An iron(ii) complex salt that crystallises in three crystal forms, one of which undergoes a sterically controlled incomplete spin-state transition on cooling
Jérôme Elhaïk; Colin A. Kilner; Malcolm A. Halcrow; CrystEngComm 7 (2005) 151–; doi:10.1039/b417718e

data_7203716
_publ_section_title
;
 An iron(ii) complex salt that crystallises in three crystal forms, one
 of which undergoes a sterically controlled incomplete spin-state
 transition on cooling
;
_journal_issue                   23
_journal_name_full               CrystEngComm
_journal_page_first              151
_journal_paper_doi               10.1039/b417718e
_journal_volume                  7
_journal_year                    2005
_chemical_formula_moiety         'C26 H26 Fe N10 O4, 2[Cl O4]'
_chemical_formula_sum            'C26 H26 Cl2 Fe N10 O12'
_chemical_formula_weight         797.32
_chemical_name_common
;
Bis(2,6-bis(3-(hydroxymethyl)pyrazol-1-yl)pyridine)iron(ii)
diperchlorate, beta polymorph
;
_chemical_name_systematic
;
Bis[2,6-bis{3-(hydroxymethyl)pyrazol-1-yl}pyridine]iron(II)
diperchlorate, beta polymorph
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 108.3160(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.1578(2)
_cell_length_b                   10.0249(1)
_cell_length_c                   16.2228(1)
_cell_measurement_reflns_used    55093
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.47
_cell_volume                     3112.22(5)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEX (McArdle, 1995)'
_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 9.091
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
'Nonius KappaCCD area detector diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_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  0.0806
_diffrn_reflns_av_sigmaI/netI    0.0344
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            55081
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.52
_exptl_absorpt_coefficient_mu    0.739
_exptl_absorpt_correction_T_max  0.866
_exptl_absorpt_correction_T_min  0.742
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Using multiple and symmetry-related data measurements via the program SORTAV
See R.H. Blessing, Acta Cryst (1995), A51, 33-38
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.702
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Rectangular prism'
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.989
_refine_diff_density_min         -0.891
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       0.0033(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     486
_refine_ls_number_reflns         7089
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.180
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0388
_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^)+(0.0586P)^2^+2.1228P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1051
_refine_ls_wR_factor_ref         0.1110
_reflns_number_gt                6254
_reflns_number_total             7089
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b417718e.txt
_cod_data_source_block           c:\datasets\leeds\je41b\je41b
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7203716