Formation of a robust, double-walled LiMOF from an L-shaped di-substituted N-heterocyclic adamantane-based ligand.
Houlihan, Joanna C. C.; Moratti, Stephen C.; Hanton, Lyall R.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 12009–12017; doi:10.1039/d0dt02437f

data_7705124
_publ_section_title
;
 Formation of a robust, double-walled LiMOF from an L-shaped
 di-substituted N-heterocyclic adamantane-based ligand.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12009
_journal_page_last               12017
_journal_paper_doi               10.1039/d0dt02437f
_journal_volume                  49
_journal_year                    2020
_chemical_formula_sum            'C44 H40 Li4 N4 O12.5'
_chemical_formula_weight         852.56
_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   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-08-03 deposited with the CCDC.	2020-08-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.4030(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.5163(4)
_cell_length_b                   32.0310(3)
_cell_length_c                   12.8356(2)
_cell_measurement_reflns_used    21837
_cell_measurement_temperature    100.01(15)
_cell_measurement_theta_max      72.3230
_cell_measurement_theta_min      4.0340
_cell_volume                     14102.4(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.01(15)
_diffrn_detector_area_resol_mean 10.3449
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_av_unetI/netI     0.0455
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            50481
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.998
_diffrn_reflns_theta_min         3.776
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.482
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83542
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.803
_exptl_crystal_description       needle
_exptl_crystal_F_000             3552
_platon_squeeze_details
;
The SQUEEZE routine of PLATON was applied to remove any unbound DEF molecules within the channels of the framework.
The total void volume is 6434 angstrom and the total electron count within the unit cell is 1319.
There is therefore 168.1 electrons per asymmetric unit (Z = 8, 1319/8 = 164.9).
The electron count attributed to approximately 3 DEF molecules within the asymmetric unit (164.9/56 = 2.94)
and approximately 1.5 DEF molecules per L1 ligand (2.94/2 = 1.47).
;
_refine_diff_density_max         1.013
_refine_diff_density_min         -0.833
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     656
_refine_ls_number_reflns         13120
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.1128
_refine_ls_R_factor_gt           0.0887
_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^)+(0.1314P)^2^+35.7642P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2501
_refine_ls_wR_factor_ref         0.2707
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10244
_reflns_number_total             13120
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02437f2.cif
_cod_data_source_block           LiMOF12
_cod_depositor_comments
'Adding full bibliography for 7705120--7705129.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C44 H40 Li4 N4 O12.50'
_cod_database_code               7705124
_shelx_shelxl_version_number     2018/3
_exptl_absorpt_special_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              11013
_shelx_fab_checksum              18984
_platon_squeeze_void_probe_radius 1.20