Synthesis and characterization of homo- and heterodinuclear M(II)-M'(III) (M(II) = Mn or Fe, M'(III) = Fe or Co) mixed-valence supramolecular pseudo-dimers. The effect of hydrogen bonding on spin state selection of M(II).
Brewer, Cynthia T.; Brewer, Greg; Butcher, Ray J.; Carpenter, Everett E.; Schmiedekamp, Ann M.; Schmiedekamp, Carl; Straka, Alison; Viragh, Carol; Yuzefpolskiy, Yevgeniy; Zavalij, Peter; Dalton transactions (Cambridge, England : 2003) 40 (2011) 181–194; doi:10.1039/c0dt01098g

data_7014722
_publ_section_title
;
 Synthesis and characterization of homo- and heterodinuclear
 M(II)-M'(III) (M(II) = Mn or Fe, M'(III) = Fe or Co) mixed-valence
 supramolecular pseudo-dimers. The effect of hydrogen bonding on spin
 state selection of M(II).
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              181
_journal_page_last               194
_journal_paper_doi               10.1039/c0dt01098g
_journal_volume                  40
_journal_year                    2011
_chemical_formula_moiety         'C42 H57 Fe2 N20, 2(B F4)'
_chemical_formula_sum            'C42 H57 B2 F8 Fe2 N20'
_chemical_formula_weight         1127.40
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 93.0491(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.3419(3)
_cell_length_b                   12.5140(2)
_cell_length_c                   19.6566(3)
_cell_measurement_reflns_used    6073
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      77.3582
_cell_measurement_theta_min      4.5013
_cell_volume                     5242.31(14)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_molecular_graphics    'Shelxtl (Bruker, 1998)'
_computing_publication_material  Shelxtl
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 10.5081
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_av_sigmaI/netI    0.0275
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            12868
_diffrn_reflns_theta_full        67.50
_diffrn_reflns_theta_max         77.48
_diffrn_reflns_theta_min         4.51
_exptl_absorpt_coefficient_mu    5.138
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44340
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2332
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.821
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         5494
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0539
_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^)+(0.1164P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1536
_refine_ls_wR_factor_ref         0.1632
_reflns_number_gt                4193
_reflns_number_total             5494
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            C0DT01098G.TXT
_cod_data_source_block           ams-4a
_cod_original_cell_volume        5242.33(14)
_cod_database_code               7014722