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_1520703
_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
; 
4(C33 H45 N7 O3 Ti), 4(C7 H8), 0.5(C6 H14), H2 O 
;
_chemical_formula_sum            'C163 H221 N28 O13 Ti4'
_chemical_formula_weight         2972.28
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.583(5)
_cell_angle_beta                 78.919(5)
_cell_angle_gamma                76.303(5)
_cell_formula_units_Z            2
_cell_length_a                   19.976(4)
_cell_length_b                   20.518(4)
_cell_length_c                   21.236(4)
_cell_measurement_reflns_used    9931
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      22.98
_cell_measurement_theta_min      2.34
_cell_volume                     8292(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.1324
_diffrn_reflns_av_sigmaI/netI    0.0969
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            186553
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    0.251
_exptl_absorpt_correction_T_max  0.9514
_exptl_absorpt_correction_T_min  0.9284
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.190
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block'
_exptl_crystal_F_000             3174
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.654
_refine_diff_density_min         -4.072
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1754
_refine_ls_number_reflns         29250
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.352
_refine_ls_R_factor_all          0.1963
_refine_ls_R_factor_gt           0.1169
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1932P)^2^+26.0719P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3106
_refine_ls_wR_factor_ref         0.3742
_reflns_number_gt                15911
_reflns_number_total             29250
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol5b01229_si_002.cif
_cod_data_source_block           t
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

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

 Adding full bibliography for 1520702--1520703.cif.
;
_cod_database_code               1520703