07-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.973(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9316(1)
_cell_length_b                   13.8145(1)
_cell_length_c                   21.7060(2)
_cell_measurement_reflns_used    25784
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.187
_cell_measurement_theta_min      3.781
_cell_volume                     3877.08(5)
_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-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Gemini-R Ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1133646
_diffrn_orient_matrix_UB_12      0.0265018
_diffrn_orient_matrix_UB_13      0.0127787
_diffrn_orient_matrix_UB_21      -0.0306057
_diffrn_orient_matrix_UB_22      -0.0290442
_diffrn_orient_matrix_UB_23      -0.0663581
_diffrn_orient_matrix_UB_31      -0.0202993
_diffrn_orient_matrix_UB_32      -0.1043549
_diffrn_orient_matrix_UB_33      0.0216969
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'fine-focus sealed X-ray tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0455
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            50223
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.288
_diffrn_reflns_theta_max         67.288
_diffrn_reflns_theta_min         3.950
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.142
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.82266
_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    1.389
_exptl_crystal_description       plate
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.167
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.047
_refine_diff_density_max         1.744
_refine_diff_density_min         -1.625
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         6917
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0599
_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^)+(0.0860P)^2^+17.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1531
_refine_ls_wR_factor_ref         0.1633
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5926
_reflns_number_total             6917
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00747a2.cif
_cod_data_source_block           3BP181106
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7241035
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.545
_shelx_estimated_absorpt_t_max   0.829
_shelx_res_checksum              28904