#------------------------------------------------------------------------------
#$Date: 2016-03-24 14:18:17 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179659 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/12/4511262.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4511262
loop_
_publ_author_name
'Aiyappa, Harshitha Barike'
'Saha, Subhadeep'
'Garai, Bikash'
'Thote, Jayshri'
'Kurungot, Sreekumar'
'Banerjee, Rahul'
_publ_contact_author
;

Dr. Rahul Banerjee

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


;
_publ_section_title
;
 A Distinctive PdCl2-Mediated Transformation of Fe-Based Metallogels into
 Metal--Organic Frameworks
;
_journal_issue                   7
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              3434
_journal_paper_doi               10.1021/cg500368q
_journal_volume                  14
_journal_year                    2014
_chemical_formula_moiety         'C22 H4 Fe4 O17 Pd'
_chemical_formula_sum            'C22 H4 Fe4 O17 Pd'
_chemical_formula_weight         870.05
_chemical_name_common            Fe-Pd-BTC
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           194
_space_group_name_Hall           '-P 6c 2c'
_space_group_name_H-M_alt        'P 63/m m c'
_symmetry_space_group_name_Hall  '-P 6c 2c'
_symmetry_space_group_name_H-M   'P 63/m m c'
_atom_sites_solution_primary     iterative
_audit_creation_date             2013-07-26
_audit_creation_method
;
  Olex2 1.2
  (compiled Mar 21 2013 11:16:32, GUI svn.r4446)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   19.9724(9)
_cell_length_b                   19.9724(9)
_cell_length_c                   26.0567(9)
_cell_measurement_temperature    293(2)
_cell_volume                     9001.4(7)
_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_solution
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.9960
_diffrn_measured_fraction_theta_max 0.9150
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1661
_diffrn_reflns_av_unetI/netI     0.1514
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            19912
_diffrn_reflns_theta_full        25.0000
_diffrn_reflns_theta_max         29.11
_diffrn_reflns_theta_min         3.13
_exptl_absorpt_coefficient_mu    1.275
_exptl_crystal_density_diffrn    0.9630
_exptl_crystal_F_000             2536.0585
_refine_diff_density_max         4.2623
_refine_diff_density_min         -2.6586
_refine_diff_density_rms         0.4537
_refine_ls_d_res_high            0.7304
_refine_ls_d_res_low             6.5142
_refine_ls_goodness_of_fit_ref   1.0710
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    2
_refine_ls_number_parameters     116
_refine_ls_number_reflns         4090
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0710
_refine_ls_R_factor_all          0.1912
_refine_ls_R_factor_gt           0.1344
_refine_ls_shift/su_max          0.0007
_refine_ls_shift/su_mean         0.0002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.2P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.3819
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              23
_reflns_limit_h_min              0
_reflns_limit_k_max              13
_reflns_limit_k_min              0
_reflns_limit_l_max              35
_reflns_limit_l_min              0
_reflns_number_gt                1934
_reflns_number_total             4090
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            cg500368q_si_002.cif
_cod_data_source_block           fe-pd-btc
_cod_depositor_comments
'Adding full bibliography for 4511261--4511262.cif.'
_cod_database_code               4511262
#BEGIN Tags that were not found in dictionaries:
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4)
;
#END Tags that were not found in dictionaries
