Tuning the tautomeric behavior of tris(salicylaldimines)
Mehr, S. Hessam M.; Oshima, Hiroya; Carta, Veronica; Patrick, Brian O.; White, Nicholas G.; MacLachlan, Mark J.; Org. Biomol. Chem.  (2017) –; doi:10.1039/C7OB02058A

data_7155895
_publ_section_title
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 Tuning the tautomeric behavior of tris(salicylaldimines)
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_journal_name_full               'Org. Biomol. Chem.'
_journal_paper_doi               10.1039/C7OB02058A
_journal_year                    2017
_chemical_compound_source        ' synthesized '
_chemical_formula_moiety         '2(C15 H15 N3 O6), C H2 Cl2'
_chemical_formula_sum            'C31 H32 Cl2 N6 O12'
_chemical_formula_weight         751.53
_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   difmap
_atom_sites_solution_primary     direct
_audit_update_record
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2017-08-16 deposited with the CCDC.
2017-09-19 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 90.408(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   4.3393(14)
_cell_length_b                   18.049(6)
_cell_length_c                   20.965(7)
_cell_measurement_reflns_used    2308
_cell_measurement_temperature    90
_cell_measurement_theta_max      26.74
_cell_measurement_theta_min      2.26
_cell_volume                     1641.9(9)
_computing_cell_refinement       'Apex2, (Bruker, 2007)'
_computing_data_collection       'Apex2, (Bruker, 2007)'
_computing_data_reduction        'Apex2, (Bruker, 2007)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      90
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       Serial
_diffrn_measurement_device_type  'Bruker Apex Duo'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.051
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10634
_diffrn_reflns_theta_full        25.374
_diffrn_reflns_theta_max         25.374
_diffrn_reflns_theta_min         1.489
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.273
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.74
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2, (Bruker, 2007)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             780
_exptl_crystal_size_max          0.79
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.63
_refine_diff_density_min         -0.47
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         2398
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0782
_refine_ls_R_factor_gt           0.0677
_refine_ls_shift/su_max          0.0002013
_refine_ls_shift/su_mean         0.0000173
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 59.2 93.8 56.4 23.1 4.83 
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_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1341
_refine_ls_wR_factor_gt          0.1305
_refine_ls_wR_factor_ref         0.1341
_reflns_limit_h_max              5
_reflns_limit_h_min              -5
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                2086
_reflns_number_total             2983
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.09
_oxford_diffrn_Wilson_scale      3.97
_oxford_refine_ls_r_factor_ref   0.0782
_oxford_refine_ls_scale          0.4902(15)
_oxford_reflns_number_all        2398
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            c7ob02058a15.cif
_cod_data_source_block           Compound9
_cod_original_sg_symbol_Hall     ' -P 2yn '
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               7155895
_iucr_refine_instructions_details_constraints
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BLOCK SCALE X'S, U'S 
SUMFIX ELEMENT SCALES 
RIDE C   (   7,X'S) H   (  71,X'S) 
RIDE C   (   9,X'S) H   (  93,X'S) H   (  92,X'S) H   (  91,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  19,X'S) H   ( 193,X'S) H   ( 192,X'S) H   ( 191,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) 
RIDE C   (  29,X'S) H   ( 293,X'S) H   ( 292,X'S) H   ( 291,X'S) 
RIDE N   (   1,X'S) H   (  11,X'S) 
RIDE N   (  21,X'S) H   ( 211,X'S) 
RIDE N   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  30,X'S) H   ( 302,X'S) H   ( 301,X'S) 
END                                                                             
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_iucr_refine_instructions_details_restraints
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NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
U(IJ)'S  0.0, 0.010000 = C(5) TO C(17) 
VIBRATION 0.0, 0.020000 = C(5) TO C(17) 
END                                                                             
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