data_Fe-MIL-88B
_audit_creation_date              2018-07-08
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_shelxl_version_number            2013-2
_publ_contact_author_address      ?
_publ_contact_author_email        ?
_publ_contact_author_id_orcid     ?
_publ_contact_author_name         ''
_publ_contact_author_phone        ?
_publ_section_references
;
Burla, M.C., Caliandro, R., Camalli, M., Carrozzini, B., Cascarano, G.L.,
 De Caro, L., Giacovazzo, C., Polidori, G., Siliqi, D., Spagna, R.
 (2007). J. Appl. Cryst. 40, 609-613.

Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common             ?
_chemical_name_systematic
;
 ?
;
_chemical_formula_moiety          '0.5(C48 H24 Fe6 N6 O32)'
_chemical_formula_sum             'C24 H12 Fe3 N3 O16'
_chemical_formula_weight          765.92
_chemical_melting_point           ?
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system       'hexagonal'
_space_group_IT_number            194
_space_group_name_H-M_alt         'P 63/m m c'
_space_group_name_Hall            '-P 6c 2c'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-y, x-y, z'
 '-x+y, -x, z'
 '-x, -y, z+1/2'
 'y, -x+y, z+1/2'
 'x-y, x, z+1/2'
 'y, x, -z'
 'x-y, -y, -z'
 '-x, -x+y, -z'
 '-y, -x, -z+1/2'
 '-x+y, y, -z+1/2'
 'x, x-y, -z+1/2'
 '-x, -y, -z'
 'y, -x+y, -z'
 'x-y, x, -z'
 'x, y, -z-1/2'
 '-y, x-y, -z-1/2'
 '-x+y, -x, -z-1/2'
 '-y, -x, z'
 '-x+y, y, z'
 'x, x-y, z'
 'y, x, z-1/2'
 'x-y, -y, z-1/2'
 '-x, -x+y, z-1/2'

