A structurally characterised, naked sp3-hybridised carbanion in the zwitterionic imido complex [Ti(NBut){C(Me2pz)3}Cl(THF)] (HMe2pz = 3,5-dimethylpyrazole)
Lawrence, Sally C.; Skinner, Michael E. G.; Green, Jennifer C.; Mountford, Philip; Chemical Communications  (2001) 705–; doi:10.1039/b100315l

data_7114960
_publ_section_title
;
 A structurally characterised, naked sp3-hybridised carbanion in the
 zwitterionic imido complex [Ti(NBut){C(Me2pz)3}Cl(THF)] (HMe2pz =
 3,5-dimethylpyrazole)
;
_journal_issue                   8
_journal_name_full               'Chemical Communications'
_journal_page_first              705
_journal_paper_doi               10.1039/b100315l
_journal_year                    2001
_chemical_compound_source
;
[Ti(N-t-Bu){HC(Me2pz)3}Cl2] + MeLi in THF
;
_chemical_formula_moiety         ' C24 H38 Cl1 N7 O1 Ti1 . 0.5(C7 H8) '
_chemical_formula_sum            'C27.5 H42 Cl N7 O Ti'
_chemical_formula_weight         570.04
_chemical_name_systematic
;
[Ti(N-t-Bu){C(Me2pz)3}Cl(THF)]
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   'Fourier maps and geometric'
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 114.882(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.894(2)
_cell_length_b                   13.8900(9)
_cell_length_c                   20.0340(9)
_cell_measurement_reflns_used    20521
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      0
_cell_volume                     6031.8(7)
_computing_cell_refinement
;
DIP2000 software 'DENZO' (Otwinowski & Minor, 1996)
;
_computing_data_collection       'DIP2000 software 'Xpress (MAC Science, 1989)''
_computing_data_reduction
;
DIP2000 software 'DENZO' (Otwinowski & Minor, 1996)
;
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1994)'
_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_measurement_device_type  'Enraf-nonius DIP2000'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_av_sigmaI/netI    0.0685
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20521
_diffrn_reflns_theta_max         26.44
_diffrn_reflns_theta_min         1.74
_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    0.40
_exptl_absorpt_correction_T_max  0.905
_exptl_absorpt_correction_T_min  0.852
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'Orange '
_exptl_crystal_density_diffrn    1.26
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       'block '
_exptl_crystal_F_000             2424
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.41
_refine_diff_density_min         -0.31
_refine_ls_abs_structure_Flack   none
_refine_ls_extinction_coef       'None required'
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_obs   1.0753
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         3675
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0412
_refine_ls_shift/esd_max         0.0108
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      unit
_refine_ls_wR_factor_obs         0.0573
_reflns_limit_h_max              27
_reflns_limit_h_min              -29
_reflns_limit_k_max              17
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_observed          3675
_reflns_number_total             5737
_reflns_observed_criterion       >3.00\s(I)
_cod_data_source_file            b100315l.txt
_cod_data_source_block           COMPOUND2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic ' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z 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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'Unit weights' was changed to
'unit'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

The following automatic conversions were performed:

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

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        6031.85
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_original_formula_sum        ' C27.50 H42 Cl1 N7 O1 Ti1 '
_cod_database_code               7114960