Metal-Organic Frameworks with Hexakis(4-carboxyphenyl)benzene - Extensions to Reticular Chemistry and Introducing Foldable Nets.
Amombo Noa, Francoise M.; Svensson Grape, Erik; Brülls, Steffen M; Cheung, Ocean; Malmberg, Per; Inge, A. Ken; McKenzie, Christine J.; Mårtensson, Jerker; Ohrstrom, Lars; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c02984

data_4134893
_publ_section_title
;
 Metal-Organic Frameworks with Hexakis(4-carboxyphenyl)benzene -
 Extensions to Reticular Chemistry and Introducing Foldable Nets.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c02984
_journal_year                    2020
_chemical_formula_moiety         'C48 H28 O14 Zn2, C4 H16 N2'
_chemical_formula_sum            'C52 H44 N2 O14 Zn2'
_chemical_formula_weight         1051.63
_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   mixed
_audit_creation_date             2020-03-17
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959)
;
_cell_angle_alpha                90
_cell_angle_beta                 99.919(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.1139(9)
_cell_length_b                   16.3925(5)
_cell_length_c                   11.4361(3)
_cell_measurement_reflns_used    6591
_cell_measurement_temperature    100.01(17)
_cell_measurement_theta_max      66.8970
_cell_measurement_theta_min      4.7760
_cell_volume                     5376.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(17)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_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    -26.00  57.00   0.50    5.00    --  -24.19  19.00  30.00  166
  2  \w    -26.00  57.00   0.50    5.00    --  -24.19  19.00 -90.00  166
  3  \w    -23.00  14.00   0.50   15.00    --  -68.97  12.00-150.00   74
  4  \w    -22.00   7.00   0.50   15.00    --  -68.97  12.00-180.00   58
  5  \w    -27.00   0.00   0.50   15.00    --  -68.97  25.00-120.00   54
  6  \w    -28.00  14.00   0.50   15.00    --  -68.97  25.00 -60.00   84
  7  \w    -22.00  13.00   0.50   15.00    --  -68.97  12.00 -90.00   70
  8  \w    -24.00  14.00   0.50   15.00    --  -68.97  12.00   0.00   76
  9  \w    -15.00  14.00   0.50   15.00    --  -68.97  50.00  30.00   58
 10  \w    -24.00  14.00   0.50   15.00    --  -68.97  12.00  90.00   76
 11  \w    -18.00   8.00   0.50   15.00    --  -68.97  12.00  30.00   52
 12  \w    -42.00  57.00   0.50    5.00    --  -24.19  37.00 120.00  198
 13  \w      3.00  29.00   0.50   15.00    --   68.97  96.00 -38.38   52
 14  \w      8.00  39.00   0.50   15.00    --   68.97  86.00 -94.68   62
 15  \w      8.00  42.00   0.50   15.00    --   68.97  87.00-137.31   68
 16  \w      0.00 175.00   0.50   45.00    --  113.75  11.00 -30.00  350
 17  \w    113.00 175.00   0.50   45.00    --  113.75  11.00-150.00  124
 18  \w    103.00 150.00   0.50   15.00    --   68.97 111.00-180.00   94
 19  \w    131.00 178.00   0.50   45.00    --  113.75 104.00   0.00   94
 20  \w    107.00 149.00   0.50   15.00    --   68.97 111.00 120.00   84
 21  \w      6.00  42.00   0.50   15.00    --   68.97  91.00 139.80   72
 22  \w      8.00  62.00   0.50   45.00    --  113.75 -54.00   0.00  108
 23  \w     24.00 108.00   0.50   15.00    --   68.97-111.00   0.00  168
 24  \w     26.00 107.00   0.50   45.00    --  113.75-104.00 -60.00  162
 25  \w     67.00 101.00   0.50   45.00    --  113.75-104.00-180.00   68
 26  \w     21.00  61.00   0.50   45.00    --  113.75-104.00-180.00   80
 27  \w     18.00 105.00   0.50   45.00    --  113.75-104.00-150.00  174
 28  \w     12.00  48.00   0.50   45.00    --  113.75 -43.00 -30.00   72
 29  \w     12.00 105.00   0.50   45.00    --  113.75 -89.00 -60.00  186
 30  \w     24.00 107.00   0.50   45.00    --  113.75-104.00  90.00  166
 31  \w      9.00  93.00   0.50   45.00    --  113.75 -89.00  90.00  168
 32  \w      2.00 104.00   0.50   45.00    --  113.75 -77.00 -30.00  204
 33  \w     18.00 107.00   0.50   45.00    --  113.75-104.00-120.00  178
 34  \w      8.00  55.00   0.50   45.00    --  113.75 -54.00-150.00   94
 35  \w     -1.00 105.00   0.50   45.00    --  113.75  11.00-150.00  212
 36  \w      7.00  61.00   0.50   45.00    --  113.75 -54.00  90.00  108
 37  \w      3.00  78.00   0.50   45.00    --  113.75 -65.00 120.00  150
 38  \w      1.00  37.00   0.50    5.00    --  -24.19 -99.00 150.00   72
 39  \w    -57.00 -28.00   0.50   15.00    --  -68.97  50.00  30.00   58
 40  \w    -57.00  14.00   0.50   15.00    --  -68.97  50.00 -60.00  142
 41  \w    -74.00   2.00   0.50   15.00    --  -68.97  63.00-150.00  152
