Reversible solid to solid transformation in a crystalline state gas‒solid reaction under ambient conditions: Fe‒N(pyridine) bond formation at the expense of Fe‒OH2bond breaking and vice versa
Sabbani, Supriya; Das, Samar K.; CrystEngComm 17 (2015) 8850–; doi:10.1039/C5CE00488H

data_7220431
_publ_section_title
;
 Reversible solid to solid transformation in a crystalline state
 gas--solid reaction under ambient conditions: Fe--N(pyridine) bond
 formation at the expense of Fe--OH2bond breaking and vice versa
;
_journal_issue                   46
_journal_name_full               CrystEngComm
_journal_page_first              8850
_journal_paper_doi               10.1039/C5CE00488H
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'C27 H33 Cl Fe3 N3 O17'
_chemical_formula_sum            'C27 H33 Cl Fe3 N3 O17'
_chemical_formula_weight         874.56
_chemical_name_common            'compound 4 in the relevant manuscript'
_chemical_name_systematic        'skd175 '
_chemical_properties_physical
'if the relevant crystals are kept in the atomosphere for long time, the coordinated pyridine may be replacd by atmospheric water vapour.'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-03-09 deposited with the CCDC.
2015-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.23(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.9670(16)
_cell_length_b                   27.574(6)
_cell_length_c                   19.131(4)
_cell_measurement_temperature    298(2)
_cell_volume                     4202.7(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_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  0.1751
_diffrn_reflns_av_sigmaI/netI    0.1538
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            41094
_diffrn_reflns_theta_full        26.36
_diffrn_reflns_theta_max         26.36
_diffrn_reflns_theta_min         1.30
_exptl_absorpt_coefficient_mu    1.151
_exptl_absorpt_correction_T_max  0.9554
_exptl_absorpt_correction_T_min  0.8196
_exptl_crystal_colour            'pale green'
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1788
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Mixture of dichloromethane, ethanol and then layering with  pyridine'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_platon_squeeze_details
;
;
_refine_diff_density_max         3.113
_refine_diff_density_min         -1.668
_refine_diff_density_rms         0.296
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.722
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         8362
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.721
_refine_ls_R_factor_all          0.2802
_refine_ls_R_factor_gt           0.2369
_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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.5238
_refine_ls_wR_factor_ref         0.5415
_reflns_number_gt                5157
_reflns_number_total             8362
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce00488h2.cif
_cod_data_source_block           skd175
_cod_depositor_comments          'Adding full bibliography for 7220431.cif.'
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7220431