1,2-Bis(pyridine-2-carboxamido)benzenate(2-), (bpb)2-: A Noninnocent Ligand. Syntheses, Structures, and Mechanisms of Formation of [(n-Bu)4N][FeIV2(μ-N)(bpb)2(X)2] (X = CN-, N3-) and the Electronic Structures of [MIII(bpbox1)(CN)2] (M = Co, Fe)
Sujit K. Dutta; Udo Beckmann; Eckhard Bill; Thomas Weyhermüller; Karl Wieghardt; Inorganic Chemistry 39 (2000) 3355–3364; doi:10.1021/ic0001107

data_4321139
_publ_section_title
;
 1,2-Bis(pyridine-2-carboxamido)benzenate(2-), (bpb)2-: A Noninnocent
 Ligand. Syntheses, Structures, and Mechanisms of Formation of
 [(n-Bu)4N][FeIV2(\m-N)(bpb)2(X)2] (X = CN-, N3-) and the Electronic
 Structures of [MIII(bpbox1)(CN)2] (M = Co, Fe)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3355
_journal_page_last               3364
_journal_paper_doi               10.1021/ic0001107
_journal_volume                  39
_journal_year                    2000
_chemical_formula_structural     '[C16 H36 N]+,[C18 H12 Fe N10 O2]-,0.5(C7 H8)'
_chemical_formula_sum            'C37.5 H52 Fe N11 O2'
_chemical_formula_weight         744.75
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.946(3)
_cell_length_b                   15.685(3)
_cell_length_c                   30.523(5)
_cell_measurement_reflns_used    15977
_cell_measurement_temperature    100(2)
_cell_volume                     7634(2)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measurement_device       'Nonius Kappa CCD'
_diffrn_measurement_method       '549 frames a 1 deg.(\w)/60 sec.'
_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  0.1269
_diffrn_reflns_av_sigmaI/netI    0.0785
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            59702
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.39
_exptl_absorpt_coefficient_mu    0.444
_exptl_absorpt_correction_type   'not measured'
_exptl_crystal_colour            'dark red almost black'
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_description       prism
_exptl_crystal_F_000             3168
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.28(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.012
_refine_ls_goodness_of_fit_obs   1.057
_refine_ls_matrix_type           full
_refine_ls_number_parameters     923
_refine_ls_number_reflns         9883
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.019
_refine_ls_restrained_S_obs      1.056
_refine_ls_R_factor_all          0.0801
_refine_ls_R_factor_obs          0.0526
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0737P)^2^+0.6219P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1295
_refine_ls_wR_factor_obs         0.1161
_reflns_number_observed          7613
_reflns_number_total             9912
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0001107_1.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0737P)^2^+0.6219P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0737P)^2^+0.6219P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        7634.2(24)
_cod_original_formula_sum        'C37.50 H52 Fe N11 O2'
_cod_database_code               4321139