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_4023592
_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         'C34 H54 N12 O12 Ti'
_chemical_formula_sum            'C34 H54 N12 O12 Ti'
_chemical_formula_weight         870.79
_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                89.161(5)
_cell_angle_beta                 76.392(5)
_cell_angle_gamma                82.305(5)
_cell_formula_units_Z            2
_cell_length_a                   10.580(3)
_cell_length_b                   12.585(3)
_cell_length_c                   18.065(4)
_cell_measurement_temperature    173(1)
_cell_volume                     2316.2(10)
_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 0.966
_diffrn_measured_fraction_theta_max 0.966
_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  0.1459
_diffrn_reflns_av_sigmaI/netI    0.2353
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            27170
_diffrn_reflns_theta_full        27.91
_diffrn_reflns_theta_max         27.91
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    0.251
_exptl_absorpt_correction_T_max  0.9875
_exptl_absorpt_correction_T_min  0.9445
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.631
_refine_diff_density_min         -0.497
_refine_diff_density_rms         0.127
_refine_ls_extinction_coef       0.028(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     534
_refine_ls_number_reflns         10718
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.3359
_refine_ls_R_factor_gt           0.1618
_refine_ls_shift/su_max          0.175
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4253
_refine_ls_wR_factor_ref         0.4964
_reflns_number_gt                3015
_reflns_number_total             10718
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo800966s-File005.cif
_cod_data_source_block           L72Ti2OiPr4
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 
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_cod_database_code               4023592