Bicyclo[2.2.2]octane-1,4-dicarboxylic acid: Towards Transparent Metal-Organic Frameworks.
Llabres, Pedro; Pitarch-Jarque, Javier; Ballesteros-Garrido, Rafael; Abarca, Belén; Ballesteros, Rafael; García-España, Enrique; Dalton Trans.  (2017) –; doi:10.1039/C7DT00855D

data_7042994
_publ_section_title
;
 Bicyclo[2.2.2]octane-1,4-dicarboxylic acid: Towards Transparent
 Metal-Organic Frameworks.
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT00855D
_journal_year                    2017
_chemical_formula_moiety         '0.25(C40 H48 O16 Zn4), 0.75(O)'
_chemical_formula_sum            'C10 H13.5 O4.75 Zn'
_chemical_formula_weight         275.08
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-04-21
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-04-21 deposited with the CCDC.
2017-05-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.798(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.1355(4)
_cell_length_b                   13.0213(7)
_cell_length_c                   14.8255(7)
_cell_measurement_reflns_used    1366
_cell_measurement_temperature    119.90(14)
_cell_measurement_theta_max      28.6150
_cell_measurement_theta_min      3.6410
_cell_volume                     1183.86(11)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41q (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 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      119.90(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.996
_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    -25.00  15.00   1.00   10.00    --  -19.63  38.00  90.00   40
  2  \w    -51.00  29.00   1.00   10.00    --   20.88 -38.00-120.00   80
  3  \w    -82.00 -35.00   1.00   10.00    --  -19.63-178.00  90.00   47
  4  \w    -95.00 -40.00   1.00   10.00    --  -19.63 178.00  30.00   55
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0372378000
_diffrn_orient_matrix_UB_12      -0.0257790000
_diffrn_orient_matrix_UB_13      -0.0397326000
_diffrn_orient_matrix_UB_21      0.0303869000
_diffrn_orient_matrix_UB_22      0.0428874000
_diffrn_orient_matrix_UB_23      -0.0262750000
_diffrn_orient_matrix_UB_31      0.1052047000
_diffrn_orient_matrix_UB_32      -0.0215166000
_diffrn_orient_matrix_UB_33      -0.0047581000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_unetI/netI     0.0647
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            2838
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         3.672
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.074
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31976
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41q (Rigaku Oxford Diffraction, 2015)
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    1.543
_exptl_crystal_description       block
_exptl_crystal_F_000             566
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.932
_refine_diff_density_min         -0.555
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         1166
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0385
_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^)+(0.0502P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0925
_refine_ls_wR_factor_ref         0.0975
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1055
_reflns_number_total             1166
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00855d2.cif
_cod_data_source_block           tmof3
_cod_original_cell_volume        1183.86(12)
_cod_original_formula_sum        'C10 H13.50 O4.75 Zn'
_cod_database_code               7042994
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C3) \\sim Ueq: with sigma of 0.008 and sigma for terminal atoms of 0.01
3. Others
 Fixed Sof: C3(0.5) H3A(0.5) H3B(0.5) C4(0.5) H4A(0.5) H4B(0.5) C5(0.5)
 H5A(0.5) H5B(0.5) C6(0.5) H6A(0.5) H6B(0.5) C7(0.5) H7A(0.5) H7B(0.5) C8(0.5)
 H8A(0.5) H8B(0.5) O4S(0.125) O3S(0.25)
4.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B)
;
_shelx_shelxl_version_number     2014/7
_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 1.891
_oxdiff_exptl_absorpt_empirical_full_min 0.540