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_7241030
_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         'C42 H78 N4, 4(Br), 6(H2 O)'
_chemical_formula_sum            'C42 H90 Br4 N4 O6'
_chemical_formula_weight         1066.81
_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                100.650(2)
_cell_angle_beta                 106.613(2)
_cell_angle_gamma                99.807(2)
_cell_formula_units_Z            1
_cell_length_a                   7.7789(2)
_cell_length_b                   12.3790(3)
_cell_length_c                   13.5879(4)
_cell_measurement_reflns_used    11231
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.336
_cell_measurement_theta_min      2.642
_cell_volume                     1197.13(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'X-Seed v. 4.0 (Barbour, 2001)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.920
_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      -0.0129815
_diffrn_orient_matrix_UB_12      -0.0586971
_diffrn_orient_matrix_UB_13      -0.0214800
_diffrn_orient_matrix_UB_21      0.0215569
_diffrn_orient_matrix_UB_22      -0.0089641
_diffrn_orient_matrix_UB_23      0.0517751
_diffrn_orient_matrix_UB_31      -0.0946565
_diffrn_orient_matrix_UB_32      -0.0087072
_diffrn_orient_matrix_UB_33      -0.0043284
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.920
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            24538
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.920
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.742
_diffrn_reflns_theta_min         2.049
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.409
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.80326
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_description       needle
_exptl_crystal_F_000             558
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.246
_exptl_crystal_size_min          0.174
_refine_diff_density_max         0.547
_refine_diff_density_min         -0.631
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         8146
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0314
_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^)+(0.0343P)^2^+0.6000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0696
_refine_ls_wR_factor_ref         0.0762
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6637
_reflns_number_total             8146
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00747a2.cif
_cod_data_source_block           171031A
_cod_database_code               7241030
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.418
_shelx_estimated_absorpt_t_max   0.588
_shelx_res_checksum              76398