Group 4 Imido Complexes Stabilized by a Tridentate Diamido-Donor Ligand
Alexander J. Blake; Philip E. Collier; Lutz H. Gade; Philip Mountford; Julian Lloyd; Stephen M. Pugh; Martin Schubart; Michael E. G. Skinner; Dominique J. M. Trösch; Inorganic Chemistry 40 (2001) 870–877; doi:10.1021/ic0005644

data_4319275
_publ_contact_author
;
 Professor L H Gade
 Laboratoire de Chimie Organometallique et de Catalyse
 Institut Le Bel
 Universite Louis Pasteur
 4 rue Blaise Pascal
 67070 Strasbourg Cedex
 FRANCE
;
_publ_contact_author_email       Gade@chimie.u-strasbg.fr
_publ_section_title
;
 Group 4 Imido Complexes Stabilized by a Tridentate Diamido-Donor Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              870
_journal_page_last               877
_journal_paper_doi               10.1021/ic0005644
_journal_volume                  40
_journal_year                    2001
_chemical_compound_source
;

 Li2[MeC(2-NC5H4)(CH2NSiMe3)2] + [Zr(N-2,6-C6H3-i-Pr2)2(py)3]

 in C6H6.  Recrystallised from hexane

;
_chemical_formula_moiety         ' C32 H51 N5 Si2 Zr1'
_chemical_formula_sum            'C32 H51 N5 Si2 Zr'
_chemical_formula_weight         653.19
_chemical_name_systematic
;

 [{(2-NC5H4)CMe(CH2NSiMe3)2}Zr(N-2,6-C6H3-i-Pr2)(py)]

;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 106.248(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.6470(8)
_cell_length_b                   11.5510(3)
_cell_length_c                   19.335(1)
_cell_measurement_reflns_used    22094
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      0
_cell_volume                     3569.4(3)
_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  0.074
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            22094
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         1.10
_diffrn_standards_decay_%        0.00
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.39
_exptl_absorpt_correction_T_max  0.856
_exptl_absorpt_correction_T_min  0.746
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.75
_refine_diff_density_max         0.836
_refine_diff_density_min         -0.69
_refine_ls_abs_structure_Flack   none
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.173
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         3983
_refine_ls_number_restraints     10
_refine_ls_R_factor_obs          0.050
_refine_ls_shift/esd_max         0.018
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      'Chebychev polynomial'
_refine_ls_wR_factor_obs         0.046
_reflns_limit_h_max              19
_reflns_limit_h_min              -20
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_observed          3983
_reflns_number_total             7575
_reflns_observed_criterion       >3\s(I)
_cod_data_source_file            ic0005644_3.cif
_cod_data_source_block           COMPOUND_5
_cod_depositor_comments
;
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:

'_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        3569.4()
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        ' C32 H51 N5 Si2 Zr1'
_cod_database_code               4319275