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_1545594
_publ_section_title
;
 In-MOFs based on amide functionalised flexible linkers
;
_journal_name_full               'Faraday Discuss.'
_journal_paper_doi               10.1039/C7FD00085E
_journal_year                    2017
_chemical_formula_moiety         'C12 H11 In N2 O7'
_chemical_formula_sum            'C12 H11 In N2 O7'
_chemical_formula_weight         410.05
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-02-10
_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                77.815(7)
_cell_angle_beta                 78.748(5)
_cell_angle_gamma                85.773(5)
_cell_formula_units_Z            2
_cell_length_a                   7.2372(4)
_cell_length_b                   10.1596(8)
_cell_length_c                   11.8645(8)
_cell_measurement_reflns_used    2896
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.2950
_cell_measurement_theta_min      1.7790
_cell_volume                     835.84(10)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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   60.00    --  -20.00 -68.00   0.00  125
  2  \w   -110.00  15.00   1.00   60.00    --  -20.00 -68.00 120.00  125
  3  \w   -110.00  15.00   1.00   60.00    --  -20.00 -68.00 240.00  125
  4  \w   -110.00  15.00   1.00   60.00    --  -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      -0.0419325000
_diffrn_orient_matrix_UB_12      -0.0258361000
_diffrn_orient_matrix_UB_13      0.0590596000
_diffrn_orient_matrix_UB_21      0.0024566000
_diffrn_orient_matrix_UB_22      -0.0653833000
_diffrn_orient_matrix_UB_23      -0.0126075000
_diffrn_orient_matrix_UB_31      0.0907355000
_diffrn_orient_matrix_UB_32      -0.0128420000
_diffrn_orient_matrix_UB_33      0.0150043000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0888
_diffrn_reflns_av_unetI/netI     0.1213
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9533
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         1.787
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.446
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78461
_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    1.629
_exptl_crystal_description       block
_exptl_crystal_F_000             404
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.580
_refine_diff_density_min         -1.411
_refine_diff_density_rms         0.194
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         3415
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.1162
_refine_ls_R_factor_gt           0.0678
_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^)+(0.0894P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1567
_refine_ls_wR_factor_ref         0.1809
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2077
_reflns_number_total             3415
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7fd00085e2.cif
_cod_data_source_block           c1_jh_pdg_47_2_sq
_cod_database_code               1545594
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.31
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O003) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
3. Rigid body (RIGU) restrains
 C00G, C00K, O007, O005
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Secondary CH2 refined with riding coordinates:
 C00C(H00B,H00C), C00G(H00E,H00F)
4.b Aromatic/amide H refined with riding coordinates:
 O003(H003), N006(H006), N00A(H00A), C00D(H00D), C00I(H00I), C00J(H00J),
 C00M(H00M)
;
_shelx_res_checksum              99053
_shelx_hkl_checksum              94983
_shelx_fab_checksum              94444
_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 1.354
_oxdiff_exptl_absorpt_empirical_full_min 0.811