Isostructural Salts of the Same Complex Showing Contrasting Thermal Spin-Crossover Mediated by Multiple Phase Changes
Thomas D. Roberts; Marc A. Little; Floriana Tuna; Colin A. Kilner; Malcolm A. Halcrow; Chem.Commun. 49 (2013) 6280–; doi:10.1039/c3cc43613f

data_7109474
_publ_section_title
;
 Isostructural Salts of the Same Complex Showing Contrasting Thermal
 Spin-Crossover Mediated by Multiple Phase Changes
;
_journal_name_full               Chem.Commun.
_journal_page_first              6280
_journal_paper_doi               10.1039/c3cc43613f
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety
'C26 H26 Fe N10, 2[ClO4], 0.83 [C H3 N O2], 0.33 [C4 H10 O]'
_chemical_formula_sum            'C28.17 H31.83 Cl2 Fe N10.83 O10'
_chemical_formula_weight         808.89
_chemical_name_systematic
; 
Bis[2,6-bis(5-methylpyrazol-3-yl)pyridine]iron(II) diperchlorate 
nitromethane (1/0.83) diethyl ether (0.33) solvate
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                86.131(2)
_cell_angle_beta                 75.642(2)
_cell_angle_gamma                81.923(2)
_cell_formula_units_Z            6
_cell_length_a                   13.1968(7)
_cell_length_b                   20.4571(12)
_cell_length_c                   20.6896(12)
_cell_measurement_reflns_used    108015
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.38
_cell_measurement_theta_min      1.02
_cell_volume                     5354.3(5)
_computing_cell_refinement       'APEX 2 software, Bruker Nonius 2004'
_computing_data_collection       'APEX 2 software, Bruker Nonius 2004'
_computing_data_reduction        'SAINT, Bruker Nonius 2004'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean '120 microns'
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker X8 Apex diffractometer'
_diffrn_measurement_method       'Rotation images'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_av_sigmaI/netI    0.0347
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            108015
_diffrn_reflns_theta_full        26.38
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         1.02
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.642
_exptl_absorpt_correction_T_max  0.884
_exptl_absorpt_correction_T_min  0.793
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Sheldrick, G. M. (2002). SADABS v. 2.03. University of 
G/ottingen, Germany.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2500
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.13
_refine_diff_density_max         2.683
_refine_diff_density_min         -1.084
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1430
_refine_ls_number_reflns         21517
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0948
_refine_ls_R_factor_gt           0.0781
_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^)+(0.1226P)^2^+17.2359P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2227
_refine_ls_wR_factor_ref         0.2363
_reflns_number_gt                17306
_reflns_number_total             21517
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc43613f_2-1.cif
_cod_data_source_block           tr11b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'triclinic ' changed to 'triclinic'
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 1891 2012-01-12 08:04:46Z andrius 
;
_cod_database_code               7109474