M2(m-dobdc) (M = Mn, Fe, Co, Ni) Metal-Organic Frameworks as Highly-Selective, High-Capacity Adsorbents for Olefin/Paraffin Separations.
Bachman, Jonathan E.; Kapelewski, Matthew T.; Reed, Douglas A.; Gonzalez, Miguel I.; Long, Jeffrey R.; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b06397

data_4126610
_publ_section_title
;
 M2(m-dobdc) (M = Mn, Fe, Co, Ni) Metal-Organic Frameworks as
 Highly-Selective, High-Capacity Adsorbents for Olefin/Paraffin
 Separations.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b06397
_journal_year                    2017
_chemical_formula_moiety         'Co2 (C8 H2 O6), 1.89(C2 H4)'
_chemical_formula_sum            'C11.78 H9.57 Co2 O6'
_chemical_formula_weight         365.03
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-05-15
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   25.720(7)
_cell_length_b                   25.720(7)
_cell_length_c                   6.853(2)
_cell_measurement_reflns_used    4864
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.616
_cell_measurement_theta_min      2.659
_cell_volume                     3926.0(19)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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_temperature      100(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.966
_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     0.6888
_diffrn_reflns_av_R_equivalents  0.0849
_diffrn_reflns_av_unetI/netI     0.0811
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2092
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        24.411
_diffrn_reflns_theta_max         26.713
_diffrn_reflns_theta_min         2.659
_diffrn_source                   'Advanced Light Source station 11.3.1'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.748
_exptl_absorpt_correction_T_max  0.933
_exptl_absorpt_correction_T_min  0.525
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1096 before and 0.0766 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.1155 before and 0.0778 after correction.
 The Ratio of minimum to maximum transmission is 0.56.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 24025 reflections, Rint = 0.0849
 (15116 with I > 3sig(I), Rint = 0.0728)
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.827
_refine_diff_density_min         -0.845
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     104
_refine_ls_number_reflns         2092
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0613
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+51.6791P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1113
_refine_ls_wR_factor_ref         0.1204
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1733
_reflns_number_total             2092
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b06397_si_003.cif
_cod_data_source_block           twin4
_cod_original_cell_volume        3926(2)
_cod_database_code               4126610
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.933
_shelx_estimated_absorpt_t_min   0.845
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.570(2)
 0.430(2)
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
 C5-C6
 1.3305 with sigma of 0.005
 C6-H6A = C6-H6B = C5-H5A = C5-H5B
 0.95 with sigma of 0.02
 H6B-C5 = H6A-C5 = C6-H5B = C6-H5A
 2.081 with sigma of 0.02
4. Restrained planarity
 C5, H5A, H5B, C6, H6A, H6B
 with sigma of 0.1
5. Others
 Fixed Sof: C5(0.946) H5A(0.946) H5B(0.946) C6(0.946) H6A(0.946) H6B(0.946)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3)
;
_shelx_res_checksum              65528
_shelx_hkl_checksum              15928
_olex2_submission_special_instructions 'No special instructions were received'