Mixed-linker solid solutions of functionalized pillared-layer MOFs - adjusting structural flexibility, gas sorption, and thermal responsiveness.
Schwedler, Inke; Henke, Sebastian; Wharmby, Michael T.; Bajpe, Sneha R.; Cheetham, Anthony K.; Fischer, Roland A.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 4230–4241; doi:10.1039/c5dt03825a

data_7037055
_publ_section_title
;
 Mixed-linker solid solutions of functionalized pillared-layer MOFs -
 adjusting structural flexibility, gas sorption, and thermal
 responsiveness.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4230
_journal_page_last               4241
_journal_paper_doi               10.1039/c5dt03825a
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C21 H30 N O6 Zn'
_chemical_formula_sum            'C21 H30 N O6 Zn'
_chemical_formula_weight         457.83
_chemical_name_systematic        DPe-DMOF(Zn)
_space_group_crystal_system      tetragonal
_space_group_IT_number           126
_space_group_name_Hall           '-P 4a 2bc'
_space_group_name_H-M_alt        'P 4/n n c'
_symmetry_space_group_name_Hall  '-P 4a 2bc'
_symmetry_space_group_name_H-M   'P 4/n n c :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-09-24
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-09-24 deposited with the CCDC.
2015-10-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.43134(14)
_cell_length_b                   15.43134(14)
_cell_length_c                   19.2746(3)
_cell_measurement_reflns_used    5254
_cell_measurement_temperature    300(3)
_cell_measurement_theta_max      35.8440
_cell_measurement_theta_min      2.6420
_cell_volume                     4589.79(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      300(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1183
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -18.00   77.00   0.5000   11.2500
omega____ theta____ kappa____ phi______ frames
    -       -0.5469   77.0000  -60.0000 190

  2 omega    5.00   34.00   0.5000   11.2500
omega____ theta____ kappa____ phi______ frames
    -       -0.5469   77.0000 -180.0000 58

  3 omega   13.00  126.00   0.5000   22.5000
omega____ theta____ kappa____ phi______ frames
    -       45.5850   77.0000 -150.0000 226

  4 omega   80.00  114.00   0.5000   22.5000
omega____ theta____ kappa____ phi______ frames
    -       45.5850   77.0000  -60.0000 68

  5 omega   73.00  105.00   0.5000   22.5000
omega____ theta____ kappa____ phi______ frames
    -       45.5850   77.0000  120.0000 64

  6 omega  -60.00   34.00   0.5000   22.5000
omega____ theta____ kappa____ phi______ frames
    -      -46.6788   77.0000 -150.0000 188

  7 omega  -76.00  -51.00   0.5000   22.5000
omega____ theta____ kappa____ phi______ frames
    -      -46.6788   77.0000  120.0000 50

  8 omega  -74.00  -24.00   0.5000   22.5000
omega____ theta____ kappa____ phi______ frames
    -      -46.6788   77.0000  -60.0000 100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0048749000
_diffrn_orient_matrix_UB_12      -0.0141814000
_diffrn_orient_matrix_UB_13      0.0347838000
_diffrn_orient_matrix_UB_21      -0.0013890000
_diffrn_orient_matrix_UB_22      -0.0437236000
_diffrn_orient_matrix_UB_23      -0.0113024000
_diffrn_orient_matrix_UB_31      0.0456868000
_diffrn_orient_matrix_UB_32      0.0001977000
_diffrn_orient_matrix_UB_33      -0.0040427000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            25509
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.998
_diffrn_reflns_theta_min         2.113
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.104
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92777
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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    1.325
_exptl_crystal_description       prism
_exptl_crystal_F_000             1928
_exptl_crystal_recrystallization_method 'solvothermal reaction'
_exptl_crystal_size_max          0.3824
_exptl_crystal_size_mid          0.1986
_exptl_crystal_size_min          0.1555
_refine_diff_density_max         0.705
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         2788
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0850
_refine_ls_R_factor_gt           0.0585
_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^)+(0.0986P)^2^+7.1383P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1961
_refine_ls_wR_factor_ref         0.2213
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1604
_reflns_number_total             2788
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03825a2.cif
_cod_data_source_block           added_by_encifer
_cod_depositor_comments          'Adding full bibliography for 7037055.cif.'
_cod_original_cell_volume        4589.80(10)
_cod_database_code               7037055
_chemical_oxdiff_formula         'C21 H30 N O6 Zn'
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.23
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O3-C5A = O3-C5B
 1.36 with sigma of 0.01
 C6-C5A = C6-C5B = C7-C6 = C8-C7 = C8-C9
 1.54 with sigma of 0.01
 C7-C9
 2.6 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C12) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C13)
\\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15) \\sim Ueq: with sigma of 0.02 and
sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: C5A(0.5) H5AA(0.5) H5AB(0.5) C5B(0.5) H5BA(0.5) H5BB(0.5)
 H6AA(0.5) H6AB(0.5) H6BC(0.5) H6BD(0.5) C10(0.25) C11(0.25) C12(0.25)
 C13(0.25) C14(0.25) C15(0.25)
5.a Secondary CH2 refined with riding coordinates:
 C5A(H5AA,H5AB), C5B(H5BA,H5BB), C6(H6AA,H6AB), C6(H6BC,H6BD), C7(H7A,H7B),
 C8(H8A,H8B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3)
5.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'