Atom-Economical Route to Substituted Pyridines via a Scandium Imide
Wicker, Benjamin F.; Scott, Jennifer; Fout, Alison R.; Pink, Maren; Mindiola, Daniel J.; Organometallics 30 (2011) 2453–; doi:10.1021/om2001537

data_4064511
_publ_section_title
;
 Atom-Economical Route to Substituted Pyridines via a Scandium Imide
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2453
_journal_paper_doi               10.1021/om2001537
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C61 H91 N4 P2 Sc'
_chemical_formula_sum            'C61 H91 N4 P2 Sc'
_chemical_formula_weight         987.28
_chemical_name_systematic
; 
 ? 
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                74.525(2)
_cell_angle_beta                 74.729(2)
_cell_angle_gamma                68.528(2)
_cell_formula_units_Z            2
_cell_length_a                   12.5519(13)
_cell_length_b                   13.9454(14)
_cell_length_c                   18.719(2)
_cell_measurement_reflns_used    4205
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.00
_cell_measurement_theta_min      2.28
_cell_volume                     2888.0(5)
_computing_cell_refinement       'APEX II v2009.5.0 (Bruker, 2009)'
_computing_data_collection       'APEX II v2009.5.0 (Bruker, 2009)'
_computing_data_reduction        'APEX II v2009.5.0 (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2008)'
_computing_publication_material  'SHELXTL (Bruker, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-2004 (Burla et al., 2005)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 83.33
_diffrn_detector_type            'Bruker APEXII'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
'0.30 degree frames measured for 60 seconds each'
_diffrn_measurement_device       'APEX Kappa Duo'
_diffrn_measurement_device_type  Kappa
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0769
_diffrn_reflns_av_sigmaI/netI    0.0838
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            37526
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    0.223
_exptl_absorpt_correction_T_max  0.9716
_exptl_absorpt_correction_T_min  0.9610
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing; 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.135
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.800
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     623
_refine_ls_number_reflns         10102
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.1070
_refine_ls_R_factor_gt           0.0612
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0828P)^2^+1.3666P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1470
_refine_ls_wR_factor_ref         0.1696
_reflns_number_gt                6552
_reflns_number_total             10102
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om2001537_si_003.cif
_cod_data_source_block           3a
_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_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'multi-scans' was replaced
with the value 'multi-scan' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_cell_volume        2888.1(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4064511