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_7236667
_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         'C36 H23 Cl3 Cu1.50 N6 O16 Sc3'
_chemical_formula_sum            'C36 H23 Cl3 Cu1.5 N6 O16 Sc3'
_chemical_formula_weight         1132.14
_space_group_crystal_system      hexagonal
_space_group_IT_number           190
_space_group_name_Hall           'P -6c -2c'
_space_group_name_H-M_alt        'P -6 2 c'
_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                 90.0
_cell_angle_gamma                120.0
_cell_formula_units_Z            2
_cell_length_a                   17.9930(10)
_cell_length_b                   17.9930(10)
_cell_length_c                   24.7387(11)
_cell_measurement_reflns_used    12990
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.9880
_cell_measurement_theta_min      2.1130
_cell_volume                     6936.1(6)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -35.00  73.00   1.00  120.00    --  -17.00  72.00-180.00  108
  2  \w    -78.00  22.00   1.00  120.00    --  -17.00 -72.00  60.00  100
  3  \w    -66.00  22.00   1.00  120.00    --  -17.00 -72.00-120.00   88
  4  \w    -89.00  21.00   1.00  120.00    --  -17.00   0.00  60.00  110
  5  \w    -32.00 -12.00   1.00  120.00    --  -17.00  54.00  30.00   20
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_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      0.0330969000
_diffrn_orient_matrix_UB_12      0.0415755000
_diffrn_orient_matrix_UB_13      0.0074686000
_diffrn_orient_matrix_UB_21      0.0297445000
_diffrn_orient_matrix_UB_22      -0.0149888000
_diffrn_orient_matrix_UB_23      0.0006068000
_diffrn_orient_matrix_UB_31      0.0095229000
_diffrn_orient_matrix_UB_32      0.0108066000
_diffrn_orient_matrix_UB_33      -0.0276818000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  graphite
_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  0.1270
_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            55176
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.025
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         2.102
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.448
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56414
_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            Green
_exptl_crystal_density_diffrn    0.542
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1133
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.045
_refine_diff_density_max         0.259
_refine_diff_density_min         -0.210
_refine_diff_density_rms         0.035
_refine_ls_abs_structure_details
;
 Flack x determined using 891 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.508(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.952
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     105
_refine_ls_number_reflns         4204
_refine_ls_number_restraints     99
_refine_ls_restrained_S_all      0.949
_refine_ls_R_factor_all          0.0910
_refine_ls_R_factor_gt           0.0614
_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^)+(0.1244P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1703
_refine_ls_wR_factor_ref         0.1891
_reflns_Friedel_coverage         0.813
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                2680
_reflns_number_total             4204
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ta09699b2.cif
_cod_data_source_block           2016ncs0703_sq
_cod_original_formula_sum        'C36 H23 Cl3 Cu1.50 N6 O16 Sc3'
_cod_database_code               7236667
_shelx_shelxl_version_number     2016/6
_cell_oxdiff_angle_alpha         90.062(5)
_cell_oxdiff_angle_beta          90.011(6)
_cell_oxdiff_angle_gamma         119.916(9)
_cell_oxdiff_length_a            17.9854(17)
_cell_oxdiff_length_b            17.9912(15)
_cell_oxdiff_length_c            24.7307(11)
_cell_oxdiff_measurement_reflns_used 12899
_cell_oxdiff_volume              6936.1(9)
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C2-C3 = N1-C3 = N1-C6 = C5-C6 = C4-C2 = C4-C5
 1.39 with sigma of 0.02
3. Restrained planarity
 C2, C4, C5, C3, N1, C6
 with sigma of 0.1
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: Cu1(0.25) Cl1(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5)
;
_shelx_res_checksum              80750
_shelx_hkl_checksum              96325
_shelx_fab_checksum              88441
_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 2.653
_oxdiff_exptl_absorpt_empirical_full_min 0.390