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_4306069
_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         'C54 H73 Co1 N6 P1'
_chemical_formula_sum            'C54 H73 Co N6 P'
_chemical_formula_weight         896.12
_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             06-11-22
_audit_creation_method           CRYSTALS_ver_12.82
_cell_angle_alpha                90
_cell_angle_beta                 92.7610(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9676(2)
_cell_length_b                   30.2749(4)
_cell_length_c                   15.4792(3)
_cell_measurement_reflns_used    30960
_cell_measurement_temperature    180
_cell_measurement_theta_max      25
_cell_measurement_theta_min      3
_cell_volume                     5133.79(15)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT. Nonius (1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_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
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.140
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            34727
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.030
_diffrn_reflns_theta_min         2.959
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.405
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.159
_exptl_crystal_description       plate
_exptl_crystal_F_000             1924
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.38
_refine_diff_density_min         -0.20
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1287
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         3729
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1096
_refine_ls_R_factor_gt           0.0340
_refine_ls_shift/su_max          0.003869
_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: 
 0.415 0.232 0.264 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0785
_refine_ls_wR_factor_gt          0.0383
_refine_ls_wR_factor_ref         0.0383
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              36
_reflns_limit_k_min              0
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                3729
_reflns_number_total             9043
_reflns_threshold_expression     I>3.00u(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_scale          0.11681(17)
_oxford_structure_analysis_title '11221440 Compound X'
_cod_data_source_file            ic800992f_si_002_2.cif
_cod_data_source_block           compound_3a.L_js0510
_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_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C54 H73 Co1 N6 P1'
_cod_database_code               4306069