Thermodynamic Separation of 1-Butene from 2-Butene in Metal-Organic Frameworks with Open Metal Sites.
Barnett, Brandon R.; Parker, Surya T.; Paley, Maria V.; Gonzalez, Miguel I.; Biggins, Naomi; Oktawiec, Julia; Long, Jeffrey R.; Journal of the American Chemical Society 141 (2019) 18325–18333; doi:10.1021/jacs.9b09942

data_4133726
_publ_section_title
;
 Thermodynamic Separation of 1-Butene from 2-Butene in Metal-Organic
 Frameworks with Open Metal Sites.
;
_journal_issue                   45
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              18325
_journal_page_last               18333
_journal_paper_doi               10.1021/jacs.9b09942
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         '(C8 H2 Co2 O6), 1.48(C4 H8)'
_chemical_formula_sum            'C13.93 H13.86 Co2 O6'
_chemical_formula_weight         395.13
_chemical_name_common            Co2(dobdc)(trans-2-butene)1.48
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-08-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   25.8130(11)
_cell_length_b                   25.8130(11)
_cell_length_c                   6.8924(3)
_cell_measurement_reflns_used    9805
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      37.96
_cell_measurement_theta_min      3.37
_cell_volume                     3977.2(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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, )'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 with PHOTON100 CMOS detector'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            41645
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         37.960
_diffrn_reflns_theta_min         3.372
_diffrn_source                   'Advanced Light Source station 11.3.1'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.405
_exptl_absorpt_correction_T_max  0.967
_exptl_absorpt_correction_T_min  0.358
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 41645 reflections, Rint = 0.0532
 (29969 with I > 3sig(I), Rint = 0.0493)
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1795
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.014
_exptl_crystal_size_min          0.014
_refine_diff_density_max         1.851
_refine_diff_density_min         -0.742
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     113
_refine_ls_number_reflns         3780
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0455
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0649P)^2^+12.8204P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1188
_refine_ls_wR_factor_ref         0.1236
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3304
_reflns_number_total             3780
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b09942_si_001.cif
_cod_data_source_block           Co2dobdc_trans-2-butene_1.48
_cod_original_cell_volume        3977.2(4)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4133726
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.967
_shelx_estimated_absorpt_t_min   0.850
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5771(16)
 0.4229(16)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C5_$1-C6_$1 \\sim C8_$1-C7_$1
 with sigma of 0.02
4. Rigid body (RIGU) restrains
 C8, C7, C6, C5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C7)=Sof(H7)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C6)=Sof(H6)=Sof(C5)=
 Sof(H5A)=Sof(H5B)=Sof(H5C)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), C6(H6)
6.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C5(H5A,H5B,H5C)
;
_shelx_res_checksum              71388
_shelx_hkl_checksum              36802
_olex2_submission_special_instructions 'No special instructions were received'