Controlling interpenetration through linker conformation in the modulated synthesis of Sc metal–organic frameworks
Marshall, Ross J.; Lennon, Ciaran T.; Tao, Andi; Senn, Hans M.; Wilson, Claire; Fairen-Jimenez, David; Forgan, Ross S.; Journal of Materials Chemistry A 6 (2018) 1181–; doi:10.1039/C7TA09699B

data_7236666
_publ_section_title
;
 Controlling interpenetration through linker conformation in the modulated
 synthesis of Sc metal--organic frameworks
;
_journal_issue                   3
_journal_name_full               'Journal of Materials Chemistry A'
_journal_page_first              1181
_journal_paper_doi               10.1039/C7TA09699B
_journal_volume                  6
_journal_year                    2018
_chemical_formula_moiety         'C18 H9 N3 O6 Sc'
_chemical_formula_sum            'C18 H9 N3 O6 Sc'
_chemical_formula_weight         408.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-05-31
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-10-06 deposited with the CCDC.
2017-12-15 downloaded from the CCDC.
;
_cell_angle_alpha                90.0
_cell_angle_beta                 102.581(4)
_cell_angle_gamma                90.0
_cell_formula_units_Z            8
_cell_length_a                   8.8618(4)
_cell_length_b                   48.6247(16)
_cell_length_c                   14.5573(6)
_cell_measurement_reflns_used    16426
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5590
_cell_measurement_theta_min      2.1940
_cell_volume                     6122.2(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)
;
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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    -27.00  73.00   0.50   25.00    --  -17.00  72.00 150.00  200
  2  \w    -69.00  22.00   0.50   25.00    --  -17.00 -72.00  30.00  182
  3  \w    -69.00  22.00   0.50   25.00    --  -17.00 -72.00-150.00  182
  4  \w    -84.00 -21.00   0.50   25.00    --  -17.00   0.00  30.00  126
  5  \w    -32.00 -12.00   0.50   25.00    --  -17.00  54.00   0.00   40
  6  \w    -35.00  73.00   0.50   25.00    --  -17.00  72.00-150.00  216
  7  \w    -77.00  22.00   0.50   25.00    --  -17.00 -72.00  90.00  198
  8  \w    -68.00  22.00   0.50   25.00    --  -17.00 -72.00 -90.00  180
  9  \w    -90.00  -4.00   0.50   25.00    --  -17.00   0.00  90.00  172
 10  \w    -27.00  -7.00   0.50   25.00    --  -17.00  72.00  30.00   40
 11  \w    -35.00  23.00   0.50   25.00    --  -17.00  72.00 120.00  116
;
_diffrn_measurement_device       'four-circle \k goniometer'
_diffrn_measurement_device_type
;
Rigaku FRE+ equipped with HF Varimax confocal mirrors and an AFC10 goniometer and HG Saturn 724+ detector
;
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0170620500
_diffrn_orient_matrix_UB_12      -0.0134753500
_diffrn_orient_matrix_UB_13      -0.0133641000
_diffrn_orient_matrix_UB_21      -0.0778227000
_diffrn_orient_matrix_UB_22      -0.0039432000
_diffrn_orient_matrix_UB_23      -0.0022943000
_diffrn_orient_matrix_UB_31      -0.0195935500
_diffrn_orient_matrix_UB_32      0.0039535500
_diffrn_orient_matrix_UB_33      -0.0480291000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, HF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0724
_diffrn_reflns_av_unetI/netI     0.0175
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       62
_diffrn_reflns_limit_k_min       -62
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            54506
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.509
_diffrn_reflns_theta_min         1.660
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku FRE+'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.265
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90265
_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            Colourless
_exptl_crystal_density_diffrn    0.886
_exptl_crystal_description       Block
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.736
_refine_diff_density_min         -0.735
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         13433
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1053
_refine_ls_R_factor_gt           0.0899
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1601P)^2^+8.8352P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2508
_refine_ls_wR_factor_ref         0.2704
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11018
_reflns_number_total             13433
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.9882\% 
 around [0.90 0.00 -0.45] (reciprocal) or [1.00 -0.00 -0.06] (direct)
;
_cod_data_source_file            c7ta09699b2.cif
_cod_data_source_block           2016ncs0620r1_hklf5_sq
_cod_original_cell_volume        6122.1(4)
_cod_database_code               7236666
_shelx_shelxl_version_number     2016/6
_cell_oxdiff_angle_alpha         89.963(2)
_cell_oxdiff_angle_beta          102.566(3)
_cell_oxdiff_angle_gamma         89.988(3)
_cell_oxdiff_length_a            8.8579(4)
_cell_oxdiff_length_b            48.6325(12)
_cell_oxdiff_length_c            14.5605(4)
_cell_oxdiff_measurement_reflns_used 15738
_cell_oxdiff_volume              6122.1(3)
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5057(18)
 0.4943(18)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C11(H11), C15(H15), C16(H16),
 C17(H17)
;
_shelx_res_checksum              86572
_shelx_hkl_checksum              58454
_shelx_fab_checksum              11469
_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 1.627
_oxdiff_exptl_absorpt_empirical_full_min 0.763
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2