Unravelling exceptional acetylene and carbon dioxide adsorption within a tetra-amide functionalized metal-organic framework
Florian Moreau; Ivan da Silva; Nada H. Al Smail; Timothy L. Easun; Mathew Savage; Harry G. W. Godfrey; Stewart F. Parker; Pascal Manuel; Sihai Yang; Martin Schroder; Nature Communications 8 (2017) 14085–; doi:10.1038/ncomms14085

data_1547886
_publ_section_title
;
 Unravelling exceptional acetylene and carbon dioxide adsorption within a
 tetra-amide functionalized metal-organic framework
;
_journal_name_full               'Nature Communications'
_journal_page_first              14085
_journal_paper_doi               10.1038/ncomms14085
_journal_volume                  8
_journal_year                    2017
_chemical_formula_moiety         '0.25(C192 H120 Cu16 N16 O96)'
_chemical_formula_sum            'C92 H173 Cu4 N9 O49 S6'
_chemical_formula_weight         2635.90
_chemical_name_common            MFM-188
_space_group_crystal_system      tetragonal
_space_group_IT_number           128
_space_group_name_Hall           '-P 4 2n'
_space_group_name_H-M_alt        'P 4/m n c'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date
;
'Tue Jul 01 14:04:53 2014'
;
_audit_creation_method
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   18.6841(7)
_cell_length_b                   18.6841(7)
_cell_length_c                   34.6796(17)
_cell_measurement_reflns_used    6817
_cell_measurement_temperature    120.03(10)
_cell_measurement_theta_max      73.4400
_cell_measurement_theta_min      4.1840
_cell_volume                     12106.5(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.03(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3271
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_details
;
  1 omega   -8.00   19.00   1.0000  160.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   37.0000 -120.0000 27

  2 omega  -48.00   22.00   1.0000  160.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   37.0000  -60.0000 70

  3 omega   64.00  109.00   1.0000  160.0000
omega____ theta____ kappa____ phi______ frames
    -       42.7573  142.0000 -160.0000 45

  4 omega   46.00   90.00   1.0000  640.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000 -120.0000 44

  5 omega  101.00  169.00   1.0000  640.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   30.0000  150.0000 68

  6 omega   35.00   97.00   1.0000  640.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -45.0000 -180.0000 62

  7 omega   88.00  124.00   1.0000  640.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -77.0000   30.0000 36

  8 omega   13.00  114.00   1.0000  160.0000
omega____ theta____ kappa____ phi______ frames
    -       42.7573   77.0000  -60.0000 101

  9 omega    2.00   97.00   1.0000  160.0000
omega____ theta____ kappa____ phi______ frames
    -       42.7573 -125.0000   90.0000 95

 10 omega   18.00  111.00   1.0000  160.0000
omega____ theta____ kappa____ phi______ frames
    -       42.7573   57.0000  150.0000 93

 11 omega   78.00  103.00   1.0000  640.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   61.0000  -30.0000 25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV1000, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0114585000
_diffrn_orient_matrix_UB_12      0.0032315000
_diffrn_orient_matrix_UB_13      -0.0439401000
_diffrn_orient_matrix_UB_21      0.0620756000
_diffrn_orient_matrix_UB_22      0.0532304000
_diffrn_orient_matrix_UB_23      0.0057879000
_diffrn_orient_matrix_UB_31      0.0530918000
_diffrn_orient_matrix_UB_32      -0.0628872000
_diffrn_orient_matrix_UB_33      0.0027464000
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1650
_diffrn_reflns_av_unetI/netI     0.2206
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            44853
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.488
_diffrn_reflns_theta_min         2.686
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_target            Cu
_diffrn_source_type              'GV1000 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.235
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_correction_T_min  0.747
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_description       plate
_exptl_crystal_F_000             5568
_exptl_crystal_size_max          0.1427
_exptl_crystal_size_mid          0.1400
_exptl_crystal_size_min          0.0120
_platon_squeeze_details
;
Approximately 68% of the unit cell volume comprises a large region of
disordered solvent which could not be modelled as discrete atomic sites.
We employed PLATON SQUEEZE to calculate the contribution to the diffraction
from the solvent region and thereby produced a set of solvent-free diffraction
intensities. SQUEEZE estimated a total count of 3034 electrons per unit cell,
which were assigned to be 24 EtOH, 20 DEF, 24 DMSO and 32 water molecules per unit cell. 
The final formula was calculated from TGA combined with elemental analysis data.
;
_refine_diff_density_max         1.261
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.915
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         6006
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.915
_refine_ls_R_factor_all          0.1305
_refine_ls_R_factor_gt           0.0855
_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^)+(0.1612P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2263
_refine_ls_wR_factor_ref         0.2746
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3021
_reflns_number_total             6006
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ncomms14085-s2.cif
_cod_data_source_block           cufyni_sq
_cod_database_code               1547886
_nottingham_internal_coll_name   CUFYNI
_nottingham_internal_coll_number 13733
_nottingham_internal_coll_client FYM/MS
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'omega scans'
_nottingham_internal_coll_frame_time '160.0000, 640.0000'
_nottingham_internal_coll_frame_width 1.0000
_nottingham_internal_coll_user   pczfym
_nottingham_internal_coll_location NOTTS
_nottingham_internal_process_user pczfym
_platon_squeeze_void_probe_radius 1.20
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C48 H30 N4 O24 Cu4'
_cell_oxdiff_angle_alpha         89.893(3)
_cell_oxdiff_angle_beta          90.028(3)
_cell_oxdiff_angle_gamma         90.021(4)
_cell_oxdiff_length_a            18.6775(9)
_cell_oxdiff_length_b            18.6843(9)
_cell_oxdiff_length_c            34.6916(11)
_cell_oxdiff_measurement_reflns_used 6820
_cell_oxdiff_volume              12106.5(9)
_reflns_odcompleteness_completeness 97.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O6(H6A,H6B)
2.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C15(H15), C18(H18), C21(H21), N1(H1)
;
_shelx_res_checksum              30832
_shelx_hkl_checksum              81063
_shelx_fab_checksum              2756
_olex2_exptl_crystal_mounting_method "'in fomblin film on a micromount"
_olex2_submission_special_instructions 'No special instructions were received'