Synthesis, Structure and Magnetic Behavior of Five-Coordinate Bis(iminopyrrolyl) Complexes of Cobalt(II) containing PMe3 and THF Ligands
Sónia A. Carabineiro; Ronan M. Bellabarba; Pedro T. Gomes; Sofia I. Pascu; Luís F. Veiros; Cristina Freire; Laura C. J. Pereira; Rui T. Henriques; M. Conceição Oliveira; John E. Warren; Inorganic Chemistry 47 (2008) 8896–8911; doi:10.1021/ic800992f

data_4306073
_publ_section_title
;
Synthesis, Structure and Magnetic Behavior of Five-Coordinate
Bis(iminopyrrolyl) Complexes of Cobalt(II) containing PMe3 and THF Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8896
_journal_page_last               8911
_journal_paper_doi               10.1021/ic800992f
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C76 H100 Co N8 O'
_chemical_formula_sum            'C76 H100 Co N8 O'
_chemical_formula_weight         1200.57
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             06-11-24
_audit_creation_method           CRYSTALS_ver_12.80
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.208(2)
_cell_length_b                   18.208(2)
_cell_length_c                   21.189(3)
_cell_measurement_reflns_used    30447
_cell_measurement_temperature    150
_cell_measurement_theta_max      25.5
_cell_measurement_theta_min      1
_cell_volume                     7024.8(15)
_computing_cell_refinement       'SAINT (Siemens ,1995)'
_computing_data_collection       'SMART (Siemens, 1993)'
_computing_data_reduction        'SAINT (Siemens ,1995)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.69040
_diffrn_reflns_av_R_equivalents  0.119
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            30447
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.476
_diffrn_reflns_theta_min         1.432
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.292
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.99
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.135
_exptl_crystal_description       shard
_exptl_crystal_F_000             2588
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.67
_refine_diff_density_min         -0.39
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1394
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         1204
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          0.1303
_refine_ls_R_factor_gt           0.0573
_refine_ls_shift/su_max          0.014048
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.608 0.540 0.360 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1005
_refine_ls_wR_factor_gt          0.0659
_refine_ls_wR_factor_ref         0.0659
_reflns_limit_h_max              16
_reflns_limit_h_min              -15
_reflns_limit_k_max              22
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                1204
_reflns_number_total             3564
_reflns_threshold_expression     I>2.00u(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_scale          0.0751(3)
_cod_data_source_file            ic800992f_si_002_6.cif
_cod_data_source_block           polymorph_4b_II_cam220
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
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_original_cell_volume        7024.6(17)
_cod_original_sg_symbol_H-M      'I 41/a '
_cod_database_code               4306073