Aryl-Containing Chelates and Amine Debenzylation to Afford 1,3-Di-2-pyridyl-2-azaallyl (smif): Structures of {κ-C,N,Npy2-(2-pyridylmethyl)2N(CH2(4-tBu-phenyl-2-yl))}FeBr and (smif)CrN(TMS)2
Brenda A. Frazier; Peter T. Wolczanski; Emil B. Lobkovsky; Inorganic Chemistry 48 (2009) 11576–11585; doi:10.1021/ic901329z

data_4303826
_publ_section_title
;
Aryl-Containing Chelates and Amine Debenzylation to Afford
1,3-Di-2-pyridyl-2-azaallyl (smif): Structures of
{\k-C,N,Npy2-(2-pyridylmethyl)2N(CH2(4-tBu-phenyl-2-yl))}FeBr and
(smif)CrN(TMS)2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11576
_journal_page_last               11585
_journal_paper_doi               10.1021/ic901329z
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C23 H26 Br Fe N3'
_chemical_formula_sum            'C23 H26 Br Fe N3'
_chemical_formula_weight         480.23
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.0576(12)
_cell_length_b                   16.9655(11)
_cell_length_c                   20.0495(18)
_cell_measurement_reflns_used    965
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      18.57
_cell_measurement_theta_min      2.56
_cell_volume                     4441.5(6)
_computing_cell_refinement       'Bruker SAINT+'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT+'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker X8 APEX II diffractometer'
_diffrn_measurement_method       'phi and omega 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  0.1178
_diffrn_reflns_av_sigmaI/netI    0.1046
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            15951
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    2.491
_exptl_absorpt_correction_T_max  0.9403
_exptl_absorpt_correction_T_min  0.6357
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.528
_refine_diff_density_min         -0.481
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         3192
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1101
_refine_ls_R_factor_gt           0.0501
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0426P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0906
_refine_ls_wR_factor_ref         0.1100
_reflns_number_gt                1896
_reflns_number_total             3192
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901329z_si_001_1.cif
_cod_data_source_block           bf7
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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               4303826