Metal‒Ligand Cooperativity in Titanium-Catalyzed Anti-Markovnikov Hydroamination
Hao, Han; Schafer, Laurel L.; ACS Catalysis  (2020) 7100–; doi:10.1021/acscatal.0c00491

data_4517771
_publ_section_title
;
 Metal--Ligand Cooperativity in Titanium-Catalyzed Anti-Markovnikov
 Hydroamination
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              7100
_journal_paper_doi               10.1021/acscatal.0c00491
_journal_year                    2020
_chemical_formula_moiety         'C49 H59 Cl N4 O2 Ti'
_chemical_formula_sum            'C49 H59 Cl N4 O2 Ti'
_chemical_formula_weight         819.35
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-06-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 98.625(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.1679(7)
_cell_length_b                   10.1706(3)
_cell_length_c                   23.0399(8)
_cell_measurement_reflns_used    9936
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      2.19
_cell_volume                     4440.8(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_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  0.0785
_diffrn_reflns_av_unetI/netI     0.0695
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            59801
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.402
_diffrn_reflns_theta_min         1.497
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.296
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6640
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0717 before and 0.0571 after correction. The Ratio of minimum to maximum transmission is 0.8904. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.314
_refine_diff_density_min         -0.433
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     526
_refine_ls_number_reflns         11110
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0883
_refine_ls_R_factor_gt           0.0454
_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^)+(0.0450P)^2^+0.8040P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0955
_refine_ls_wR_factor_ref         0.1129
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7242
_reflns_number_total             11110
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs0c00491_si_003.cif
_cod_data_source_block           ls843
_cod_database_code               4517771
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.977
_shelx_estimated_absorpt_t_min   0.965
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C00I(H00I), C00S(H00S), C00Y(H00Y), C019(H019)
2.b Secondary CH2 refined with riding coordinates:
 C00V(H00A,H00B), C010(H01A,H01B), C012(H01C,H01D), C016(H01H,H01I), C01B(H01N,
 H01O)
2.c Aromatic/amide H refined with riding coordinates:
 C00K(H00K), C00L(H00L), C00N(H00N), C00O(H00O), C00P(H00P), C00Q(H00Q),
 C00R(H00R), C00T(H00T), C00U(H00U), C00W(H00W), C00X(H00X), C00Z(H00Z),
 C011(H011), C014(H014), C017(H017), C01A(H01M), C01C(H01P), C01G(H01Z),
 C01H(H01), C01L(H3AA)
2.d Idealised Me refined as rotating group:
 C015(H01E,H01F,H01G), C018(H01J,H01K,H01L), C01D(H01Q,H01R,H01S), C01E(H01T,
 H01U,H01V), C01F(H01W,H01X,H01Y), C01I(H0AA,H,HA), C01J(H1AA,HB,HC), C01K(H2AA,
 HD,HE)
;
_shelx_res_checksum              18455
_shelx_hkl_checksum              86979
_olex2_submission_special_instructions 'No special instructions were received'