Synthesis and Conformational Analysis of Constrained Ethylene-Bridged Bis(hydroxylamino-1,3,5-triazine) Compounds as Tetradentate Ligands; Structure of Rigid Dinuclear Ti(IV) Complex
Tal Hermon; Edit Y. Tshuva; Journal of Organic Chemistry 73 (2008) 5953–5958; doi:10.1021/jo800966s

data_4023591
_publ_section_title
;
 Synthesis and Conformational Analysis of Constrained
 Ethylene-Bridged Bis(hydroxylamino-1,3,5-triazine) Compounds as
 Tetradentate Ligands; Structure of Rigid Dinuclear Ti(IV) Complex
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              5953
_journal_page_last               5958
_journal_paper_doi               10.1021/jo800966s
_journal_volume                  73
_journal_year                    2008
_chemical_formula_moiety         'C18 H32 N12 O4 Ti, 0.5(C4 H8 O)'
_chemical_formula_sum            'C20 H36 N12 O4.5 Ti'
_chemical_formula_weight         564.51
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 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                 92.9260(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.0304(9)
_cell_length_b                   14.6037(9)
_cell_length_c                   25.6883(16)
_cell_measurement_temperature    173(1)
_cell_volume                     5256.6(6)
_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      173(1)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0298
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            29915
_diffrn_reflns_theta_full        28.04
_diffrn_reflns_theta_max         28.04
_diffrn_reflns_theta_min         2.52
_exptl_absorpt_coefficient_mu    0.380
_exptl_absorpt_correction_T_max  0.9523
_exptl_absorpt_correction_T_min  0.9111
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2384
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.390
_refine_diff_density_min         -0.315
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.169
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         6265
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.169
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0505
_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^)+(0.0476P)^2^+6.4884P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1140
_refine_ls_wR_factor_ref         0.1170
_reflns_number_gt                5750
_reflns_number_total             6265
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo800966s-File004.cif
_cod_data_source_block           TiL42
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

2021-12-16
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_original_formula_moiety     '2(C18 H32 N12 O4 Ti), C4 H8 O'
_cod_original_formula_sum        'C40 H72 N24 O9 Ti2'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     1129.02
_cod_database_code               4023591