_cell_length_a                    12.9009(10)
_cell_length_b                    12.9009(10)
_cell_length_c                    18.2641(10)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 120
_cell_volume                      2632.5(4)
_cell_formula_units_Z             2
_cell_measurement_reflns_used     2931
_cell_measurement_temperature     150(2)
_cell_measurement_theta_max       27.7830
_cell_measurement_theta_min       2.8280
_shelx_estimated_absorpt_T_max    ?
_shelx_estimated_absorpt_T_min    ?
_exptl_absorpt_coefficient_mu     0.861
_exptl_absorpt_correction_T_max   1.00000
_exptl_absorpt_correction_T_min   0.15098
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.39.43c (Rigaku Oxford Diffraction, 2018)'
_exptl_crystal_colour             'clear red'
_exptl_crystal_colour_lustre      clear
_exptl_crystal_colour_primary     red
_exptl_crystal_density_diffrn     0.966
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_description        prism
_exptl_crystal_F_000              766
_exptl_crystal_size_max           0.1
_exptl_crystal_size_mid           0.03
_exptl_crystal_size_min           0.01
_exptl_special_details
;
 ?
;
_exptl_transmission_factor_max    ?
_exptl_transmission_factor_min    ?
_diffrn_reflns_av_R_equivalents   0.0494
_diffrn_reflns_av_unetI/netI      0.0256
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max        13
_diffrn_reflns_limit_h_min        -14
_diffrn_reflns_limit_k_max        11
_diffrn_reflns_limit_k_min        -15
_diffrn_reflns_limit_l_max        16
_diffrn_reflns_limit_l_min        -22
_diffrn_reflns_number             12908
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full         26.000
_diffrn_reflns_theta_max          25.958
_diffrn_reflns_theta_min          2.137
_diffrn_ambient_temperature       150.15
_diffrn_detector_area_resol_mean  ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type   'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method        ?
_diffrn_radiation_type            MoK\a
_diffrn_radiation_wavelength      0.71073
_diffrn_source                    ?
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_full     .
_reflns_Friedel_fraction_max      .
_reflns_number_gt                 735
_reflns_number_total              1020
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression      'I > 2σ(I)'
_computing_cell_refinement        ?
_computing_data_collection        ?
_computing_data_reduction         ?
_computing_molecular_graphics     'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material   'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement   'ShelXL (Sheldrick, 2015)'
_computing_structure_solution     'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max          0.502
_refine_diff_density_min          -0.585
_refine_diff_density_rms          0.097
_refine_ls_extinction_coef        .
_refine_ls_extinction_method      none
_refine_ls_goodness_of_fit_ref    1.159
_refine_ls_hydrogen_treatment     constr
_refine_ls_matrix_type            full
_refine_ls_number_parameters      51
_refine_ls_number_reflns          1020
_refine_ls_number_restraints      6
_refine_ls_R_factor_all           0.0833
_refine_ls_R_factor_gt            0.0626
_refine_ls_restrained_S_all       1.164
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_weighting_details
;
 w=1/[σ²(Fo²)+(0.1397P)²+0.6348P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme       calc
_refine_ls_wR_factor_gt           0.2096
_refine_ls_wR_factor_ref          0.2274
_refine_special_details
;
 ?
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
N1: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
3. Others
 Fixed Sof: H3A(0.25) H3B(0.25) N1(0.25) H1A(0.25) H1B(0.25)
4.a Riding coordinates:
 O3(H3A,H3B)
4.b Rotating group:
 N1(H1A,H1B)
;
_atom_sites_solution_hydrogens    difmap
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    ?
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_site_symmetry_order
  _atom_site_calc_flag
  _atom_site_refinement_flags_posn
  _atom_site_refinement_flags_adp
  _atom_site_refinement_flags_occupancy
  _atom_site_disorder_assembly
  _atom_site_disorder_group
 Fe1 Fe 0.75218(5) 0.50436(11) 0.2500 0.0623(6) Uani 1 4 d S T P . .
 O1 O 0.6667 0.3333 0.2500 0.059(2) Uani 1 12 d S T P . .
 O2 O 0.6531(3) 0.5185(3) 0.32922(15) 0.0784(10) Uani 1 1 d . . . . .
 O3 O 0.8409(2) 0.6818(5) 0.2500 0.0798(18) Uani 1 4 d S T P . .
 H3A H 0.8629 0.7257 0.2880 0.120 Uiso 0.5 2 d RS T P . .
 H3B H 0.8629 0.7257 0.2120 0.120 Uiso 0.5 2 d RS T P . .
 N1 N 0.3321(16) 0.2838(16) 0.4419(8) 0.095(5) Uani 0.25 1 d . U . . .
 H1A H 0.3100 0.2173 0.4732 0.114 Uiso 0.25 1 d GR . . . .
 H1B H 0.2567 0.2767 0.4340 0.114 Uiso 0.25 1 d GR . . . .
 C1 C 0.5559(3) 0.4441(3) 0.3579(3) 0.0751(17) Uani 1 2 d S T P . .
 C2 C 0.5260(3) 0.4740(3) 0.4317(3) 0.0710(17) Uani 1 2 d S T P . .
 C3 C 0.4211(5) 0.3941(5) 0.4658(2) 0.0834(14) Uani 1 1 d . . . . .


_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
  _geom_bond_atom_site_label_1
  _geom_bond_atom_site_label_2
  _geom_bond_distance
  _geom_bond_site_symmetry_2
  _geom_bond_publ_flag
 Fe1 O1 1.9108(12) . ?
 Fe1 O2 1.999(3) 20_655 ?
 Fe1 O2 1.999(3) 11_655 ?
 Fe1 O2 1.999(3) . ?
 Fe1 O2 1.999(3) 16_556 ?
 Fe1 O3 1.983(6) . ?
 O1 Fe1 1.9108(12) 2_655 ?
 O1 Fe1 1.9108(12) 3_665 ?
 O2 C1 1.250(4) . ?
 O3 H3A 0.8499 . ?
 O3 H3B 0.8499 . ?
 N1 H1A 0.9491 . ?
 N1 H1B 0.9408 . ?
 N1 C3 1.378(17) . ?
 C1 O2 1.250(4) 19_665 ?
 C1 C2 1.505(7) . ?
 C2 C3 1.373(6) . ?
 C2 C3 1.373(6) 19_665 ?
 C3 C3 1.388(8) 7_556 ?

