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_7116559
_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         'C27 H21 Fe1 N9 Ni1 O2'
_chemical_formula_sum            'C27 H21 Fe N9 Ni O2'
_chemical_formula_weight         618.08
_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   difmap
_atom_sites_solution_primary     direct
_audit_update_record
;
2014-11-27 deposited with the CCDC.
2015-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.117(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.3572(6)
_cell_length_b                   15.1852(4)
_cell_length_c                   10.1318(2)
_cell_measurement_reflns_used    5003
_cell_measurement_temperature    100
_cell_measurement_theta_max      70
_cell_measurement_theta_min      5
_cell_volume                     2669.96(13)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'Gemini, (Oxford Diffraction, 2006)'
_computing_data_reduction        'XRED (Stoe & Cie 1996)'
_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    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction Gemini'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.038
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            13075
_diffrn_reflns_theta_full        69.285
_diffrn_reflns_theta_max         70.699
_diffrn_reflns_theta_min         3.868
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.598
_exptl_absorpt_correction_T_max  0.85
_exptl_absorpt_correction_T_min  0.54
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       planar
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.42
_refine_diff_density_min         -0.60
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1310
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         2203
_refine_ls_number_restraints     28
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0634
_refine_ls_shift/su_max          0.0092193
_refine_ls_shift/su_mean         0.0005256
_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: 
 17.3 2.15 11.9 5.15 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0648
_refine_ls_wR_factor_gt          0.0624
_refine_ls_wR_factor_ref         0.0618
_reflns_limit_h_max              21
_reflns_limit_h_min              -21
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              12
_reflns_limit_l_min              0
_reflns_number_gt                2320
_reflns_number_total             2550
_reflns_threshold_expression     I>2.0\s(I)
_oxford_refine_ls_r_factor_ref   0.0604
_oxford_reflns_number_all        2540
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            c4cc10182k2.cif
_cod_data_source_block           cpd3
_cod_original_sg_symbol_H-M      'C 2/c '
_cod_original_formula_sum        'C27 H21 Fe1 N9 Ni1 O2'
_cod_database_code               7116559
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE C(9,U'S) C(90,U'S) 
RIDE C(10,U'S) C(100,U'S) 
RIDE C(11,U'S) C(110,U'S) 
RIDE C(12,U'S) C(120,U'S) 
RIDE C(13,U'S) C(130,U'S) 
RIDE C(14,U'S) C(140,U'S) 
RIDE C(9,X'S) C(90,X'S) 
RIDE C(10,X'S) C(100,X'S) 
RIDE C(11,X'S) C(110,X'S) 
RIDE C(12,X'S) C(120,X'S) 
RIDE C(13,X'S) C(130,X'S) 
RIDE C(14,X'S) C(140,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   (  71,X'S) H   (  73,X'S) H   (  72,X'S) 
RIDE N   (   5,X'S) H   (  51,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
SAME C(9) C(10) C(11) C(12) C(13) C(14) 
CONT AND  C(90) C(100) C(110) C(120) C(130) C(140) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;