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_4306812
_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         'C53 H66 N2 O4 Ti1, 2 (C7 H8)'
_chemical_formula_sum            'C67 H82 N2 O4 Ti'
_chemical_formula_weight         1027.30
_chemical_name_systematic
;
(Me2calix)TiNN(Me)Ph . 2(C7H8)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 111.6514(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.9438(3)
_cell_length_b                   13.0864(2)
_cell_length_c                   23.3105(5)
_cell_measurement_reflns_used    12688
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     5938.15(18)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.985
_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  0.057
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            24932
_diffrn_reflns_theta_full        25.303
_diffrn_reflns_theta_max         27.504
_diffrn_reflns_theta_min         5.111
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.192
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.149
_exptl_crystal_description       plate
_exptl_crystal_F_000             2208
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.03
_refine_diff_density_min         -0.72
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1748
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         6447
_refine_ls_number_restraints     78
_refine_ls_R_factor_all          0.1333
_refine_ls_R_factor_gt           0.0593
_refine_ls_shift/su_max          0.000345
_refine_ls_structure_factor_coef F
_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: 
 1.23 0.802 1.03 0.192 0.217 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1076
_refine_ls_wR_factor_gt          0.0628
_refine_ls_wR_factor_ref         0.0628
_reflns_limit_h_max              25
_reflns_limit_h_min              -27
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              30
_reflns_limit_l_min              0
_reflns_number_gt                6447
_reflns_number_total             13443
_reflns_threshold_expression     I>3.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.07
_oxford_diffrn_Wilson_scale      19.33
_oxford_refine_ls_scale          0.2336(4)
_cod_data_source_file            ic801735c_si_001_3.cif
_cod_data_source_block           COMPOUND_2
_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/a 1 '
_cod_original_formula_sum        'C67 H82 N2 O4 Ti1'
_cod_database_code               4306812