Iterative Supervised Principal Component Analysis Driven Ligand Design for Regioselective Ti-Catalyzed Pyrrole Synthesis
See, Xin Yi; Wen, Xuelan; Wheeler, T. Alexander; Klein, Channing K.; Goodpaster, Jason D.; Reiner, Benjamin R.; Tonks, Ian A.; ACS Catalysis 10 (2020) 13504–13517; doi:10.1021/acscatal.0c03939

data_4518202
_publ_section_title
;
 Iterative Supervised Principal Component Analysis Driven Ligand Design
 for Regioselective Ti-Catalyzed Pyrrole Synthesis
;
_journal_issue                   22
_journal_name_full               'ACS Catalysis'
_journal_page_first              13504
_journal_page_last               13517
_journal_paper_doi               10.1021/acscatal.0c03939
_journal_volume                  10
_journal_year                    2020
_chemical_formula_moiety         'C80 H78 Cl N2 O3 P3 Ti2'
_chemical_formula_sum            'C80 H78 Cl N2 O3 P3 Ti2'
_chemical_formula_weight         1339.60
_chemical_name_common            Ti(NtBu)(O^P)3Ti(NtBu)Cl
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 114.010(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.117(3)
_cell_length_b                   15.0952(14)
_cell_length_c                   20.943(2)
_cell_measurement_reflns_used    9953
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      29.7265
_cell_measurement_theta_min      2.2885
_cell_volume                     6964.6(13)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'APEX3, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      125(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Photon-II CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1029
_diffrn_reflns_av_unetI/netI     0.0386
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            423837
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.558
_diffrn_reflns_theta_min         2.147
_diffrn_source                   micro
_exptl_absorpt_coefficient_mu    0.387
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_description       Cube
_exptl_crystal_F_000             2808
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.050
_exptl_transmission_factor_max   0.7449
_exptl_transmission_factor_min   0.7125
_refine_diff_density_max         1.025
_refine_diff_density_min         -0.747
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.227
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     899
_refine_ls_number_reflns         21340
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.226
_refine_ls_R_factor_all          0.0911
_refine_ls_R_factor_gt           0.0747
_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^)+22.2094P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1468
_refine_ls_wR_factor_ref         0.1525
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17896
_reflns_number_total             21340
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            e.cif
_cod_data_source_block           19131a_a
_cod_depositor_comments
'Adding full bibliography for 4518200--4518203.cif.'
_cod_original_cell_volume        6964.5(12)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4518202
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.962
_shelx_estimated_absorpt_t_max   0.981
_shelx_res_checksum              34002
_shelx_hkl_checksum              54048