Optically active bis(aminophenols) and their metal complexes
Carbonel, Halen; Mikulski, Timothy D.; Nugraha, Kahargyan; Johnston, James; Wang, Yichun; Brown, Seth N.; Dalton Transactions  (2023) –; doi:10.1039/D3DT02436A

data_7713822
_publ_section_title
;
 Optically active bis(aminophenols) and their metal complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02436A
_journal_year                    2023
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C46 H56 N2 O6 Pd, 0.25(C H4 O)'
_chemical_formula_sum            'C46.25 H57 N2 O6.25 Pd'
_chemical_formula_weight         847.34
_chemical_name_common            '(C,R,R)-(Bdan)Pd . 0.25 CH3OH'
_chemical_name_systematic
'(C,R,R)-[2,3-butanediyl-di-2-(2-oxy-3,5-di-tert-butylphenyl-imino)benzoate]palladium hemidemimethanol solvate'
_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   mixed
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2023-07-14 deposited with the CCDC.	2023-08-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.7503(5)
_cell_length_b                   19.4021(6)
_cell_length_c                   31.1892(11)
_cell_measurement_reflns_used    9863
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.02
_cell_measurement_theta_min      2.17
_cell_volume                     8925.9(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1088
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            287291
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.319
_diffrn_reflns_theta_min         1.306
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.463
_exptl_absorpt_correction_T_max  0.8576
_exptl_absorpt_correction_T_min  0.7721
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. 
& Stalke D., J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3556
_exptl_crystal_recrystallization_method
'Crystals deposited from a solution of the crude reactionmixture in methanol.'
_exptl_crystal_size_max          0.162
_exptl_crystal_size_mid          0.084
_exptl_crystal_size_min          0.065
_exptl_transmission_factor_max   0.8576
_exptl_transmission_factor_min   0.7721
_refine_diff_density_max         0.380
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
; 
 Flack x determined using 8077 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   0.020(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1422
_refine_ls_number_reflns         22201
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0384
_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^)+(0.0197P)^2^+5.6145P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0661
_refine_ls_wR_factor_ref         0.0693
_reflns_Friedel_coverage         0.846
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                19585
_reflns_number_total             22201
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02436a2.cif
_cod_data_source_block           bdanpd
_cod_database_code               7713822
_shelx_estimated_absorpt_t_min   0.929
_shelx_estimated_absorpt_t_max   0.971
_shelxl_version_number           2013-4
_shelx_res_checksum              72998