A Distinctive PdCl2-Mediated Transformation of Fe-Based Metallogels into Metal‒Organic Frameworks
Aiyappa, Harshitha Barike; Saha, Subhadeep; Garai, Bikash; Thote, Jayshri; Kurungot, Sreekumar; Banerjee, Rahul; Crystal Growth & Design 14 (2014) 3434–; doi:10.1021/cg500368q

data_4511261
_publ_contact_author
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Dr. Rahul Banerjee

Scientist
Physical/Materials Chemistry Division  
National Chemical Laboratory
Dr. Homi Bhaba Road
Pune 411008, India

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_publ_section_title
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 A Distinctive PdCl2-Mediated Transformation of Fe-Based Metallogels into
 Metal--Organic Frameworks
;
_journal_issue                   7
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              3434
_journal_paper_doi               10.1021/cg500368q
_journal_volume                  14
_journal_year                    2014
_chemical_formula_moiety         'C6 H7 Fe N O5'
_chemical_formula_sum            'C6 H7 Fe N O5'
_chemical_formula_weight         228.98
_chemical_name_common            Fe-BTC-NMF
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-07-21
_audit_creation_method
;
  Olex2 1.2
  (compiled May  9 2012 12:37:22, GUI svn.r4230)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            18
_cell_length_a                   14.0339(6)
_cell_length_b                   14.0339(6)
_cell_length_c                   21.2738(10)
_cell_measurement_reflns_used    1408
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.8570
_cell_measurement_theta_min      3.8550
_cell_volume                     3628.5(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
olex2.refine (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.1640
_diffrn_measured_fraction_theta_full 0.9976
_diffrn_measured_fraction_theta_max 0.8349
_diffrn_measurement_details
;
  1 omega   25.00   52.00   1.0000    4.3700
omega____ theta____ kappa____ phi______ frames
    -      -18.5831   77.0000   90.0000 27

  2 omega  -48.00   49.00   1.0000    4.3700
omega____ theta____ kappa____ phi______ frames
    -       18.5831  -77.0000   90.0000 97
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0396017000
_diffrn_orient_matrix_UB_12      -0.0231127000
_diffrn_orient_matrix_UB_13      0.0244298000
_diffrn_orient_matrix_UB_21      0.0358178000
_diffrn_orient_matrix_UB_22      -0.0122961000
_diffrn_orient_matrix_UB_23      0.0171839000
_diffrn_orient_matrix_UB_31      0.0235883000
_diffrn_orient_matrix_UB_32      0.0521526000
_diffrn_orient_matrix_UB_33      0.0148363000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_av_unetI/netI     0.0448
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3022
_diffrn_reflns_theta_full        29.27
_diffrn_reflns_theta_max         29.27
_diffrn_reflns_theta_min         2.90
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.858
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98483
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour
;
;
_exptl_crystal_density_diffrn    1.886
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description
;
;
_exptl_crystal_F_000             1788
_refine_diff_density_max         0.535
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.930
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         1841
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.930
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0349
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1150
_refine_ls_wR_factor_ref         0.1363
_reflns_number_gt                1501
_reflns_number_total             2205
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg500368q_si_002.cif
_cod_data_source_block           fe-btc-nmf
_cod_depositor_comments
'Adding full bibliography for 4511261--4511262.cif.'
_cod_database_code               4511261
_chemical_oxdiff_formula         'C20 H20 N6 O8 Cu2'
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32