In-MOFs based on amide functionalised flexible linkers
Haddad, Jibreel; Whitehead, George F. S.; Katsoulidis, Alexandros; Rosseinsky, Matthew J.; Faraday Discuss.  (2017) –; doi:10.1039/C7FD00085E

data_1545593
_publ_section_title
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 In-MOFs based on amide functionalised flexible linkers
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_journal_name_full               'Faraday Discuss.'
_journal_paper_doi               10.1039/C7FD00085E
_journal_year                    2017
_chemical_formula_moiety         'C11 H10 In N O6, H2O'
_chemical_formula_sum            'C11 H12 In N O7'
_chemical_formula_weight         385.04
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-02-24
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2017-02-24 deposited with the CCDC.
2017-03-17 downloaded from the CCDC.
;
_cell_angle_alpha                90.0
_cell_angle_beta                 93.708(8)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   8.0483(8)
_cell_length_b                   7.2282(3)
_cell_length_c                   24.2472(18)
_cell_measurement_reflns_used    2515
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.3350
_cell_measurement_theta_min      2.5340
_cell_volume                     1407.62(18)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -110.00  15.00   1.00    5.00    --  -20.00 -68.00   0.00  125
  2  \w   -110.00  15.00   1.00    5.00    --  -20.00 -68.00 120.00  125
  3  \w   -110.00  15.00   1.00    5.00    --  -20.00 -68.00 240.00  125
  4  \w   -110.00  15.00   1.00    5.00    --  -20.00 -30.00  90.00  125
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0130581000
_diffrn_orient_matrix_UB_12      0.0727947000
_diffrn_orient_matrix_UB_13      0.0188266000
_diffrn_orient_matrix_UB_21      -0.0013247000
_diffrn_orient_matrix_UB_22      -0.0649949000
_diffrn_orient_matrix_UB_23      0.0219115000
_diffrn_orient_matrix_UB_31      0.0873275000
_diffrn_orient_matrix_UB_32      0.0099239000
_diffrn_orient_matrix_UB_33      0.0050536000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0929
_diffrn_reflns_av_unetI/netI     0.0520
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            3669
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.510
_diffrn_reflns_theta_min         2.536
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.708
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89900
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.817
_exptl_crystal_description       plate
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.691
_refine_diff_density_min         -2.051
_refine_diff_density_rms         0.210
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         3669
_refine_ls_number_restraints     213
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.1138
_refine_ls_R_factor_gt           0.0867
_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^)+(0.0698P)^2^+36.7518P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1869
_refine_ls_wR_factor_ref         0.1993
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2809
_reflns_number_total             3669
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7fd00085e2.cif
_cod_data_source_block           c2_jh_csa_36_4_twin1_hklf4
_cod_database_code               1545593
_shelx_shelxl_version_number     2016/6
_cell_oxdiff_angle_alpha         89.929(5)
_cell_oxdiff_angle_beta          93.685(6)
_cell_oxdiff_angle_gamma         90.019(6)
_cell_oxdiff_length_a            8.0487(6)
_cell_oxdiff_length_b            7.2310(5)
_cell_oxdiff_length_c            24.2358(16)
_cell_oxdiff_measurement_reflns_used 2515
_cell_oxdiff_volume              1407.62(17)
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.570(3) 0.430(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All O(H) groups
3. Shared sites
{C12A, C12}
4. Uiso/Uaniso restraints and constraints
Uanis(O19) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C0AA) = Uanis(C18)
Uanis(C5) = Uanis(C4AA)
Uanis(N8) = Uanis(N1)
Uanis(C10) = Uanis(C10A)
Uanis(C15A) = Uanis(C15)
Uanis(O3) = Uanis(O14)
Uanis(C6AA) = Uanis(C6)
Uanis(C12A) = Uanis(C12)
5. Rigid body (RIGU) restrains
 C1AA, In1, O19, O2, C2AA, O4, C5AA, C3AA, N1, O3, N8, O14, C6, C6AA, C15A,
 C4AA, C5, C15, C10, C18, C0AA, C10A, C12, C12A, C7, O5, O6
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.004
6. Others
 Sof(O3)=Sof(O1AA)=Sof(C10A)=Sof(H10A)=Sof(C12A)=Sof(C0AA)=Sof(H0AA)=Sof(C5)=
 Sof(H5)=Sof(C6AA)=Sof(C15)=Sof(H15)=Sof(N8)=Sof(H8)=1-FVAR(1)
 Sof(C12)=Sof(C10)=Sof(H10)=Sof(C15A)=Sof(H15A)=Sof(C6)=Sof(C4AA)=Sof(H4AA)=
 Sof(C18)=Sof(H18)=Sof(N1)=Sof(H1)=Sof(O1)=Sof(O14)=FVAR(1)
7.a Secondary CH2 refined with riding coordinates:
 C3AA(H3AA,H3AB), C5AA(H5AA,H5AB)
7.b Aromatic/amide H refined with riding coordinates:
 O19(H19), C10(H10), C15A(H15A), C4AA(H4AA), C18(H18), N1(H1), C10A(H10A),
 C0AA(H0AA), C5(H5), C15(H15), N8(H8)
7.c Fitted hexagon refined as free rotating group:
 C12(C10,C15A,C6,C4AA,C18), C10A(C12A,C0AA,C5,C6AA,C15)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.125
_oxdiff_exptl_absorpt_empirical_full_min 0.882
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
_twin_special_details
;
Component 2 rotated by 179.9927\% 
 around [-0.00 -0.00 1.00] (reciprocal) or [0.18 -0.01 0.98] (direct)
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