Structure and Magnetism of Heptanuclear Complexes Formed on Encapsulation of Hexacyanoferrate(II) with the Mn(II) and Ni(II) Complexes of 1,4-Bis(2-pyridylmethyl)-1,4,7-triazacyclononane
Richard J. Parker; Leone Spiccia; Boujemaa Moubaraki; Keith S. Murray; David C. R. Hockless; A. David Rae; Anthony C. Willis; Inorganic Chemistry 41 (2002) 2489–2495; doi:10.1021/ic010711d

data_4317904
_publ_contact_author_address
;
Research School of Chemistry,
Australian National University,
Canberra, A. C. T. 0200, Australia
;
_publ_contact_author_email       ' willis@rsc.anu.edu.au '
_publ_contact_author_fax         ' 61 2 6125 0750 '
_publ_contact_author_name        ' Anthony C. Willis '
_publ_contact_author_phone       ' 61 2 6125 4109 '
_publ_section_title
;
 Structure and Magnetism of Heptanuclear Complexes Formed on Encapsulation
 of Hexacyanoferrate(II) with the Mn(II) and Ni(II) Complexes of
 1,4-Bis(2-pyridylmethyl)-1,4,7-triazacyclononane
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2489
_journal_page_last               2495
_journal_paper_doi               10.1021/ic010711d
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety
' C114 H150 Fe Mn6 N36 8+, 8(Cl O4 -), 5(H2 O)'
_chemical_formula_sum            'C114 H160 Cl8 Fe Mn6 N36 O37'
_chemical_formula_weight         3295.84
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      148
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_audit_creation_date             2001-03-07
_audit_creation_method           'by teXsan v1.8'
_audit_update_record
;
2001-03-08 - Report on C114 H160 Cl8 Fe Mn6 N36 O37
            by A. David Rae, David C. R. Hockless  and  Anthony C. Willis
            for Richard Parker and Leone Spiccia
2001-03-09 - third version arrives
2001-03-13 - passes checkcif tests with minor warnings
            *  note use of spherically averaged perchlorate ion called Cl7A
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   30.073(3)
_cell_length_b                   30.073
_cell_length_c                   13.303(4)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    183.2
_cell_measurement_theta_max      31.3
_cell_measurement_theta_min      27.6
_cell_volume                     10419(3)
_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      183.2
_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      -0.03785
_diffrn_orient_matrix_UB_12      -0.01487
_diffrn_orient_matrix_UB_13      -0.00865
_diffrn_orient_matrix_UB_21      -0.00555
_diffrn_orient_matrix_UB_22      -0.03489
_diffrn_orient_matrix_UB_23      0.01620
_diffrn_orient_matrix_UB_31      -0.00326
_diffrn_orient_matrix_UB_32      0.00599
_diffrn_orient_matrix_UB_33      0.07289
_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  0.02577
_diffrn_reflns_av_sigmaI/netI    0.070
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3724
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         60.08
_diffrn_reflns_theta_min         2.94
_diffrn_standards_decay_%        -5.12
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.302
_exptl_absorpt_correction_T_max  0.645
_exptl_absorpt_correction_T_min  0.565
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
\y scans (North,Phillips & Matthews, 1968)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.576
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             5112.00
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.435
_refine_diff_density_min         -0.515
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.5719
_refine_ls_goodness_of_fit_ref   1.8992
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         1926
_refine_ls_R_factor_all          0.1314
_refine_ls_R_factor_gt           0.0655
_refine_ls_shift/su_max          0.2
_refine_ls_shift/su_mean         0.1
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.0016|Fo|^2^]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.1070
_refine_ls_wR_factor_ref         0.0975
_reflns_number_gt                1923
_reflns_number_total             3436
_reflns_threshold_expression     I>3.00\s(I)
_cod_data_source_file            ic010711d_1.cif
_cod_data_source_block           PAR3b
_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      'R -3 '
_cod_original_formula_sum        'C114 H160 Cl8 Fe Mn6 N36 O37 '
_cod_database_code               4317904