Synthesis and Characterization of the Most Active Copper ATRP Catalyst Based on Tris[(4-dimethylaminopyridyl)methyl]amine.
Ribelli, Thomas G.; Fantin, Marco; Daran, Jean-Claude; Augustine, Kyle F.; Poli, Rinaldo; Matyjaszewski, Krzysztof; Journal of the American Chemical Society  (2018) –; doi:10.1021/jacs.7b12180

data_4127062
_publ_section_title
;
 Synthesis and Characterization of the Most Active Copper ATRP Catalyst
 Based on Tris[(4-dimethylaminopyridyl)methyl]amine.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b12180
_journal_year                    2018
_chemical_formula_sum            'C24 H35.5 Br2 Cu N7 O1.5'
_chemical_formula_weight         669.45
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d'
_symmetry_space_group_name_Hall  '-F 2uv 2vw'
_symmetry_space_group_name_H-M   'F d d d :2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            32
_cell_length_a                   17.207(5)
_cell_length_b                   24.701(5)
_cell_length_c                   55.119(5)
_cell_measurement_reflns_used    23808
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      29.1080
_cell_measurement_theta_min      3.6270
_cell_volume                     23427(9)
_computing_cell_refinement       CrysAlisPro
_computing_data_collection       'CrysAlisPro (Rigaku Oxford Diffraction, 2015)'
_computing_data_reduction        CrysAlisPro
_computing_molecular_graphics
;
ORTEPIII (Burnett & Johnson, 1996); ORTEP-3 for Windows (Farrugia, 1997);
MERCURY (Bruno et al., 2002); PLATON (Spek, 2009)
;
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2013(Sheldrick, 2014)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1978
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.908
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.908
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       74
_diffrn_reflns_limit_l_min       -72
_diffrn_reflns_number            65038
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.908
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.515
_diffrn_reflns_theta_min         2.957
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.506
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80618
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
CrysAlisPro (Rigaku Oxford Diffraction,2015)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_description       box
_exptl_crystal_F_000             10864
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.614
_refine_diff_density_min         -0.464
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         7433
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0413
_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^)+(0.0338P)^2^+171.6706P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0890
_refine_ls_wR_factor_ref         0.0947
_reflns_number_gt                5745
_reflns_number_total             7433
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b12180_si_001.cif
_cod_data_source_block           shelx
_cod_original_formula_sum        'C24 H35.50 Br2 Cu N7 O1.50'
_cod_database_code               4127062
_shelx_estimated_absorpt_t_min   0.541
_shelx_estimated_absorpt_t_max   0.678
_shelxl_version_number           2014/6
_shelx_res_checksum              42175
_shelx_hkl_checksum              68030