Mechanistic aspects of the chemistry of mononuclear CrIII complexes with pendant-arm macrocyclic ligands and formation of discrete CrIII/FeII and CrIII/FeII/CoIII cyano-bridged mixed valence compounds
Basallote, Manuel G.; Bernhardt, Paul V.; Calvet, Teresa; Castillo, Carmen E.; Font-Bardia, Mercè; Martínez, Manuel; Rodríguez, Carlos; Dalton Transactions  (2009) 9567–9577; doi:10.1039/b909151c

data_7002740
_publ_section_title
;
 Mechanistic aspects of the chemistry of mononuclear CrIII complexes
 with pendant-arm macrocyclic ligands and formation of discrete
 CrIII/FeII and CrIII/FeII/CoIII cyano-bridged mixed valence compounds
;
_journal_issue                   43
_journal_name_full               'Dalton Transactions'
_journal_page_first              9567
_journal_page_last               9577
_journal_paper_doi               10.1039/b909151c
_journal_year                    2009
_chemical_formula_moiety         'C12 H29 Cl Cr N5, 2(Cl O4)'
_chemical_formula_sum            'C12 H29 Cl3 Cr N5 O8'
_chemical_formula_weight         529.75
_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                   13.225(5)
_cell_length_b                   13.727(3)
_cell_length_c                   23.329(7)
_cell_measurement_reflns_used    313
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31
_cell_measurement_theta_min      3
_cell_volume                     4235(2)
_computing_cell_refinement       AUTOMAR
_computing_data_collection       MARXDS
_computing_data_reduction        MARSCALE
_computing_molecular_graphics    'ORTEP (Brueggermann and Smith, 1990)'
_computing_publication_material  'PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.863
_diffrn_measurement_device_type  'MAR345 with image plate detector'
_diffrn_measurement_method       'phi scan'
_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  0.0535
_diffrn_reflns_av_sigmaI/netI    0.0298
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            41669
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         32.41
_diffrn_reflns_theta_min         2.76
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.969
_exptl_absorpt_correction_T_max  0.91
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2200
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.552
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.100
_refine_ls_extinction_coef       0.0043(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.187
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         6564
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.268
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0589
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1044P)^2^+2.4045P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2052
_refine_ls_wR_factor_ref         0.2138
_reflns_number_gt                5157
_reflns_number_total             6564
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b909151c.txt
_cod_data_source_block           mmmm95b
_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_original_sg_symbol_H-M      Pbca
_cod_database_code               7002740