Synthesis of chiral-at-metal rhodium complexes from achiral tripodal tetradentate ligands: resolution and application to enantioselective Diels–Alder and 1,3-dipolar cycloadditions
Tejero, Alvaro G.; Carmona, María; Rodríguez, Ricardo; Viguri, Fernando; Lahoz, Fernando J.; García-Orduña, Pilar; Carmona, Daniel; RSC Advances 12 (2022) 34704–34714; doi:10.1039/D2RA06982B

data_7245948
_publ_section_title
;
 Synthesis of chiral-at-metal rhodium complexes from achiral tripodal
 tetradentate ligands: resolution and application to enantioselective
 Diels--Alder and 1,3-dipolar cycloadditions
;
_journal_issue                   53
_journal_name_full               'RSC Advances'
_journal_page_first              34704
_journal_page_last               34714
_journal_paper_doi               10.1039/D2RA06982B
_journal_volume                  12
_journal_year                    2022
_chemical_formula_moiety         'C37 H33 F3 N4 P Rh,2(F6 Sb),2(C H2 Cl2)'
_chemical_formula_sum            'C39 H37 Cl4 F15 N4 P Rh Sb2'
_chemical_formula_weight         1365.90
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-09-12 deposited with the CCDC.	2022-11-24 downloaded from the CCDC.
;
_cell_angle_alpha                96.0690(10)
_cell_angle_beta                 102.032(2)
_cell_angle_gamma                92.269(2)
_cell_formula_units_Z            2
_cell_length_a                   12.2805(9)
_cell_length_b                   13.6365(9)
_cell_length_c                   14.6021(10)
_cell_measurement_reflns_used    6927
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.745
_cell_measurement_theta_min      2.340
_cell_volume                     2373.4(3)
_computing_cell_refinement       'SAINT+ in APEX3 v. 2017.3 (Bruker AXS, 2008)'
_computing_data_collection       'SMART in APEX2 v. 2008.4 (Bruker AXS, 2008)'
_computing_data_reduction        'SAINT+ in APEX3 v. 2017.3 (Bruker AXS, 2008)'
_computing_molecular_graphics    'ORTEP-3 (farrugia, 2012)'
_computing_publication_material  'XCIF program, PLATON(Spek, 1998)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker APEX CCD system'
_diffrn_measurement_method       'narrow \w frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_av_unetI/netI     0.0632
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            32424
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.187
_diffrn_reflns_theta_min         1.436
_exptl_absorpt_coefficient_mu    1.826
_exptl_absorpt_correction_T_max  0.8373
_exptl_absorpt_correction_T_min  0.7569
_exptl_absorpt_correction_type   multi-scan
_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            colourless
_exptl_crystal_density_diffrn    1.911
_exptl_crystal_description       prism
_exptl_crystal_F_000             1328
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane/acetone'
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.070
_refine_diff_density_max         2.977
_refine_diff_density_min         -1.679
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     597
_refine_ls_number_reflns         12574
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0800
_refine_ls_R_factor_gt           0.0485
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0526P)^2^+4.4625P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1051
_refine_ls_wR_factor_ref         0.1180
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9063
_reflns_number_total             12574
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ra06982b2.cif
_cod_data_source_block           cmpnd_2
_cod_database_code               7245948
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              60915