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_7241033
_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         'C27 H54 N3, 3(Br), 5(H2 O)'
_chemical_formula_sum            'C27 H64 Br3 N3 O5'
_chemical_formula_weight         750.54
_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                 105.02
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.7042(1)
_cell_length_b                   25.8169(1)
_cell_length_c                   18.0462(1)
_cell_measurement_reflns_used    76467
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.246
_cell_measurement_theta_min      3.047
_cell_volume                     7516.55(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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      -0.0549505
_diffrn_orient_matrix_UB_12      0.0039279
_diffrn_orient_matrix_UB_13      -0.0827731
_diffrn_orient_matrix_UB_21      -0.0241751
_diffrn_orient_matrix_UB_22      -0.0573977
_diffrn_orient_matrix_UB_23      0.0028169
_diffrn_orient_matrix_UB_31      -0.0742726
_diffrn_orient_matrix_UB_32      0.0157845
_diffrn_orient_matrix_UB_33      0.0308891
_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  0.0471
_diffrn_reflns_av_unetI/netI     0.0174
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            159274
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.308
_diffrn_reflns_theta_max         67.308
_diffrn_reflns_theta_min         3.214
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.248
_exptl_absorpt_correction_T_max  0.549
_exptl_absorpt_correction_T_min  0.403
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_description       block
_exptl_crystal_F_000             3136
_exptl_crystal_size_max          0.313
_exptl_crystal_size_mid          0.226
_exptl_crystal_size_min          0.189
_refine_diff_density_max         4.602
_refine_diff_density_min         -3.948
_refine_diff_density_rms         0.205
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.659
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     714
_refine_ls_number_reflns         13442
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.669
_refine_ls_R_factor_all          0.1255
_refine_ls_R_factor_gt           0.1152
_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^)+(0.0500P)^2^+50.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2551
_refine_ls_wR_factor_ref         0.2613
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11726
_reflns_number_total             13442
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00747a2.cif
_cod_data_source_block           3TEA_190718
_cod_original_cell_volume        7516.45(7)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7241033
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.350
_shelx_estimated_absorpt_t_max   0.501
_shelx_res_checksum              73071