The 6-amino-6-methyl-1,4-diazepine group as ancillary ligand framework for neutral and cationic scandium and yttrium alkyls
Bart Hessen; Sergio Bambirra; Shaozhong Ge; Auke Meetsma; Chemical Communications  (2006) –; doi:10.1039/b606384e

data_7101328
_publ_section_title
;
The 6-amino-6-methyl-1,4-diazepine group as ancillary
ligand framework for neutral and cationic scandium and yttrium alkyls
;
_journal_issue                   31
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/b606384e
_journal_year                    2006
_chemical_compound_source        'see text'
_chemical_formula_moiety         '2(C31 H64 N3 O Si3 Y), 0.5(C7 H8)'
_chemical_formula_sum            'C131 H264 N12 O4 Si12 Y4'
_chemical_formula_weight         1382.13
_chemical_name_systematic        ?
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   direct
_audit_creation_date             '2006-04-11 10:53:50'
_audit_creation_method
;
PLATON <TABLE ACC> option (version :: 280206)
SHELXL97-2 & Manual Editing
;
_audit_update_record
;
?
;
_cell_angle_alpha                80.864(2)
_cell_angle_beta                 87.771(2)
_cell_angle_gamma                85.449(2)
_cell_formula_units_Z            2
_cell_length_a                   10.653(1)
_cell_length_b                   17.454(2)
_cell_length_c                   21.730(2)
_cell_measurement_reflns_used    8235
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      2.37
_cell_volume                     3975.2(7)
_computing_cell_refinement       'SAINTPLUS, Version 6.02A, (Bruker, 2000)'
_computing_data_collection       'SMART, Version 5.624, (Bruker, 2001)'
_computing_data_reduction        'XPREP, Version 5.1/NT, (Bruker, 2000)'
_computing_molecular_graphics
;
PLUTO (Meetsma, 2006)
PLATON (Spek, 2003)
;
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
DIRDIF-99 (Beurskens et al., 1999)
;
_diffrn_ambient_temperature      100(1)
_diffrn_detector_area_resol_mean '4096x4096 / 62x62 (binned 512)'
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type
;
Bruker Smart Apex; CCD area detector
;
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_detector
;
CCD area-detector
;
_diffrn_radiation_monochromator  'parallel mounted graphite'
_diffrn_radiation_source         'fine focus sealed Siemens Mo tube '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0622
_diffrn_reflns_av_sigmaI/netI    0.1077
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            30900
_diffrn_reflns_reduction_process
;
Intensity data were corrected for Lorentz and polarization
effects, decay and absorption and reduced to F~o~^2^
using SAINT (Bruker, 2000) and SADABS (Sheldrick, 2001)
;
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         2.39
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.584
_exptl_absorpt_correction_T_max  0.8451
_exptl_absorpt_correction_T_min  0.6121
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Sheldrick, Bruker, 2001))'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1490
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.800
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     729
_refine_ls_number_reflns         15266
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0956
_refine_ls_R_factor_gt           0.0534
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0423P)^2^+0.0P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1013
_refine_ls_wR_factor_ref         0.1154
_reflns_number_gt                10248
_reflns_number_total             15266
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b606384e.txt
_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.

'_exptl_absorpt_correction_type' value 'Multi-Scan' changed
to 'multi-scan' 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_database_code               7101328