Synthesis and characterisation of a mesocyclic tripodal triamine ligand.
Ure, Andrew D.; Lázaro, Isabel Abánades; Cotter, Michelle; McDonald, Aidan R.; Organic & biomolecular chemistry 14 (2015) 483–494; doi:10.1039/c5ob01556a

data_7154762
_publ_section_title
;
 Synthesis and characterisation of a mesocyclic tripodal triamine ligand.
;
_journal_issue                   2
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              483
_journal_page_last               494
_journal_paper_doi               10.1039/c5ob01556a
_journal_volume                  14
_journal_year                    2015
_chemical_formula_sum            'C8 H22 Br6 N3'
_chemical_formula_weight         675.69
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-07-27 deposited with the CCDC.
2015-10-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   19.6192(13)
_cell_length_b                   19.6192(13)
_cell_length_c                   22.6973(15)
_cell_measurement_temperature    100(2)
_cell_volume                     7566.0(9)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            26536
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.329
_diffrn_reflns_theta_min         1.497
_exptl_absorpt_coefficient_mu    14.323
_exptl_crystal_density_diffrn    2.669
_exptl_crystal_F_000             5634
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         3.244
_refine_diff_density_min         -3.160
_refine_diff_density_rms         0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     132
_refine_ls_number_reflns         4199
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0450
_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^)+(0.0662P)^2^+166.1049P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1347
_refine_ls_wR_factor_ref         0.1404
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3528
_reflns_number_total             4199
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ob01556a2.cif
_cod_data_source_block           tcd32_a
_cod_depositor_comments
;
Adding full bibliography for 7154759--7154762.cif.

2018-03-12
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C24 H20 Br3 N6'
_cod_original_formula_weight         632.18
_cod_original_formula_units_Z            18
_cod_original_cell_volume        7566.0(11)
_cod_database_code               7154762
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.223
_shelx_estimated_absorpt_t_max   0.328
_shelx_res_checksum              82709