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 x-y,x,z+1/2
3 y,-x+y,z+1/2
4 -y,x-y,z
5 -x+y,-x,z
6 x-y,-y,-z
7 -x,-x+y,-z
8 -x,-y,z+1/2
9 y,x,-z
10 -y,-x,-z+1/2
11 -x+y,y,-z+1/2
12 x,x-y,-z+1/2
13 -x,-y,-z
14 -x+y,-x,-z-1/2
15 -y,x-y,-z-1/2
16 y,-x+y,-z
17 x-y,x,-z
18 -x+y,y,z
19 x,x-y,z
20 x,y,-z-1/2
21 -y,-x,z
22 y,x,z-1/2
23 x-y,-y,z-1/2
24 -x,-x+y,z-1/2
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
C6 C 0.8217(4) 0.6435(8) 0.6708(4) 0.049(3) Uani 1.000000 S T
C5 C 0.8054(5) 0.6108(9) 0.6180(5) 0.062(4) Uani 1.000000 S T
C4 C 0.8546(5) 0.5901(5) 0.5937(3) 0.051(2) Uani 1.000000 . .
H4 H 0.8987(5) 0.5981(5) 0.6109(3) 0.061(3) Uiso 1.000000 R .
C2 C 0.8409(5) 0.5586(5) 0.5457(3) 0.0455(19) Uani 1.000000 . .
C1 C 0.8983(5) 0.5396(5) 0.5217(3) 0.0454(19) Uani 1.000000 . .
C7 C 0.5781(7) 0.6120(8) 0.750000 0.051(3) Uani 1.000000 S T
C8 C 0.4751(4) 0.5249(4) 0.6757(5) 0.047(3) Uani 1.000000 S T
Fe2 Fe 1.03962(8) 0.51981(4) 0.55057(5) 0.0308(5) Uani 1.000000 S T
Fe1 Fe 0.76585(10) 0.71473(11) 0.750000 0.0492(6) Uani 1.000000 S T
O5 O 0.6424(8) 0.6608(7) 0.750000 0.088(3) Uani 1.000000 S T
O6 O 0.4741(3) 0.5259(3) 0.6287(4) 0.065(3) Uani 1.000000 S T
O1 O 0.9524(4) 0.5495(4) 0.5502(3) 0.0614(17) Uani 1.000000 . .
O2 O 0.8849(4) 0.5135(4) 0.4781(3) 0.0616(17) Uani 1.000000 . .
Pd1 Pd 0.47600(4) 0.52400(4) 0.750000 0.0477(5) Uani 1.000000 S T
O3 O 0.7740(4) 0.6560(5) 0.6894(3) 0.076(2) Uani 1.000000 . .
O4 O 0.8945(4) 0.7890(7) 0.750000 0.065(3) Uani 1.000000 S T
C3 C 0.7727(3) 0.5454(7) 0.5195(4) 0.049(3) Uani 1.000000 S T
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
_atom_type_scat_dispersion_source
O 0.01158 0.00611 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
H 0.00000 0.00000 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
C 0.00347 0.00161 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Fe 0.35822 0.84933 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Pd -0.98845 1.01473 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O3 C6 C5 116.1(6) . .
O3 C6 C5 116.1(6) 18_655 .
O3 C6 O3 127.7(12) 18_655 .
C4 C5 C6 121.2(6) 18_655 .
C4 C5 C6 121.2(6) . .
C4 C5 C4 117.0(12) . 18_655
H4 C4 C5 118.5(6) . 18_655
C2 C4 C5 123.1(9) . 18_655
C2 C4 H4 118.5(5) . .
C1 C2 C4 119.5(7) . .
C3 C2 C4 118.5(8) 18_655 .
C3 C2 C1 122.0(8) 18_655 .
O1 C1 C2 114.9(7) . .
O2 C1 C2 117.3(8) . .
O2 C1 O1 127.6(8) . .
Pd1 C7 O5 174.0(13) . .
Pd1 C8 O6 179.3(10) . .
O1 Fe2 O6 94.5(3) . 5_665
O1 Fe2 O6 94.5(3) 19 5_665
O1 Fe2 O1 88.3(4) . 19
O2 Fe2 O6 107.1(3) 7_766 5_665
O2 Fe2 O6 107.1(3) 13_766 5_665
O2 Fe2 O1 158.3(3) 7_766 19
O2 Fe2 O1 88.5(3) 7_766 .
O2 Fe2 O1 88.5(3) 13_766 19
O2 Fe2 O1 158.3(3) 13_766 .
O2 Fe2 O2 86.7(4) 7_766 13_766
O3 Fe1 O5 96.6(3) 20_557 .
O3 Fe1 O5 96.6(3) . .
O3 Fe1 O3 102.8(5) 20_557 .
O4 Fe1 O5 170.7(4) 11_656 .
O4 Fe1 O3 89.2(3) 11_656 20_557
O4 Fe1 O3 89.2(3) 11_656 .
Fe1 O5 C7 159.2(12) . .
Fe2 O6 C8 172.5(9) 4_655 .
Fe2 O1 C1 137.4(6) 19 .
Fe2 O2 C1 115.6(6) 13_766 .
C7 Pd1 C7 165.3(8) 10_666 .
C8 Pd1 C7 90.12(5) 10_666 10_666
C8 Pd1 C7 90.12(5) 10_666 .
C8 Pd1 C7 90.12(5) . 10_666
C8 Pd1 C7 90.12(5) . .
C8 Pd1 C8 178.2(7) 10_666 .
Fe1 O3 C6 137.5(7) . .
Fe1 O4 Fe1 109.8(5) . 11_656
C2 C3 C2 119.2(10) . 18_655
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C6 C5 1.487(17) .
C6 O3 1.202(8) .
C6 O3 1.202(8) 18_655
C5 C4 1.394(11) .
C5 C4 1.394(11) 18_655
C4 H4 0.9300 .
C4 C2 1.363(11) .
C2 C1 1.513(11) .
C2 C3 1.426(10) 18_655
C1 O1 1.241(10) .
C1 O2 1.224(10) .
C7 O5 1.161(16) .
C7 Pd1 1.914(12) .
C8 O6 1.226(18) .
C8 Pd1 1.936(14) .
Fe2 Fe2 2.971(3) 7_766
Fe2 O6 2.046(10) 5_665
Fe2 O1 2.102(6) .
Fe2 O1 2.102(6) 19
Fe2 O2 2.068(6) 13_766
Fe2 O2 2.068(6) 7_766
Fe1 O5 2.141(13) .
Fe1 O3 2.021(6) 20_557
Fe1 O3 2.021(6) .
Fe1 O4 2.234(7) 11_656
