Structural and Magnetic Diversity in Cyano-Bridged Bi- and Trimetallic Complexes Assembled from Cyanometalates and [M(rac-CTH)]n+Building Blocks (CTH =d,l-5,5,7,12,12,14-Hexamethyl-1,4,8,11-tetraazacyclotetradecane)
Rodríguez-Diéguez, Antonio; Kivekäs, Raikko; Sillanpää, Reijo; Cano, Joan; Lloret, Francesc; McKee, Vickie; Stoeckli-Evans, Helen; Colacio, Enrique; Inorganic Chemistry 45 (2006) 10537–10551; doi:10.1021/ic061187j

data_4332986
_publ_section_title
;
 Structural and Magnetic Diversity in Cyano-Bridged Bi- and Trimetallic
 Complexes Assembled from Cyanometalates and [M(rac-CTH)]n+Building Blocks
 (CTH =d,l-5,5,7,12,12,14-Hexamethyl-1,4,8,11-tetraazacyclotetradecane)
;
_journal_issue                   26
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10537
_journal_page_last               10551
_journal_paper_doi               10.1021/ic061187j
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C42 H72 Cu3 Fe2 N24, 5(H2 O)'
_chemical_formula_sum            'C42 H82 Cu3 Fe2 N24 O5'
_chemical_formula_weight         1305.64
_chemical_name_systematic
; 
 ? 
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.357(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.7784(8)
_cell_length_b                   33.112(3)
_cell_length_c                   9.7326(9)
_cell_measurement_reflns_used    5091
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.99
_cell_measurement_theta_min      2.41
_cell_volume                     2811.6(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.919
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_device_type  'Bruker Smart Apex CCD'
_diffrn_measurement_method       \w--\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_sigmaI/netI    0.0450
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            17862
_diffrn_reflns_theta_full        28.34
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         2.19
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    1.684
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.788056
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (G.M. Sheldrick, 2003)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1362.0
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.385
_refine_diff_density_min         -0.703
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         6443
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0461
_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^)+(0.0544P)^2^+5.3866P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1136
_refine_ls_wR_factor_ref         0.1187
_reflns_number_gt                5465
_reflns_number_total             6443
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061187jsup1.cif
_cod_data_source_block           compound_9
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        2811.6(5)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4332986