Gas confinement in compartmentalized coordination polymers for highly selective sorption
Giménez-Marqués, Mónica; Calvo Galve, Néstor; Palomino, Miguel; Valencia, Susana; Rey, Fernando; Sastre, Germán; Vitórica-Yrezábal, Iñigo J.; Jiménez-Ruiz, Mónica; Rodríguez-Velamazán, J. Alberto; González, Miguel A.; Jordá, José L.; Coronado, Eugenio; Espallargas, Guillermo Mínguez; Chem. Sci. 8 (2017) 3109–; doi:10.1039/C6SC05122G

data_1545255
_publ_section_title
;
 Gas confinement in compartmentalized coordination polymers for highly
 selective sorption
;
_journal_issue                   4
_journal_name_full               'Chem. Sci.'
_journal_page_first              3109
_journal_paper_doi               10.1039/C6SC05122G
_journal_volume                  8
_journal_year                    2017
_chemical_formula_moiety         '0.5(C60 H60 Fe2 N48), 2(B1 F4)'
_chemical_formula_sum            'C30 H30 B2 F8 Fe N24'
_chemical_formula_weight         956.25
_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_Hall           '-P 6c'
_space_group_name_H-M_alt        'P 63/m'
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2016-05-31
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-10-13 deposited with the CCDC.
2017-02-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   10.4852(10)
_cell_length_b                   10.4852(10)
_cell_length_c                   23.308(3)
_cell_measurement_reflns_used    248
_cell_measurement_temperature    240.00(14)
_cell_measurement_theta_max      16.8120
_cell_measurement_theta_min      3.9740
_cell_volume                     2219.2(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      240.00(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.933
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     -4.00  67.00   1.00   70.00    --   15.51  38.00  30.00   71
  2  \w    -17.00  22.00   1.00   70.00    --   15.51 -77.00 -90.00   39
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0026230000
_diffrn_orient_matrix_UB_12      -0.0670594000
_diffrn_orient_matrix_UB_13      -0.0070258000
_diffrn_orient_matrix_UB_21      0.0678509000
_diffrn_orient_matrix_UB_22      0.0395742000
_diffrn_orient_matrix_UB_23      -0.0149704000
_diffrn_orient_matrix_UB_31      0.0388104000
_diffrn_orient_matrix_UB_32      0.0048019000
_diffrn_orient_matrix_UB_33      0.0255336000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.2445
_diffrn_reflns_Laue_measured_fraction_full 0.933
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            1400
_diffrn_reflns_point_group_measured_fraction_full 0.933
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.345
_diffrn_reflns_theta_min         2.844
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.428
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95839
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41q (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_description       plate
_exptl_crystal_F_000             972
_exptl_crystal_preparation       ', Magnetic properties'
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.200
_refine_diff_density_min         -1.000
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     113
_refine_ls_number_reflns         1400
_refine_ls_number_restraints     112
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.2252
_refine_ls_R_factor_gt           0.1085
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1104P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2302
_refine_ls_wR_factor_ref         0.3038
_reflns_Friedel_coverage         0.000
_reflns_number_gt                608
_reflns_number_total             1400
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc05122g3.cif
_cod_data_source_block           CCP-2_HS
_cod_depositor_comments
'Adding full bibliography for 1545255--1545262.cif.'
_cod_original_cell_volume        2219.2(5)
_cod_database_code               1545255
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C10 N3 O3 H25 cl'
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.620(8) 0.380(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Restrained distances
 F2A-F1A
 2 with sigma of 0.02
 C1-C1_$1 \\sim C4_$1-C1_$1 \\sim C4_$1-C2_$1 \\sim C2-C2_$1 \\sim C4-C2 \\sim
C4-C1
 with sigma of 0.002
 F1-B0AA \\sim F2-B0AA
 with sigma of 0.002
 F2A-B0AA \\sim F1-B0AA \\sim F1A-B0AA \\sim F2-B0AA
 with sigma of 0.002
4. Uiso/Uaniso restraints and constraints
F1 \\sim F2 \\sim F2A \\sim F1A: within 2A with sigma of 0.002 and sigma for
terminal atoms of 0.004
5. Rigid body (RIGU) restrains
 C2, C4, C1, C3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N14, C8, N3, N7, N13
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F2A, F1, F1A, B0AA, F2
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
6. Others
 Sof(F1A)=1-FVAR(1)
 Sof(F2A)=0.33333*(1-FVAR(2))
 Sof(F2)=0.33333*FVAR(2)
 Sof(F1)=FVAR(1)
7.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B)
7.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C1(H1), C2(H2)
;
_shelx_res_checksum              61813
_olex2_date_sample_data_collection 2012-12-04
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.208
_oxdiff_exptl_absorpt_empirical_full_min 0.877