Synthesis, crystal structures and magnetic properties of linear and bent trinuclear complexes formed by hexacyanometallates and copper(ii) complexes
Parker, Richard J.; Lu, Kevin D.; Batten, Stuart R.; Moubaraki, Boujemaa; Murray, Keith S.; Spiccia, Leone; Cashion, John D.; Rae, A. David; Willis, Anthony C.; Journal of the Chemical Society, Dalton Transactions  (2002) 3723–; doi:10.1039/b205749m

data_7011913
_publ_section_title
;
 Synthesis, crystal structures and magnetic properties of linear and
 bent trinuclear complexes formed by hexacyanometallates and copper(ii)
 complexes
;
_journal_issue                   19
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3723
_journal_paper_doi               10.1039/b205749m
_journal_year                    2002
_chemical_formula_moiety         'C42 H36 Cu2 Fe N14 +, Cl O4 -, 8(H2 O) '
_chemical_formula_sum            'C42 H52 Cl Cu2 Fe N14 O12'
_chemical_formula_weight         1163.35
_space_group_IT_number           145
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      145
_symmetry_space_group_name_Hall  'P 32'
_symmetry_space_group_name_H-M   'P 32'
_audit_creation_date             2001-08-13
_audit_creation_method           'by teXsan v1.8'
_audit_update_record
;
1997-02-04 - Report on C42 H52 Cl Cu2 Fe  N14 O12
by  David C. R. Hockless
for Richard Parker and Leone Spiccia
2001-08-10 - A. David Rae fixes problems
2001-08-13 - Anthony C. Willis makes up cif
2001-03-13 - passes checkcif tests with minor warnings
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   12.665(2)
_cell_length_b                   12.665
_cell_length_c                   27.860(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      49.7
_cell_measurement_theta_min      45.5
_cell_volume                     3870.1(7)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan (MSC, 1992-1997)'
_computing_publication_material  'teXsan (MSC, 1992-1997)'
_computing_structure_refinement  RAELS00
_computing_structure_solution
;
SIR92 (Altomare, et. al. 1994)
;
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device_details
;
Rigaku AFC6R diffractometer with extended arm and
evacuated collimator and beam tunnel.
Data cannot be collected beyond \y 60 deg in this configuration.
;
_diffrn_measurement_device_type  'Rigaku AFC6R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      -0.04105
_diffrn_orient_matrix_UB_12      -0.04223
_diffrn_orient_matrix_UB_13      -0.03049
_diffrn_orient_matrix_UB_21      0.07519
_diffrn_orient_matrix_UB_22      -0.00130
_diffrn_orient_matrix_UB_23      -0.00997
_diffrn_orient_matrix_UB_31      -0.03120
_diffrn_orient_matrix_UB_32      -0.08079
_diffrn_orient_matrix_UB_33      0.01610
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.04747
_diffrn_reflns_av_sigmaI/netI    0.060
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6212
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         60.05
_diffrn_reflns_theta_min         0.00
_diffrn_standards_decay_%        -0.94
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.269
_exptl_absorpt_correction_T_max  .426
_exptl_absorpt_correction_T_min  .309
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
\y scans (North,Phillips & Matthews, 1968)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1797.00
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.56
_refine_diff_density_min         -0.54
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.35
_refine_ls_goodness_of_fit_ref   1.41
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     260
_refine_ls_number_reflns         3290
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.057
_refine_ls_R_factor_gt           0.044
_refine_ls_shift/su_max          0.2
_refine_ls_shift/su_mean         0.03
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.0009|Fo|^2^]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.063
_refine_ls_wR_factor_ref         0.061
_reflns_number_gt                3183
_reflns_number_total             3845
_reflns_threshold_expression     I>3.00\s(I)
_cod_data_source_file            b205749m.txt
_cod_data_source_block           PAR2
_cod_original_cell_volume        3870(1)
_cod_original_sg_symbol_H-M      'P 32       '
_cod_original_formula_sum        'C42 H52 Cl Cu2 Fe N14 O12 '
_cod_database_code               7011913