A tricky water molecule coordinated to a verdazyl radical-iron(ii) complex: a multitechnique approach.
Kamebuchi, Hajime; Okubo, Masashi; Okazawa, Atsushi; Enomoto, Masaya; Harada, Jun; Ogawa, Keiichiro; Maruta, Goro; Takeda, Sadamu; Kojima, Norimichi; Train, Cyrille; Verdaguer, Michel; Physical chemistry chemical physics : PCCP 16 (2014) 9086–9095; doi:10.1039/c4cp00310a

data_7214451
_publ_section_title
;
 A tricky water molecule coordinated to a verdazyl radical-iron(ii)
 complex: a multitechnique approach.
;
_journal_issue                   19
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              9086
_journal_page_last               9095
_journal_paper_doi               10.1039/c4cp00310a
_journal_volume                  16
_journal_year                    2014
_chemical_formula_sum            'C10 H20 Fe N8 O10'
_chemical_formula_weight         468.19
_chemical_name_systematic
; 
 ? 
;
_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     direct
_audit_creation_method           SHELXL-97
_cell_angle_alpha                84.837(2)
_cell_angle_beta                 83.709(2)
_cell_angle_gamma                80.095(2)
_cell_formula_units_Z            2
_cell_length_a                   9.1722(7)
_cell_length_b                   9.5972(7)
_cell_length_c                   10.5527(8)
_cell_measurement_reflns_used    5464
_cell_measurement_temperature    300
_cell_measurement_theta_max      29.9
_cell_measurement_theta_min      2.2
_cell_volume                     907.17(12)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      300
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD diffractometer'
_diffrn_measurement_method       \w_scan
_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  0.0367
_diffrn_reflns_av_sigmaI/netI    0.0315
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            26015
_diffrn_reflns_theta_full        30.04
_diffrn_reflns_theta_max         30.04
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    0.904
_exptl_absorpt_correction_T_max  0.9151
_exptl_absorpt_correction_T_min  0.7990
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'twinabs 2008/4'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.714
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             484
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         5285
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0408
_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^)+(0.0718P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1089
_refine_ls_wR_factor_ref         0.1206
_reflns_number_gt                3588
_reflns_number_total             5285
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cp00310a3.cif
_cod_data_source_block           fed2ort
_cod_database_code               7214451