An expanded MIL-53-type coordination polymer with a reactive pendant ligand
Kunicki, Hannah; Chamberlain, Thomas W.; Clarkson, Guy J.; Kashtiban, Reza J.; Hooper, Joseph E.; Dawson, Daniel M.; Ashbrook, Sharon E.; Walton, Richard I.; CrystEngComm 20 (2018) 4355–; doi:10.1039/C8CE00891D

data_7231205
_publ_section_title
;
 An expanded MIL-53-type coordination polymer with a reactive pendant
 ligand
;
_journal_issue                   31
_journal_name_full               CrystEngComm
_journal_page_first              4355
_journal_paper_doi               10.1039/C8CE00891D
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         'C13 H11 N O, C4 H3 O2'
_chemical_formula_sum            'C17 H14 N O3'
_chemical_formula_weight         280.29
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-03-01
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3461 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-05-08 deposited with the CCDC.
2018-06-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.7663(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.43953(14)
_cell_length_b                   20.7625(4)
_cell_length_c                   8.87540(15)
_cell_measurement_reflns_used    2604
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      76.5820
_cell_measurement_theta_min      4.2510
_cell_volume                     1337.03(4)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48)'
_computing_data_collection
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48)'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48)'
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2833
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_details
'#__ type_ start__ end____ width___ exp.time_ 1 omega -39.00 16.00 1.0000 22.5000 omega____ theta____ kappa____ phi______ frames - -41.3359 38.0000 -120.0000 55 #__ type_ start__ end____ width___ exp.time_ 2 omega -111.00 -13.00 1.0000 22.5000 omega____ theta____ kappa____ phi______ frames - -41.3359 -57.0000 -60.0000 98 #__ type_ start__ end____ width___ exp.time_ 3 omega 5.00 82.00 1.0000 22.5000 omega____ theta____ kappa____ phi______ frames - 41.3359 -99.0000 150.0000 77 #__ type_ start__ end____ width___ exp.time_ 4 omega 63.00 151.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 114.0000 178.0000 -90.0000 88 #__ type_ start__ end____ width___ exp.time_ 5 omega 89.00 177.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 114.0000 30.0000 150.0000 88 #__ type_ start__ end____ width___ exp.time_ 6 omega 74.00 105.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 114.0000 -94.0000 90.0000 31 #__ type_ start__ end____ width___ exp.time_ 7 omega 38.00 116.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 114.0000 -111.0000 60.0000 78 #__ type_ start__ end____ width___ exp.time_ 8 omega 88.00 147.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 114.0000 30.0000 90.0000 59 #__ type_ start__ end____ width___ exp.time_ 9 omega 41.00 94.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 114.0000 -45.0000 -120.0000 53 #__ type_ start__ end____ width___ exp.time_ 10 omega 44.00 88.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 114.0000 -30.0000 -180.0000 44'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.2000319000
_diffrn_orient_matrix_UB_12      0.0115159000
_diffrn_orient_matrix_UB_13      -0.0886998000
_diffrn_orient_matrix_UB_21      -0.0276983000
_diffrn_orient_matrix_UB_22      -0.0731508000
_diffrn_orient_matrix_UB_23      -0.0231984000
_diffrn_orient_matrix_UB_31      -0.0655333000
_diffrn_orient_matrix_UB_32      -0.0044227000
_diffrn_orient_matrix_UB_33      0.1526429000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0205
_diffrn_reflns_av_unetI/netI     0.0267
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            5234
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.224
_diffrn_reflns_theta_min         4.259
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.785
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63331
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_description       plate
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.252
_refine_diff_density_min         -0.193
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         2775
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0423
_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^)+(0.0646P)^2^+0.3462P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1195
_refine_ls_wR_factor_ref         0.1252
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2433
_reflns_number_total             2775
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce00891d2.cif
_cod_data_source_block           hk1
_cod_depositor_comments
'Adding full bibliography for 7231205--7231207.cif.'
_cod_database_code               7231205
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C20 H20 N" O2'
_reflns_odcompleteness_completeness 99.07
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.08
_olex2_refinement_description
;
Hydrogen H15 was located on the carboxylate of the terephthalate asymmetric unit but was placed at a 
calculate position for the refinement.
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C18(H18), C19(H19)
2.b Idealised tetrahedral OH refined as rotating group:
 O15(H15)
;
_shelx_res_checksum              27755
_olex2_submission_special_instructions 'No special instructions were received'