Single-ion magnet behaviour of heptacoordinated Fe(II) complexes: on the importance of supramolecular organization
Arun Kumar Bar; Celine Pichon; Nayanmoni Gogoi; Carine Duhayon; S. Ramasesha; Jean-Pascal Sutter; Chem.Commun. 51 (2015) 3616–; doi:10.1039/C4cc10182K

data_7116558
_publ_section_title
;
 Single-ion magnet behaviour of heptacoordinated Fe(II) complexes: on the
 importance of supramolecular organization
;
_journal_name_full               Chem.Commun.
_journal_page_first              3616
_journal_paper_doi               10.1039/C4cc10182K
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C24 H27 Fe N5 O4, 2(B F4), 2(C H4 O)'
_chemical_formula_sum            'C26 H35 B2 F8 Fe N5 O6'
_chemical_formula_weight         743.05
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_update_record
;
2014-11-27 deposited with the CCDC.
2015-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                82.716(2)
_cell_angle_beta                 85.057(2)
_cell_angle_gamma                84.926(2)
_cell_formula_units_Z            2
_cell_length_a                   7.7688(4)
_cell_length_b                   8.5125(4)
_cell_length_c                   24.4247(11)
_cell_measurement_reflns_used    9658
_cell_measurement_temperature    100
_cell_measurement_theta_max      35
_cell_measurement_theta_min      2
_cell_volume                     1591.34(13)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.577
_diffrn_measured_fraction_theta_max 0.527
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.022
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            78089
_diffrn_reflns_theta_full        25.283
_diffrn_reflns_theta_max         34.634
_diffrn_reflns_theta_min         0.843
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.569
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            grey
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             764
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_refine_diff_density_max         1.75
_refine_diff_density_min         -1.47
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0875
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         6777
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0657
_refine_ls_shift/su_max          0.0013553
_refine_ls_shift/su_mean         0.0000322
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.256 0.210 0.619E-01 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0749
_refine_ls_wR_factor_gt          0.0708
_refine_ls_wR_factor_ref         0.0700
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              13
_reflns_limit_k_min              -13
_reflns_limit_l_max              14
_reflns_limit_l_min              0
_reflns_number_gt                6940
_reflns_number_total             7192
_reflns_threshold_expression     I>2.0\s(I)
_oxford_refine_ls_r_factor_ref   0.0646
_oxford_reflns_number_all        7165
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            c4cc10182k2.cif
_cod_data_source_block           cpd1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 2827 2014-09-09 07:05:25Z andrius 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C26 H35 B2 F8 Fe1 N5 O6'
_cod_database_code               7116558
_iucr_refine_instructions_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE C   (   2,X'S) H   (  21,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   7,X'S) H   (  73,X'S) H   (  71,X'S) H   (  72,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) H   ( 113,X'S) H   ( 112,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) H   ( 243,X'S) H   ( 242,X'S) 
RIDE C   (  25,X'S) H   ( 252,X'S) H   ( 251,X'S) H   ( 253,X'S) 
RIDE C   (  26,X'S) H   ( 263,X'S) H   ( 261,X'S) H   ( 262,X'S) 
RIDE N   (  32,X'S) H   ( 321,X'S) 
RIDE N   (  42,X'S) H   ( 421,X'S) 
RIDE O   (   5,X'S) H   (  51,X'S) 
RIDE O   (   6,X'S) H   (  61,X'S) 
RIDE O   (  30,X'S) H   ( 301,X'S) 
RIDE O   (  40,X'S) H   ( 402,X'S) H   ( 401,X'S) 
RIDE N(2,U'S) N(32,U'S) C(8,U'S) N(5,U'S) N(42,U'S) C(9,U'S) 
CONT O(1,U'S) O(2,U'S) C(1,U'S) C(5,U'S) C(6,U'S) C(10,U'S) 
RIDE F(1,U'S) F(10,U'S) 
RIDE F(2,U'S) F(20,U'S) 
RIDE F(3,U'S) F(30,U'S) 
RIDE F(7,U'S) F(8,U'S) 
RIDE F(1,X'S) F(10,X'S) F(2,X'S) F(20,X'S) F(3,X'S) F(30,X'S) 
END                                                                             
;
_iucr_refine_instructions_details_restraints
;
SAME F(1) F(2) F(3) AND F(10) F(20) F(30) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;