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_4317905
_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         'C37 H50 N11 Mn2 3+, 3(Cl O4 -) '
_chemical_formula_sum            'C37 H50 Cl3 Mn2 N11 O12'
_chemical_formula_weight         1057.10
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      60
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_audit_creation_date             2001-03-21
_audit_creation_method           'by teXsan v1.8'
_audit_update_record
;

2001-03-21 - Report on C37 H50 Cl3 N11 Mn2 O12

             by  David C. R. Hockless  and  Anthony C. Willis

             for Richard Parker and Leone Spiccia

2001-03-21 - passes checkcif tests with minor warnings

             *  note N1/C1 common site

;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.225(3)
_cell_length_b                   16.320(2)
_cell_length_c                   18.052(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      13.4
_cell_measurement_theta_min      6.0
_cell_volume                     4780.0(13)
_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  xtal_CRYLSQ
_computing_structure_solution
;

SIR92 (Altomare, et. al. 1994)

;
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device_type  'Rigaku AFC6S'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.03943
_diffrn_orient_matrix_UB_12      -0.02864
_diffrn_orient_matrix_UB_13      -0.03377
_diffrn_orient_matrix_UB_21      0.00021
_diffrn_orient_matrix_UB_22      -0.04852
_diffrn_orient_matrix_UB_23      0.03384
_diffrn_orient_matrix_UB_31      -0.04737
_diffrn_orient_matrix_UB_32      -0.02408
_diffrn_orient_matrix_UB_33      -0.02799
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.00000
_diffrn_reflns_av_sigmaI/netI    0.043
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            3546
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         22.5
_diffrn_reflns_theta_min         2.10
_diffrn_standards_decay_%        0.09
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.764
_exptl_absorpt_correction_T_max  0.795
_exptl_absorpt_correction_T_min  0.739
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;

\y scans (North,Phillips & Matthews, 1968)

;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2184.00
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.551
_refine_diff_density_min         -0.225
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.415
_refine_ls_goodness_of_fit_ref   1.61
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         1951
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.096
_refine_ls_R_factor_gt           0.046
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00040|Fo|^2^]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.075
_refine_ls_wR_factor_ref         0.065
_reflns_number_gt                1951
_reflns_number_total             3142
_reflns_threshold_expression     I>2.00\s(I)
_cod_data_source_file            ic010711d_2.cif
_cod_data_source_block           RXP4
_cod_depositor_comments
;
 Changing the _atom_site_occupancy data item value from '.' to '1'
 for all fully occupied atom sites.

 Antanas Vaitkus,
 2017-02-19

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        4780(1)
_cod_original_sg_symbol_H-M      'P b c n '
_cod_original_formula_sum        'C37 H50 Cl3 Mn2 N11 O12 '
_cod_database_code               4317905