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_1545256
_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), 4.63(B0.43 F1.73)'
_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
_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                   10.3690(5)
_cell_length_b                   10.3690(5)
_cell_length_c                   22.9628(15)
_cell_measurement_reflns_used    877
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      24.9582
_cell_measurement_theta_min      3.4904
_cell_volume                     2138.1(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      120.15
_diffrn_measured_fraction_theta_full 0.902
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0883
_diffrn_reflns_Laue_measured_fraction_full 0.902
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            1300
_diffrn_reflns_point_group_measured_fraction_full 0.902
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.012
_diffrn_reflns_theta_min         3.497
_exptl_absorpt_coefficient_mu    0.444
_exptl_absorpt_correction_type   none
_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    1.485
_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         2.320
_refine_diff_density_min         -1.012
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         1300
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.1389
_refine_ls_R_factor_gt           0.1090
_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/[\s^2^(Fo^2^)+(0.1380P)^2^+19.7224P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2739
_refine_ls_wR_factor_ref         0.2978
_reflns_Friedel_coverage         0.000
_reflns_number_gt                981
_reflns_number_total             1300
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc05122g3.cif
_cod_data_source_block           CCP-2_LS
_cod_depositor_comments
'Adding full bibliography for 1545255--1545262.cif.'
_cod_database_code               1545256
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.991
_shelx_estimated_absorpt_t_min   0.978
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.631(8) 0.369(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H) groups
3. Restrained distances
 B1-F1
 1.38 with sigma of 0.01
 B1-F2
 1.38 with sigma of 0.01
 B1'-F1'
 1.38 with sigma of 0.01
 B1'-F2'
 1.38 with sigma of 0.01
4. Rigid body (RIGU) restrains
 B1, F1, F2
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F2', B1', F1'
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Sof(F2')=1-FVAR(1)
 Sof(B1')=Sof(F1')=0.33333*(1-FVAR(2))
 Sof(B1)=Sof(F1)=0.33333*FVAR(2)
 Sof(F2)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8), C9(H9)
6.c Fitted pentagon refined as free rotating group:
 N1(C2,N3,N4,N5)
;
_shelx_res_checksum              6907
_olex2_submission_special_instructions 'No special instructions were received'