Synthesis, Structures and Reactivity of Group 4 Hydrazido Complexes Supported by Calix[4]arene Ligands
Andrew J. Clulow; Jonathan D. Selby; Michael G. Cushion; Andrew D. Schwarz; Philip Mountford; Inorganic Chemistry 47 (2008) 12049–12062; doi:10.1021/ic801735c

data_4306815
_publ_contact_author
;
 Prof P. Mountford           
 Chemistry Reaearch Laboratory
 Mansfield Road
 Oxford
 OX1 3TA
 UK
;
_publ_contact_author_email       Philip.Mountford@chem.ox.ac.uk
_publ_contact_author_fax         '+44 1865 285141'
_publ_contact_author_phone       '+44 1865 285140'
_publ_section_title
;
Synthesis, Structures and Reactivity of Group 4 Hydrazido Complexes
Supported by Calix[4]arene Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12049
_journal_page_last               12062
_journal_paper_doi               10.1021/ic801735c
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety
'C51 H70 F3 N2 O7 S1 Ti1, C10.5 H10.5, CF3O3S'
_chemical_formula_sum            'C62.5 H80.5 F6 N2 O10 S2 Ti'
_chemical_formula_weight         1245.85
_chemical_name_systematic
;
[Ti(NNMe3)(Me3Calix)(OTf)][OTf]
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 108.1990(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.998(3)
_cell_length_b                   25.675(6)
_cell_length_c                   16.425(3)
_cell_measurement_reflns_used    22722
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     6409(2)
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.106
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            47114
_diffrn_reflns_theta_full        26.674
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         5.107
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.272
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_description       block
_exptl_crystal_F_000             2630
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.13
_refine_diff_density_min         -0.94
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.8943
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     766
_refine_ls_number_reflns         14582
_refine_ls_number_restraints     72
_refine_ls_R_factor_all          0.1676
_refine_ls_R_factor_gt           0.0677
_refine_ls_shift/su_max          0.0046
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.08P)^2^ + 0.00P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1885
_refine_ls_wR_factor_gt          0.1626
_refine_ls_wR_factor_ref         0.1885
_reflns_limit_h_max              19
_reflns_limit_h_min              -20
_reflns_limit_k_max              33
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                6083
_reflns_number_total             14582
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.27
_oxford_diffrn_Wilson_scale      12.75
_oxford_refine_ls_scale          0.13703(7)
_cod_data_source_file            ic801735c_si_001_6.cif
_cod_data_source_block           COMPOUND_9
_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 
;
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C62.50 H80.50 F6 N2 O10 S2 Ti1'
_cod_database_code               4306815