 42  \w    -95.00 -27.00   0.50   45.00    -- -106.00 138.00 -30.00  136
 43  \w    -41.00  14.00   0.50   15.00    --  -68.97  37.00 120.00  110
 44  \w    -42.00  10.00   0.50   15.00    --  -68.97  37.00 150.00  104
 45  \w    -90.00 -39.00   0.50    5.00    --   24.19 178.00 120.00  102
 46  \w   -175.00 -79.00   0.50   45.00    -- -106.00 -89.00-150.00  192
 47  \w   -132.00 -86.00   0.50    5.00    --  -24.19 -99.00   0.00   92
 48  \w      7.00  33.00   0.50   45.00    --  113.75  34.00  -4.00   52
 49  \w   -113.00 -87.00   0.50    5.00    --  -24.19 -99.00-150.00   52
 50  \w   -118.00 -92.00   0.50    5.00    --  -24.19 -99.00 120.00   52
 51  \w    -24.00   1.00   0.50   15.00    --  -68.97  12.00-120.00   50
 52  \w    -23.00   3.00   0.50   15.00    --  -68.97  12.00 -30.00   52
 53  \w    -78.00 -53.00   0.50   45.00    -- -106.00  65.00-180.00   50
 54  \w    137.00 163.00   0.50   45.00    --  113.75 104.00-120.00   52
 55  \w     71.00 111.00   0.50   45.00    --  113.75  34.00  -4.00   80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0536029000
_diffrn_orient_matrix_UB_12      0.0050425000
_diffrn_orient_matrix_UB_13      0.0184972000
_diffrn_orient_matrix_UB_21      0.0030822000
_diffrn_orient_matrix_UB_22      -0.0407683000
_diffrn_orient_matrix_UB_23      0.1224677000
_diffrn_orient_matrix_UB_31      0.0017677000
_diffrn_orient_matrix_UB_32      -0.0845341000
_diffrn_orient_matrix_UB_33      -0.0579367000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0118
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            17681
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.106
_diffrn_reflns_theta_max         67.106
_diffrn_reflns_theta_min         3.082
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.628
_exptl_absorpt_correction_T_max  0.909
_exptl_absorpt_correction_T_min  0.776
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.71a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
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    1.299
_exptl_crystal_description       block
_exptl_crystal_F_000             2168
_exptl_crystal_size_max          0.147
_exptl_crystal_size_mid          0.057
_exptl_crystal_size_min          0.048
_refine_diff_density_max         0.843
_refine_diff_density_min         -0.698
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.144
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         17681
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0463
_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^)+(0.0800P)^2^+7.5160P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1532
_refine_ls_wR_factor_ref         0.1560
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16719
_reflns_number_total             17681
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.9847\% 
 around [-0.71 0.71 0.00] (reciprocal) or [-0.31 0.94 -0.13] (direct)
Component 3 rotated by 179.9917\% 
 around [0.95 0.32 0.00] (reciprocal) or [0.67 0.69 0.29] (direct)
Component 4 rotated by 59.4855\% 
 around [0.40 -0.00 -0.92] (reciprocal) or [0.00 -0.00 -1.00] (direct)
;
_cod_data_source_file            ja0c02984_si_007.cif
_cod_data_source_block           zn-complex_twin1_hklf4_sq
_cod_database_code               4134893
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C212  H160  O56  Zn8  '
_chemical_oxdiff_usercomment     hemisphere
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.200(2)
 0.2468(11) 0.3868(14) 0.1665(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(H4BC)=Sof(H4BD)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=1-FVAR(1)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(H4AA)=Sof(H4AB)=FVAR(1)
 Sof(O00J)=1-FVAR(2)
 Sof(O00K)=FVAR(2)
5.a Free rotating group:
 O002(H00A,H00B)
5.b Secondary CH2 refined with riding coordinates:
 N4(H4AA,H4AB), N4(H4BC,H4BD)
5.c Me refined with riding coordinates:
 C2(H2A,H2B,H2C)
5.d Aromatic/amide H refined with riding coordinates:
 C008(H008), C00A(H00C), C00D(H00D), C00F(H00F), C00I(H00I), C00K(H00K),
 C00N(H00N), C00O(H00O), C00P(H00P), C00Q(H00Q), C00R(H00R), C00T(H00T)
5.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C1A(H1AA,H1AB,H1AC)
;
_shelx_res_checksum              85440
_shelx_hkl_checksum              21225
_shelx_fab_checksum              96995
_platon_squeeze_void_probe_radius 1.20
_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 1.465
_oxdiff_exptl_absorpt_empirical_full_min 0.759
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               4