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
  _geom_angle_publ_flag
 O1 Fe1 O2 94.54(9) . . ?
 O1 Fe1 O2 94.54(9) . 11_655 ?
 O1 Fe1 O2 94.54(9) . 20_655 ?
 O1 Fe1 O2 94.54(9) . 16_556 ?
 O1 Fe1 O3 180.00(8) . . ?
 O2 Fe1 O2 170.92(18) 20_655 16_556 ?
 O2 Fe1 O2 86.53(19) 16_556 11_655 ?
 O2 Fe1 O2 92.75(19) 20_655 11_655 ?
 O2 Fe1 O2 86.53(19) . 20_655 ?
 O2 Fe1 O2 170.92(18) . 11_655 ?
 O2 Fe1 O2 92.75(19) . 16_556 ?
 O3 Fe1 O2 85.46(9) . 11_655 ?
 O3 Fe1 O2 85.46(9) . . ?
 O3 Fe1 O2 85.46(9) . 16_556 ?
 O3 Fe1 O2 85.46(9) . 20_655 ?
 Fe1 O1 Fe1 120.0 3_665 . ?
 Fe1 O1 Fe1 120.0 . 2_655 ?
 Fe1 O1 Fe1 120.0 3_665 2_655 ?
 C1 O2 Fe1 132.4(3) . . ?
 Fe1 O3 H3A 125.2 . . ?
 Fe1 O3 H3B 125.2 . . ?
 H3A O3 H3B 109.5 . . ?
 H1A N1 H1B 100.1 . . ?
 C3 N1 H1A 117.5 . . ?
 C3 N1 H1B 115.9 . . ?
 O2 C1 O2 124.6(5) 19_665 . ?
 O2 C1 C2 117.7(3) 19_665 . ?
 O2 C1 C2 117.7(3) . . ?
 C3 C2 C1 119.8(3) . . ?
 C3 C2 C1 119.8(3) 19_665 . ?
 C3 C2 C3 120.4(5) 19_665 . ?
 N1 C3 C3 111.1(6) . 7_556 ?
 C2 C3 N1 129.1(7) . . ?
 C2 C3 C3 119.8(3) . 7_556 ?

loop_
  _geom_torsion_atom_site_label_1
  _geom_torsion_atom_site_label_2
  _geom_torsion_atom_site_label_3
  _geom_torsion_atom_site_label_4
  _geom_torsion
  _geom_torsion_site_symmetry_1
  _geom_torsion_site_symmetry_2
  _geom_torsion_site_symmetry_3
  _geom_torsion_site_symmetry_4
  _geom_torsion_publ_flag
 Fe1 O2 C1 O2 -20.1(10) . . . 19_665 ?
 Fe1 O2 C1 C2 160.4(4) . . . . ?
 O2 C1 C2 C3 -179.0(6) . . . . ?
 O2 C1 C2 C3 -1.5(9) . . . 19_665 ?
 O2 C1 C2 C3 179.0(6) 19_665 . . 19_665 ?
 O2 C1 C2 C3 1.5(9) 19_665 . . . ?
 C1 C2 C3 N1 -0.5(15) . . . . ?
 C1 C2 C3 C3 179.4(6) . . . 7_556 ?
 C3 C2 C3 N1 -178.0(11) 19_665 . . . ?
 C3 C2 C3 C3 1.9(12) 19_665 . . 7_556 ?


# SQUEEZE RESULTS (Version = 230318)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1 -0.021 -0.015 -0.001      1329       289 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                           ?


