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_4332980
_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         'C44 H72 Fe2 N20 Ni2, C16 H38 N4, 5(H2 O)'
_chemical_formula_sum            'C60 H120 Fe2 N24 Ni2 O5'
_chemical_formula_weight         1486.92
_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                 115.530(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.5680(9)
_cell_length_b                   16.6502(12)
_cell_length_c                   16.9719(9)
_cell_measurement_reflns_used    7442
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      0.407
_cell_volume                     3969.7(4)
_computing_cell_refinement       'HKL Scalepack (Otwinowsky & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
;
HKL Denzo and Scalepack (Otwinowsky & Minor, 1997)
;
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           Mok\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1038
_diffrn_reflns_av_sigmaI/netI    0.1009
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24933
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.35
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    0.883
_exptl_absorpt_correction_T_max  0.9490
_exptl_absorpt_correction_T_min  0.8864
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
Sheldrick, G.M. (anon) SHELX97 Release 97-2 (1998)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.955
_refine_diff_density_min         -0.574
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         7749
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.1777
_refine_ls_R_factor_gt           0.0858
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[\s^2^(Fo^2^)+(0.1150P)^2^+1.3712P] where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2090
_refine_ls_wR_factor_ref         0.2423
_reflns_number_gt                3911
_reflns_number_total             7749
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061187jsup1.cif
_cod_data_source_block           compound_2
_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_sg_symbol_H-M      'P 21/n'
_cod_database_code               4332980