Deciphering preferred geometries of pyridylmethylamines-based complexes: A robust strategy combining NMR, DFT and X-ray
Large, Benjamin; Meddeb, Maissa; Pucheta, José Enrique Herbert; Gaucher, Anne; Cordier, Marie; Gosmini, Corinne; Farjon, Jonathan; Auffrant, Audrey; Prim, Damien; Inorganica Chimica Acta 498 (2019) 119070–; doi:10.1016/j.ica.2019.119070

data_1565724
_publ_section_title
;
 Deciphering preferred geometries of pyridylmethylamines-based complexes:
 A robust strategy combining NMR, DFT and X-ray
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119070
_journal_paper_doi               10.1016/j.ica.2019.119070
_journal_volume                  498
_journal_year                    2019
_chemical_formula_moiety         'C14 H16 Br2 Co N2'
_chemical_formula_sum            'C14 H16 Br2 Co N2'
_chemical_formula_weight         431.04
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90.00(3)
_cell_angle_beta                 90.00(3)
_cell_angle_gamma                90.00(3)
_cell_formula_units_Z            4
_cell_length_a                   8.531(2)
_cell_length_b                   13.271(3)
_cell_length_c                   13.849(3)
_cell_measurement_reflns_used    2844
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.910
_cell_volume                     1567.9(6)
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997) & COLLECT'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction        'DENZO & COLLECT'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.0(1)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Kappa APEX II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0616
_diffrn_reflns_av_unetI/netI     0.0484
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9789
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         27.641
_diffrn_reflns_theta_min         3.197
_exptl_absorpt_coefficient_mu    6.179
_exptl_absorpt_correction_T_max  1.38265
_exptl_absorpt_correction_T_min  0.715338
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   DENZO/SCALEPACK
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.826
_exptl_crystal_description       plate
_exptl_crystal_F_000             844
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.980
_refine_diff_density_min         -0.825
_refine_diff_density_rms         0.147
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.11(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         3428
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0547
_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^)+(0.0601P)^2^+5.4493P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1331
_refine_ls_wR_factor_ref         0.1436
_reflns_Friedel_coverage         0.705
_reflns_Friedel_fraction_full    0.961
_reflns_Friedel_fraction_max     0.907
_reflns_number_gt                2996
_reflns_number_total             3428
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2019-498-119070.cif
_cod_data_source_block           aaco2_a
_cod_database_code               1565724
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.296
_shelx_estimated_absorpt_t_max   0.790
_shelx_res_checksum              44220
_shelx_hkl_checksum              91088