Reversible Single Crystal to Single Crystal Transformation through Fe-O(H)Me/Fe-OH2 Bond Formation/Bond Breaking in a Gas-Solid Reaction at an Ambient Condition
Sabbani Supriya; Samar K. Das; Journal of the American Chemical Society 129 (2007) 3464–3465; doi:10.1021/ja067572p

data_4109210
_publ_section_title
;
 Reversible Single Crystal to Single Crystal Transformation through
 Fe-O(H)Me/Fe-OH2 Bond Formation/Bond Breaking in a Gas-Solid Reaction at
 an Ambient Condition
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3464
_journal_page_last               3465
_journal_paper_doi               10.1021/ja067572p
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         'C22 H30 Fe3 N2 O16, Cl O4, H6 O3'
_chemical_formula_sum            'C22 H36 Cl Fe3 N2 O23'
_chemical_formula_weight         899.53
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.6883(9)
_cell_length_b                   17.6585(9)
_cell_length_c                   24.2830(13)
_cell_measurement_reflns_used    8641
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      26.76
_cell_measurement_theta_min      2.37
_cell_volume                     7156.0(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Diamond 2.1'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0646
_diffrn_reflns_av_sigmaI/netI    0.0395
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            79173
_diffrn_reflns_theta_full        28.68
_diffrn_reflns_theta_max         28.68
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    1.365
_exptl_absorpt_correction_T_max  0.7912
_exptl_absorpt_correction_T_min  0.6112
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.670
_exptl_crystal_description       block
_exptl_crystal_F_000             3688
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.940
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         8856
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0443
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0810P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1181
_refine_ls_wR_factor_ref         0.1253
_reflns_number_gt                6435
_reflns_number_total             8856
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja067572psi20061023_021758.cif
_cod_data_source_block           compound1
_cod_database_code               4109210