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_7155894
_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         'C9 H12 N6 O3'
_chemical_formula_sum            'C9 H12 N6 O3'
_chemical_formula_weight         252.23
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_update_record
;
2017-08-16 deposited with the CCDC.
2017-09-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.182(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.537(2)
_cell_length_b                   4.4790(7)
_cell_length_c                   14.849(2)
_cell_measurement_reflns_used    9911
_cell_measurement_temperature    90
_cell_measurement_theta_max      30.55
_cell_measurement_theta_min      2.66
_cell_volume                     1017.1(2)
_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    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      90
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.029
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            20240
_diffrn_reflns_theta_full        30.568
_diffrn_reflns_theta_max         30.568
_diffrn_reflns_theta_min         1.332
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.128
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.911
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2, (Bruker, 2007)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             528.0
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.44
_refine_diff_density_min         -0.35
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9843
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         3094
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0486
_refine_ls_shift/su_max          0.0006548
_refine_ls_shift/su_mean         0.0000579
_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: 
 1.16 1.45 0.355 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1092
_refine_ls_wR_factor_gt          0.1054
_refine_ls_wR_factor_ref         0.1091
_reflns_limit_h_max              21
_reflns_limit_h_min              -22
_reflns_limit_k_max              6
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                2723
_reflns_number_total             3116
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.95
_oxford_diffrn_Wilson_scale      67.55
_oxford_refine_ls_r_factor_ref   0.0578
_oxford_refine_ls_scale          0.13806(10)
_oxford_reflns_number_all        3104
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_iucr_refine_instructions_details_constraints
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BLOCK SCALE X'S 
CONT C(1,U'S) UNTIL N(18) 
CONT C(21,U[ISO]) UNTIL N(38) 
EQUIV PART(0001,OCC),PART(0002,OCC) 
WEIGHT -1 PART(0002,OCC) 
RIDE C   (   7,X'S) H   (  71,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE N   (  13,X'S) H   ( 131,X'S) 
RIDE N   (  14,X'S) H   ( 141,X'S) H   ( 142,X'S) 
RIDE N   (  15,X'S) H   ( 151,X'S) 
RIDE N   (  16,X'S) H   ( 161,X'S) H   ( 162,X'S) 
RIDE N   (  17,X'S) H   ( 171,X'S) 
RIDE N   (  18,X'S) H   ( 181,X'S) H   ( 182,X'S) 
RIDE C   (   27,X'S) H   (  271,X'S) 
RIDE C   (   28,X'S) H   (  281,X'S) 
RIDE C   (   29,X'S) H   (  291,X'S) 
RIDE N   (  34,X'S) H   ( 341,X'S) H   ( 342,X'S) 
RIDE N   (  36,X'S) H   ( 361,X'S) H   ( 362,X'S) 
RIDE N   (  38,X'S) H   ( 382,X'S) H   ( 381,X'S) 
RIDE O   (  30,X'S) H   ( 301,X'S) 
RIDE O   (  31,X'S) H   ( 311,X'S) 
RIDE O   (  32,X'S) H   ( 321,X'S) 
END   
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_iucr_refine_instructions_details_restraints
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NO 
END                                                                             
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_cod_data_source_file            c7ob02058a15.cif
_cod_data_source_block           Compound5
_cod_depositor_comments
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The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/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 4973 2017-02-22 13:04:09Z antanas 
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_cod_original_cell_volume        1017.1(3)
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_database_code               7155894