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_4306071
_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         'C38 H50 Co1 N4 O1'
_chemical_formula_sum            'C38 H50 Co N4 O'
_chemical_formula_weight         637.77
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             07-11-04
_audit_creation_method           CRYSTALS_ver_12.80
_cell_angle_alpha                90
_cell_angle_beta                 93.3850(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6637(11)
_cell_length_b                   21.386(2)
_cell_length_c                   14.1464(13)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    150
_cell_measurement_theta_max      30
_cell_measurement_theta_min      0
_cell_volume                     3522.5(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_device_type  'Bruker SMART APEX2 CCD'
_diffrn_measurement_method       'fine-slice \w scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6709
_diffrn_reflns_av_R_equivalents  0.028
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            42070
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         32.148
_diffrn_reflns_theta_min         1.728
_diffrn_standards_decay_%        5
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.521
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_description       block
_exptl_crystal_F_000             1364
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.38
_refine_diff_density_min         -0.37
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0392
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         5189
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0952
_refine_ls_R_factor_gt           0.0411
_refine_ls_shift/su_max          0.001481
_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: 
 0.487 0.440 0.301 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0784
_refine_ls_wR_factor_gt          0.0441
_refine_ls_wR_factor_ref         0.0441
_reflns_limit_h_max              17
_reflns_limit_h_min              -16
_reflns_limit_k_max              31
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                5189
_reflns_number_total             11528
_reflns_threshold_expression     I>3.00u(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_scale          0.1515(2)
_oxford_structure_analysis_title 'compound_4a_ox088 in P2(1)/n'
_cod_data_source_file            ic800992f_si_002_4.cif
_cod_data_source_block           compound_4a_CRYSTALS_cif
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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        3522.6(6)
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C38 H50 Co1 N4 O1'
_cod_database_code               4306071