Reactions of cyclopentadienyl-amidinate titanium imido compounds with CO2: cycloaddition-extrusion vs. cycloaddition-insertion
Guiducci, Aldo E.; Boyd, Catherine L.; Clot, Eric; Mountford, Philip; Dalton Transactions  (2009) 5960–5979; doi:10.1039/b901774g

data_7001742
_publ_section_title
;
 Reactions of cyclopentadienyl-amidinate titanium imido compounds with
 CO2: cycloaddition-extrusion vs. cycloaddition-insertion
;
_journal_issue                   30
_journal_name_full               'Dalton Transactions'
_journal_page_first              5960
_journal_page_last               5979
_journal_paper_doi               10.1039/b901774g
_journal_year                    2009
_chemical_formula_moiety         ' C29 H39 N3 O4 Si2 Ti1 '
_chemical_formula_sum            'C29 H39 N3 O4 Si2 Ti'
_chemical_formula_weight         597.72
_chemical_name_common
(Ti(C5H4Me)(PhC(NSiMe3)2)(OC(O)N(-2,6-C6H3Me2)C(O)O))
_chemical_name_systematic
;
[Ti(C5H4Me){PhC(NSiMe3)2}{OC(O)N(-2,6-C6H3Me2)C(O)O}]
;
_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
_cell_angle_alpha                90
_cell_angle_beta                 90.704
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7126(2)
_cell_length_b                   17.2231(4)
_cell_length_c                   16.6483(4)
_cell_measurement_reflns_used    6533
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.85
_cell_measurement_theta_min      2.91
_cell_volume                     3071.45(12)
_computing_cell_refinement
;
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996)
;
_computing_data_collection
;
KappaCCD software 'Collect' (Nonius, 2000)
;
_computing_data_reduction
;
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996)
;
_computing_molecular_graphics    'CAMERON (Watkin, Prout and Pearce, 1996)'
_computing_publication_material
;
CRYSTALS Issue 10 (Watkin et al, 1996)
;
_computing_structure_refinement
;
CRYSTALS Issue 10 (Watkin et al, 1996)
;
_computing_structure_solution    'SIR92 (Altomare, et al, 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       CCD
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.05
_diffrn_reflns_av_sigmaI/netI    0.107
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11752
_diffrn_reflns_theta_full        27.490
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.04
_diffrn_standards_decay_%        'not measured'
_diffrn_standards_interval_count 'not measured'
_diffrn_standards_interval_time  'not measured'
_diffrn_standards_number         'not measured'
_exptl_absorpt_coefficient_mu    0.394
_exptl_absorpt_correction_T_max  0.925
_exptl_absorpt_correction_T_min  0.925
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_exptl_crystal_colour            'yellow '
_exptl_crystal_density_diffrn    1.29
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.30
_refine_diff_density_min         -0.28
_refine_ls_extinction_coef       192.5(126)
_refine_ls_extinction_method     'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_obs   0.9819
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         4207
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0396
_refine_ls_shift/esd_max         0.004
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979,
12.3 -15.2 13.2
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0478
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              22
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_observed          4207
_reflns_number_total             7025
_reflns_observed_criterion       >3.00\s(I)
_cod_data_source_file            b901774g.txt
_cod_data_source_block           compound_21
_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 

The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'direct methods' was changed to
'direct'.

'_atom_sites_solution_hydrogens' value 'geometric' was changed to
'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 

The following automatic conversions were performed:

data name '_diffrn_measurement_device-type' was replaced with
'_diffrn_measurement_device_type' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_cell_volume        3071.5
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        ' C29 H39 N3 O4 Si2 Ti1 '
_cod_database_code               7001742