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_7042995
_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         'C40 H48 O16 Zn4'
_chemical_formula_sum            'C46 H62 N2 O18 Zn4'
_chemical_formula_weight         1192.45
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-05-07
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-05-07 deposited with the CCDC.
2017-05-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.675(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.1210(2)
_cell_length_b                   19.5910(9)
_cell_length_c                   19.6970(7)
_cell_measurement_reflns_used    914
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.910
_cell_volume                     2361.83(16)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      120(1)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            3902
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.322
_exptl_absorpt_coefficient_mu    2.086
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.677
_exptl_crystal_description       block
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.938
_refine_diff_density_min         -0.589
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         2076
_refine_ls_number_restraints     177
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0576
_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^)+(0.0983P)^2^+26.9843P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1671
_refine_ls_wR_factor_ref         0.1747
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1837
_reflns_number_total             2076
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00855d2.cif
_cod_data_source_block           pytmof
_cod_database_code               7042995
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.898(4) 0.102(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
3. 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
4. Others
 Fixed Sof: C2A(0.5) C2B(0.5) C3A(0.5) H3AA(0.5) H3AB(0.5) C3B(0.5) H3BA(0.5)
 H3BB(0.5) C4A(0.5) H4AA(0.5) H4AB(0.5) C4B(0.5) H4BA(0.5) H4BB(0.5) C5A(0.5)
 H5AA(0.5) H5AB(0.5) C5B(0.5) H5BA(0.5) H5BB(0.5) C8A(0.5) H8AA(0.5) H8AB(0.5)
 C8B(0.5) H8BB(0.5) H8BA(0.5) C9A(0.5) H9AA(0.5) H9AB(0.5) C9B(0.5) H9BA(0.5)
 H9BB(0.5) C10A(0.5) H10A(0.5) H10B(0.5) C10B(0.5) H10C(0.5) H10D(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C3A(H3AA,H3AB), C3B(H3BA,H3BB), C4A(H4AA,H4AB), C4B(H4BA,H4BB), C5A(H5AA,
 H5AB), C5B(H5BA,H5BB), C8A(H8AA,H8AB), C8B(H8BB,H8BA), C9A(H9AA,H9AB),
 C9B(H9BA,H9BB), C10A(H10A,H10B), C10B(H10C,H10D)
;
_shelx_fab_checksum              27627
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'