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_4126609
_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), 2(C2 H4)'
_chemical_formula_sum            'C12 H10 Co2 O6'
_chemical_formula_weight         362.02
_space_group_crystal_system      trigonal
_space_group_IT_number           160
_space_group_name_Hall           'R 3 -2"'
_space_group_name_H-M_alt        'R 3 m :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'intrinsic phasing'
_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                   25.751(4)
_cell_length_b                   25.751(4)
_cell_length_c                   6.8192(11)
_cell_measurement_reflns_used    3795
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.23
_cell_measurement_theta_min      3.89
_cell_volume                     3916.1(11)
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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     0.8856
_diffrn_reflns_av_R_equivalents  0.0738
_diffrn_reflns_av_unetI/netI     0.0672
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            6619
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        32.097
_diffrn_reflns_theta_max         32.231
_diffrn_reflns_theta_min         3.415
_diffrn_source                   'Advanced Light Source station 11.3.1'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.485
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.611
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1382 before and 0.1000 after correction.
The Ratio of minimum to maximum transmission is 0.6187.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.0036
_exptl_crystal_size_min          0.0036
_refine_diff_density_max         0.569
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details
;
 Flack x determined using 625 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.14(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     94
_refine_ls_number_reflns         1642
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0456
_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^)+(0.0564P)^2^+5.2548P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1099
_refine_ls_wR_factor_ref         0.1151
_reflns_Friedel_coverage         0.905
_reflns_Friedel_fraction_full    0.926
_reflns_Friedel_fraction_max     0.919
_reflns_number_gt                1478
_reflns_number_total             1642
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b06397_si_002.cif
_cod_data_source_block           mtk011s
_cod_depositor_comments
;
 Updating space group information.

 Antanas Vaitkus,
 2018-07-04

The following automatic conversions were performed:

'_atom_sites_solution_secondary' value 'diffmap' was changed to
'difmap'.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        3916.1(14)
_cod_database_code               4126609
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.988
_shelx_estimated_absorpt_t_min   0.573
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C7-C6
 1.3305 with sigma of 0.005
3. Rigid body (RIGU) restrains
 C7, C6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4)
;
_shelx_res_checksum              30069
_shelx_hkl_checksum              93690
_olex2_submission_special_instructions 'No special instructions were received'