Cubane-forming cyclic dienes that exhibit orthogonal reactivities in the solid state.
Li, Changan; Sinnwell, Michael A.; Swenson, Dale C.; MacGillivray, Leonard R.; Chemical communications (Cambridge, England) 57 (2021) 6725–6727; doi:10.1039/d1cc02725e

data_7128450
_publ_section_title
;
 Cubane-forming cyclic dienes that exhibit orthogonal reactivities in the
 solid state.
;
_journal_issue                   55
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              6725
_journal_page_last               6727
_journal_paper_doi               10.1039/d1cc02725e
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C14.61 H13.22 O14, 4(H2 O), 2(H1.7 O0.7)'
_chemical_formula_sum            'C14.61 H24.61 O19.39'
_chemical_formula_weight         510.51
_chemical_name_common            'tetraacid cage CG1'
_chemical_name_systematic
'6,6,12,12-tetrahydroxy-3,9-dioxapentacyclo[6.4.0.0^2,7.0^4,11.0^5,10]dodecane-2,4,8,10-tetracarboxylic acid hydrate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-04-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-05-08 deposited with the CCDC.	2021-06-07 downloaded from the CCDC.
;
_cell_angle_alpha                82.568(7)
_cell_angle_beta                 82.756(8)
_cell_angle_gamma                65.804(6)
_cell_formula_units_Z            1
_cell_length_a                   7.7763(19)
_cell_length_b                   8.1868(17)
_cell_length_c                   8.683(2)
_cell_measurement_reflns_used    9198
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.92
_cell_measurement_theta_min      2.3725
_cell_volume                     498.4(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker D8 Venture Duo'
_diffrn_measurement_method       'CCD phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0767
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1743
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.020
_diffrn_reflns_theta_max         25.020
_diffrn_reflns_theta_min         2.373
_exptl_absorpt_coefficient_mu    0.163
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8822
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1218 before and 0.0527 after correction.
The Ratio of minimum to maximum transmission is 0.8822.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.701
_exptl_crystal_description       plates
_exptl_crystal_F_000             267
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: MeOH/benzene'
_exptl_crystal_size_max          0.105
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   1.0000
_exptl_transmission_factor_min   0.8822
_refine_diff_density_max         0.341
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         1743
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.1004
_refine_ls_R_factor_gt           0.0605
_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^)+1.2197P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1220
_refine_ls_wR_factor_ref         0.1424
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1220
_reflns_number_total             1743
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc02725e2.cif
_cod_data_source_block           mcg2151_5
_cod_depositor_comments
'Adding full bibliography for 7128449--7128452.cif.'
_cod_database_code               7128450
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.997
_shelx_estimated_absorpt_t_min   0.983
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.786(3)
 0.214(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
3. Shared sites
{O2, O2'}
4. Restrained distances
 O1A-H1AA
 0.84 with sigma of 0.02
5. Uiso/Uaniso restraints and constraints
Uanis(O2) = Uanis(O2')
6. Others
 Sof(O2')=Sof(C1')=Sof(H1'A)=Sof(H1'B)=Sof(H1'C)=1-FVAR(1)
 Sof(O2)=Sof(H2)=Sof(O1A)=Sof(H1AA)=FVAR(1)
7.a Free rotating group:
 O3A(H3AA,H3AB), O2A(H2AA,H2AB)
7.b Ternary CH refined with riding coordinates:
 C3(H3), C5(H5A)
7.c Me refined with riding coordinates:
 C1'(H1'A,H1'B,H1'C)
7.d Idealised tetrahedral OH refined as rotating group:
 O4(H4), O7(H7), O2(H2)
;
_shelx_res_checksum              72275
_olex2_submission_special_instructions 'No special instructions were received'