Scandium and yttrium complexes of the diamide–diamine donor ligand (2-C5H4N)CH2N(CH2CH2NSiMe3)2: chloride, primary and secondary amide, benzamidinate and alkyl functionalised derivatives
Skinner, Michael E. G.; Mountford, Philip; Journal of the Chemical Society, Dalton Transactions  (2002) 1694–; doi:10.1039/b111469g

data_7702779
_publ_section_title
;
 Scandium and yttrium complexes of the diamide--diamine donor ligand
 (2-C5H4N)CH2N(CH2CH2NSiMe3)2: chloride, primary and secondary amide,
 benzamidinate and alkyl functionalised derivatives
;
_journal_issue                   8
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1694
_journal_paper_doi               10.1039/b111469g
_journal_year                    2002
_chemical_compound_source
;
[Sc(N2NN')Cl] + LiCH2SiMe3
;
_chemical_formula_moiety         ' C20 H43 Sc1 N4 Si3 '
_chemical_formula_sum            'C20 H43 N4 Sc Si3'
_chemical_formula_weight         468.81
_chemical_name_systematic
;
[Sc(CH2SiMe3)(N2NN')]
;
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   'diff maps and geometric'
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.131(1)
_cell_length_b                   13.069(1)
_cell_length_c                   17.548(1)
_cell_measurement_reflns_used    15716
_cell_measurement_temperature    175
_cell_measurement_theta_max      27
_cell_measurement_theta_min      0
_cell_volume                     2782.1(4)
_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      175
_diffrn_measurement_device_type  'Enraf-nonius DIP2000'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.02
_diffrn_reflns_av_sigmaI/netI    0.0495
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15718
_diffrn_reflns_theta_max         26.42
_diffrn_reflns_theta_min         1.94
_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  0.887
_exptl_absorpt_correction_T_min  0.835
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.45
_refine_diff_density_min         -0.45
_refine_ls_abs_structure_Flack   '0.03 (.05)'
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.0841
_refine_ls_hydrogen_treatment    'riding model and U[iso]'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         5037
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0299
_refine_ls_shift/esd_max         0.0018
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979, 
1.65    0.716     1.20    
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0372
_reflns_limit_h_max              15
_reflns_limit_h_min              0
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_observed          5037
_reflns_number_total             5422
_reflns_observed_criterion       >3.00\s(I)
_cod_data_source_file            b111469g.txt
_cod_data_source_block           COMPOUND_7
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Orthorhombic ' was changed
to 'orthorhombic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

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

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 

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        2782.0(3)
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_original_formula_sum        ' C20 H43 Sc1 N4 Si3 '
_cod_database_code               7702779