Directed Amination of Aryl Methyl Ethers Mediated by Ti(NMe2)4 at Room Temperature.
Chen, Zhou; Liu, Jinna; Pei, Hao; Liu, Wei; Chen, Yanmei; Wu, Jian; Li, Wu; Li, Yahong; Organic letters 17 (2015) 3406–3409; doi:10.1021/acs.orglett.5b01229

data_1520702
_publ_section_title
;
 Directed Amination of Aryl Methyl Ethers Mediated by Ti(NMe2)4 at Room
 Temperature.
;
_journal_issue                   14
_journal_name_full               'Organic letters'
_journal_page_first              3406
_journal_page_last               3409
_journal_paper_doi               10.1021/acs.orglett.5b01229
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'C41 H60 N8 O3 Ti2'
_chemical_formula_sum            'C41 H60 N8 O3 Ti2'
_chemical_formula_weight         808.77
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.793(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.8643(6)
_cell_length_b                   9.0349(2)
_cell_length_c                   24.8875(7)
_cell_measurement_reflns_used    2804
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      21.001
_cell_measurement_theta_min      2.322
_cell_volume                     4276.1(2)
_computing_cell_refinement       'Bruker SMART (Bruker, 2005)'
_computing_data_collection       'Bruker SMART APEX-II (Bruker, 2005)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2005)'
_computing_molecular_graphics    'Bruker SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'Bruker SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'Bruker SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'Bruker SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0832
_diffrn_reflns_av_unetI/netI     0.0791
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            41087
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.55
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.419
_exptl_absorpt_correction_T_max  0.9246
_exptl_absorpt_correction_T_min  0.9024
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2005)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.655
_refine_diff_density_min         -0.730
_refine_diff_density_rms         0.065
_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     500
_refine_ls_number_reflns         10591
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1046
_refine_ls_R_factor_gt           0.0552
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0651P)^2^+0.0838P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1262
_refine_ls_wR_factor_ref         0.1492
_reflns_number_gt                6329
_reflns_number_total             10591
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol5b01229_si_003.cif
_cod_data_source_block           ccdc843692
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 1520702--1520703.cif.
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1520702