Cycloaddition reactions of titanium and zirconium imido, oxo and hydrazido complexes supported by tetraaza macrocyclic ligands ‡
Blake, Alexander J.; McInnes, Jacqueline M.; Mountford, Philip; Nikonov, Georgii I.; Swallow, Daniel; Watkin, David J.; Journal of the Chemical Society, Dalton Transactions  (1999) 379–; doi:10.1039/a806827e

data_7027102
_publ_contact_author
;
 Dr P Mountford
 School of Chemistry
 University of Nottingham
 Nottingham
 NG7 2RD
;
_publ_section_title
;
 Cycloaddition reactions of titanium and zirconium imido, oxo and
 hydrazido complexes supported by tetraaza macrocyclic
 ligands&#x200A;&#x2021;
;
_journal_issue                   3
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              379
_journal_paper_doi               10.1039/a806827e
_journal_year                    1999
_chemical_compound_source
;
 [Ti(NTol)(Me4taa)] + CO2
;
_chemical_formula_moiety         ' C30 H28 Ti1 O2 N5 '
_chemical_formula_sum            'C30 H28 N5 O2 Ti'
_chemical_formula_weight         538.49
_chemical_melting_point          ?
_chemical_name_systematic
;
 [Ti{N(Tol)C(O)O}(Me4taa)]
;
_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
_audit_creation_date             98-06-09
_audit_creation_method           CRYSTALS_ver_07-07-97
_cell_angle_alpha                67.19(4)
_cell_angle_beta                 76.02(4)
_cell_angle_gamma                73.68(2)
_cell_formula_units_Z            2
_cell_length_a                   8.920(2)
_cell_length_b                   12.903(3)
_cell_length_c                   13.55(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173
_cell_measurement_theta_max      40
_cell_measurement_theta_min      8
_cell_volume                     1364.1(12)
_computing_cell_refinement       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_collection       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_reduction
;
RC93 (Watkin, D.J., Prout, C.K., Lilley, P.M.deQ. 1994)
;
_computing_molecular_graphics
;
 CAMERON (Watkin, Prout & Pearce,  1996)
;
_computing_publication_material
;
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)
;
_computing_structure_refinement
;
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)
;
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_device       'Enraf-nonius CAD4 '
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.03
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5433
_diffrn_reflns_theta_max         75.00
_diffrn_reflns_theta_min         0.00
_diffrn_standards_decay_%        3.57
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.94
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.40
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
; 
 refined from delta-F (Walker & Stuart , 1983)'
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.31
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             562
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.80
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.46
_refine_diff_density_min         -0.47
_refine_ls_abs_structure_Flack   none
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.106
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         3045
_refine_ls_number_restraints     none
_refine_ls_R_factor_obs          0.0670
_refine_ls_shift/esd_max         0.002
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'chebychev polynomial'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0736
_reflns_limit_h_max              11
_reflns_limit_h_min              -10
_reflns_limit_k_max              16
_reflns_limit_k_min              -14
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_observed          2677
_reflns_number_total             5233
_reflns_observed_criterion       >2.00\s(I)
_cod_data_source_file            806827esup1.cif
_cod_data_source_block           Compound_14
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_symmetry_cell_setting' value
'Triclinic' changed to 'triclinic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        1364.5(22)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        ' C30 H28 Ti1 O2 N5 '
_cod_database_code               7027102