Synthesis of mixed-donor amido/amino/siloxo ligands from symmetrical diamidosilylether ligands via a retro-Brook rearrangement and their chromium(ii) complexes
Haftbaradaran, Farzad; Mund, Garry; Batchelor, Raymond J.; Britten, James F.; Leznoff, Daniel B.; Dalton Transactions  (2005) 2343–; doi:10.1039/b506322a

data_7008717
_publ_section_title
;
 Synthesis of mixed-donor amido/amino/siloxo ligands from symmetrical
 diamidosilylether ligands via a retro-Brook rearrangement and their
 chromium(ii) complexes
;
_journal_issue                   14
_journal_name_full               'Dalton Transactions'
_journal_page_first              2343
_journal_paper_doi               10.1039/b506322a
_journal_year                    2005
_chemical_formula_moiety         'C44 H68 Cr2 N4 O2 Si4'
_chemical_formula_sum            'C44 H68 Cr2 N4 O2 Si4'
_chemical_formula_weight         901.39
_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
_cell_angle_alpha                105.800(18)
_cell_angle_beta                 95.03(2)
_cell_angle_gamma                103.31(2)
_cell_formula_units_Z            2
_cell_length_a                   11.349(3)
_cell_length_b                   11.513(3)
_cell_length_c                   20.346(4)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293
_cell_measurement_theta_max      17
_cell_measurement_theta_min      16
_cell_volume                     2457.0(11)
_computing_cell_refinement       'Cad4 Express, (Straver, 1992)'
_computing_data_collection       'Cad4 Express, (Straver, 1992)'
_computing_data_reduction        'RC93 (Watkin, Prout & Lilley, 1994)'
_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    'USER DEFINED STRUCTURE SOLUTION'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.70930
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            6917
_diffrn_reflns_theta_full        22.997
_diffrn_reflns_theta_max         22.997
_diffrn_reflns_theta_min         2.104
_diffrn_standards_decay_%        1.10
_diffrn_standards_interval_count 35
_diffrn_standards_interval_time  200
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.577
_exptl_absorpt_correction_T_max  0.84
_exptl_absorpt_correction_T_min  0.73
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
Azimutal absorption correction (North et al, 1968)
;
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.44
_refine_diff_density_min         -0.35
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   2.3920
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         2974
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1737
_refine_ls_R_factor_gt           0.0575
_refine_ls_shift/su_max          0.000203
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
p=P(6)*max(Fo^2^,0) + (1-P(6))Fc^2^
Method = SHELXL 97 (Sheldrick, 1997)
W = 1. / [Sigma^2^(F*)+(P(1)p)^2^+P(2)p+P(4)+P(5)Sin(theta) ]
P(i) are:
0.100E-01 0.00 0.00 0.00 0.00 1.00
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0557
_refine_ls_wR_factor_gt          0.0520
_refine_ls_wR_factor_ref         0.0520
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              12
_reflns_limit_k_min              -12
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                2974
_reflns_number_total             6892
_reflns_threshold_expression     I>2.50u(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_scale          1.084(2)
_cod_data_source_file            b506322a.txt
_cod_data_source_block           Me3PhNONCr
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 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 '
_cod_database_code               7008717