Solvent-switchable continuous-breathing behaviour in a diamoniod metal-organic framework and its influence on CO2 vs CH4 selectivity
Carrington, Elliot J.; McAnally, Craig A.; Fletcher, Ashleigh J.; Thompson, Stephen P.; Warren, Mark; Brammer, Lee; Nature Chemistry 9 (2017) 882–889; doi:10.1038/nchem.2747

data_1551161
_publ_section_title
;
 Solvent-switchable continuous-breathing behaviour in a diamoniod
 metal-organic framework and its influence on CO2 vs CH4 selectivity
;
_journal_name_full               'Nature Chemistry'
_journal_page_first              882
_journal_page_last               889
_journal_paper_doi               10.1038/nchem.2747
_journal_volume                  9
_journal_year                    2017
_chemical_formula_moiety         'C18 H18 In N3 O8'
_chemical_formula_sum            'C18 H18 In N3 O8'
_chemical_formula_weight         519.17
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d'
_symmetry_space_group_name_Hall  '-F 2uv 2vw'
_symmetry_space_group_name_H-M   'F d d d :2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   15.3069(5)
_cell_length_b                   26.9467(8)
_cell_length_c                   31.2840(10)
_cell_measurement_reflns_used    9864
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.491
_cell_measurement_theta_min      2.481
_cell_volume                     12903.7(7)
_computing_cell_refinement       'SAINT v7.60A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.60A (Bruker, 2009)'
_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
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_unetI/netI     0.0124
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            43105
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.526
_diffrn_reflns_theta_min         1.663
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.765
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6666
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0526 before and 0.0433 after correction.
The Ratio of minimum to maximum transmission is 0.8940.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.069
_exptl_crystal_density_meas      .
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             4160
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.205
_refine_diff_density_min         -0.858
_refine_diff_density_rms         0.217
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.204
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         3725
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.208
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0523
_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^)+(0.1080P)^2^+158.6311P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1834
_refine_ls_wR_factor_ref         0.1961
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3136
_reflns_number_total             3725
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            nchem.2747-s2.cif
_cod_data_source_block           A1
_cod_database_code               1551161
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C11-N2B
 1.48 with sigma of 0.02
 C9-N2A
 1.48 with sigma of 0.02
 N2A-C10
 1.48 with sigma of 0.02
 C9-C10
 2.47 with sigma of 0.02
3. Restrained planarity
 N1B, C3B, C7B, C4B, C6B
 with sigma of 0.1
 N1A, C3A, C4A, C6A, C7A
 with sigma of 0.1
4. Others
 Sof(N1B)=Sof(H1BA)=Sof(H1BB)=Sof(C3B)=Sof(C7B)=Sof(H7B)=Sof(C4B)=Sof(H4B)=
 Sof(C6B)=Sof(H6B)=1-FVAR(1)
 Sof(N1A)=Sof(H1AA)=Sof(H1AB)=Sof(C3A)=Sof(C4A)=Sof(H4A)=Sof(C6A)=Sof(H6A)=
 Sof(C7A)=Sof(H7A)=FVAR(1)
 Fixed Sof: N2A(0.25) H2AA(0.25) H2AB(0.25) C9(0.25) H9A(0.25) H9B(0.25)
 H9C(0.25) C10(0.25) H10A(0.25) H10B(0.25) H10C(0.25) N2B(0.25) H2BA(0.25)
 H2BB(0.25) C11(0.5) H11A(0.5) H11C(0.5) H11B(0.5)
5.a Rotating group:
 N1A(H1AA,H1AB), N1B(H1BA,H1BB)
5.b Secondary CH2 refined with riding coordinates:
 N2A(H2AA,H2AB), N2B(H2BA,H2BB)
5.c Me refined with riding coordinates:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11C,H11B)
5.d Aromatic/amide H refined with riding coordinates:
 C4A(H4A), C6A(H6A), C7A(H7A), C7B(H7B), C4B(H4B), C6B(H6B)
;
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              38071
_shelx_hkl_checksum              8586
_olex2_date_sample_data_collection '23 June 2014'
_olex2_exptl_crystal_mounting_method 'on Loop under Oil'
_olex2_submission_special_instructions 'No special instructions were received'