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_7042997
_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         '0.5(C80 H96 O32 Zn8), 2(C3 H7 N O)'
_chemical_formula_sum            'C46 H62 N2 O18 Zn4'
_chemical_formula_weight         1192.45
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-05-06
_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                 90.564(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.1341(4)
_cell_length_b                   19.5931(11)
_cell_length_c                   19.6981(13)
_cell_measurement_reflns_used    2735
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      29.6730
_cell_measurement_theta_min      3.2610
_cell_volume                     2367.3(3)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_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 0.996
_diffrn_measurement_details
;
  1 omega  -25.00   93.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       20.8840    0.0000   30.0000 118

  2 omega  -67.00  -21.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.6340  120.0000   43.0000 46

  3 omega  -87.00  -61.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.6340 -178.0000 -120.0000 26

  4 omega  -95.00  -66.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.6340 -178.0000   30.0000 29
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0139703000
_diffrn_orient_matrix_UB_12      0.0016079000
_diffrn_orient_matrix_UB_13      -0.0357774000
_diffrn_orient_matrix_UB_21      -0.0251792000
_diffrn_orient_matrix_UB_22      -0.0353233000
_diffrn_orient_matrix_UB_23      -0.0007286000
_diffrn_orient_matrix_UB_31      -0.1119376000
_diffrn_orient_matrix_UB_32      0.0076975000
_diffrn_orient_matrix_UB_33      0.0042901000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0700
_diffrn_reflns_av_unetI/netI     0.0746
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            8680
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.103
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.081
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65606
_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.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.673
_exptl_crystal_description       block
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.898
_refine_diff_density_min         -0.897
_refine_diff_density_rms         0.146
_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     416
_refine_ls_number_reflns         4127
_refine_ls_number_restraints     313
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0945
_refine_ls_R_factor_gt           0.0753
_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^)+(0.1051P)^2^+6.7870P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1989
_refine_ls_wR_factor_ref         0.2227
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3006
_reflns_number_total             4127
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00855d2.cif
_cod_data_source_block           tmof
_cod_database_code               7042997
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.866(3) 0.134(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N2S-C21S_$1 \\sim N2S-C21S
 with sigma of 0.02
 N2S-C23S \\sim N2S-C21S
 with sigma of 0.02
 N1S-C13S \\sim N1S-C12S
 with sigma of 0.02
4. 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
5. Others
 Fixed Sof: C14(0.5) H14a(0.5) H14b(0.5) C15(0.5) H15a(0.5) H15b(0.5) C26(0.5)
 H26a(0.5) H26b(0.5) C17(0.5) H17a(0.5) H17b(0.5) C21(0.5) H21a(0.5) H21b(0.5)
 C16(0.5) H16a(0.5) H16b(0.5) C23(0.5) H23a(0.5) H23b(0.5) C25(0.5) H25a(0.5)
 H25b(0.5) C24(0.5) H24a(0.5) H24b(0.5) C18(0.5) H18a(0.5) H18b(0.5) C13(0.5)
 H13a(0.5) H13b(0.5) N2S(0.5) C21S(0.5) H21c(0.5) H21d(0.5) H21e(0.5) C22S(0.5)
 H22S(0.5) O2S(0.5) C11S(0.5) H11S(0.5) O1S(0.5) C12S(0.5) H12a(0.5) H12b(0.5)
 H12c(0.5) C22(0.5) H22a(0.5) H22b(0.5) C13S(0.5) H13c(0.5) H13d(0.5) H13e(0.5)
 C23S(0.5) H23c(0.5) H23d(0.5) H23e(0.5) N1S(0.5)
6.a Riding coordinates:
 C4(H4a,H4b), C7(H7a,H7b), C5(H5a,H5b), C8(H8a,H8b), C14(H14a,H14b), C15(H15a,
 H15b), C6(H6a,H6b), C26(H26a,H26b), C17(H17a,H17b), C21(H21a,H21b), C16(H16a,
 H16b), C3(H3a,H3b), C23(H23a,H23b), C25(H25a,H25b), C24(H24a,H24b), C18(H18a,
 H18b), C13(H13a,H13b), C22(H22a,H22b)
6.b Me refined with riding coordinates:
 C21S(H21c,H21d,H21e), C12S(H12a,H12b,H12c), C13S(H13c,H13d,H13e), C23S(H23c,
 H23d,H23e)
6.c Aromatic/amide H refined with riding coordinates:
 C22S(H22S), C11S(H11S)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'