Remarkable Scan Rate Dependence for a Highly Constrained Dinuclear Iron(II) Spin Crossover Complex with a Wide Thermal Hysteresis Loop.
Kulmaczewski, Rafal; Olguín, Juan; Kitchen, Jonathan A.; Feltham, Humphrey L. C.; Jameson, Guy N. L.; Tallon, Jeffery L.; Brooker, Sally; Journal of the American Chemical Society 136 (2014) 878–881; doi:10.1021/ja411563x

data_4120527
_publ_section_title
;
 Remarkable Scan Rate Dependence for a Highly Constrained Dinuclear
 Iron(II) Spin Crossover Complex with a Wide Thermal Hysteresis Loop.
;
_journal_issue                   3
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              878
_journal_page_last               881
_journal_paper_doi               10.1021/ja411563x
_journal_volume                  136
_journal_year                    2014
_chemical_formula_sum            'C59.5 H74.5 B4 F16 Fe2 N17 O0.5'
_chemical_formula_weight         1494.80
_chemical_name_systematic
; 
 ? 
;
_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                 93.898(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.422(2)
_cell_length_b                   12.2868(16)
_cell_length_c                   35.081(5)
_cell_measurement_reflns_used    2202
_cell_measurement_temperature    91(2)
_cell_measurement_theta_max      16.247
_cell_measurement_theta_min      2.328
_cell_volume                     7062.1(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      91(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Kappa Apex II area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1334
_diffrn_reflns_av_sigmaI/netI    0.1146
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            37783
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    0.505
_exptl_absorpt_correction_T_max  0.9801
_exptl_absorpt_correction_T_min  0.5153
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALE (Bruker AXS Inc)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3082
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.767
_refine_diff_density_min         -0.669
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     512
_refine_ls_number_reflns         5991
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.1724
_refine_ls_R_factor_gt           0.1128
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1043P)^2^+121.9254P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2793
_refine_ls_wR_factor_ref         0.3093
_reflns_number_gt                3619
_reflns_number_total             5991
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja411563x_si_001.cif
_cod_data_source_block           jak550
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C59.50 H74.50 B4 F16 Fe2 N17 O0.50'
_cod_database_code               4120527