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_7002739
_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_compound_source        'synthesis as described'
_chemical_formula_moiety         'C11 H30 Cl Cr N5 O,3(Cl O4),2(H2 O)'
_chemical_formula_sum            'C11 H34 Cl4 Cr N5 O15'
_chemical_formula_weight         670.23
_chemical_name_systematic
;
?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      62
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2009-06-25T16:37:39-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.920(10)
_cell_length_b                   13.841(2)
_cell_length_c                   11.964(2)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.58
_cell_measurement_theta_min      11.21
_cell_measurement_wavelength     0.71073
_cell_volume                     2636.3(18)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       '\w-2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0
_diffrn_reflns_av_unetI/netI     0.0154
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            2419
_diffrn_reflns_theta_full        24.96
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         2.13
_diffrn_standards_decay_%        'less than 5%'
_diffrn_standards_interval_count 120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.914
_exptl_absorpt_correction_T_max  0.9966
_exptl_absorpt_correction_T_min  0.747
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
A.C.T. North, D.C. Phillips, F.S. Mathews, Acta. Cryst. Sect A, 1968, 24, 351
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.689
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1388
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.921
_refine_diff_density_min         -0.788
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         2419
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0636
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1243P)^2^+4.3240P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1798
_refine_ls_wR_factor_ref         0.1944
_reflns_number_gt                1930
_reflns_number_total             2419
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b909151c.txt
_cod_data_source_block           1334pb31
_cod_database_code               7002739