Influence of Sample Preparation, Temperature, Light, and Pressure on the Two-Step Spin Crossover Mononuclear Compound [Fe(bapbpy)(NCS)2]
Bonnet, Sylvestre; Molnár, Gábor; Sanchez Costa, José; Siegler, Maxime A.; Spek, Anthony L.; Bousseksou, Azedine; Fu, Wen-Tian; Gamez, Patrick; Reedijk, Jan; Chemistry of Materials 21 (2009) 1123–; doi:10.1021/cm803414q

data_4001006
_publ_section_title
;
 Influence of Sample Preparation, Temperature, Light, and Pressure on the
 Two-Step Spin Crossover Mononuclear Compound [Fe(bapbpy)(NCS)2]
;
_journal_issue                   6
_journal_name_full               'Chemistry of Materials'
_journal_page_first              1123
_journal_paper_doi               10.1021/cm803414q
_journal_volume                  21
_journal_year                    2009
_chemical_formula_moiety         'C22 H16 Fe N8 S2, 2(C3 H7 N O)'
_chemical_formula_sum            'C28 H30 Fe N10 O2 S2'
_chemical_formula_weight         658.59
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                91.086(2)
_cell_angle_beta                 103.967(2)
_cell_angle_gamma                95.266(2)
_cell_formula_units_Z            2
_cell_length_a                   8.8298(8)
_cell_length_b                   12.2817(4)
_cell_length_c                   14.3159(5)
_cell_measurement_reflns_used    13639
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.67
_cell_volume                     1498.87(15)
_computing_cell_refinement       'PEAKREF (Schreurs, 2005)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'EVALCCD (Duisenberg et al., 2003)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF08 (Beurskens et al., 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0469
_diffrn_reflns_av_sigmaI/netI    0.0510
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            32805
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    0.688
_exptl_absorpt_correction_T_max  0.954
_exptl_absorpt_correction_T_min  0.834
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2002)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'thick plate'
_exptl_crystal_F_000             684
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.457
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.191
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         6883
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.191
_refine_ls_R_factor_all          0.0785
_refine_ls_R_factor_gt           0.0464
_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^)+(0.0029P)^2^+2.2671P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0860
_refine_ls_wR_factor_ref         0.0930
_reflns_number_gt                5064
_reflns_number_total             6883
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cm803414q_si_001.cif
_cod_data_source_block           2
_cod_database_code               4001006