Pillared Two-Dimensional Metal–Organic Frameworks Based on a Lower-Rim Acid Appended Calix[4]arene
Redshaw, Carl; Rowe, Oliver; Elsegood, Mark R. J.; Horsburgh, Lynne; Teat, Simon J.; Crystal Growth & Design 14 (2014) 270–; doi:10.1021/cg4014703

data_4510023
_publ_section_title
;
 Pillared Two-Dimensional Metal--Organic Frameworks Based on a Lower-Rim
 Acid Appended Calix[4]arene
;
_journal_issue                   1
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              270
_journal_paper_doi               10.1021/cg4014703
_journal_volume                  14
_journal_year                    2014
_chemical_formula_moiety         'C108 H126 N2 O16 Zn2, C5 H11 N O'
_chemical_formula_sum            'C113 H137 N3 O17 Zn2'
_chemical_formula_weight         1939.99
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                103.240(16)
_cell_angle_beta                 95.592(14)
_cell_angle_gamma                91.319(17)
_cell_formula_units_Z            1
_cell_length_a                   10.539(8)
_cell_length_b                   12.738(10)
_cell_length_c                   23.029(19)
_cell_measurement_reflns_used    7362
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.3
_cell_measurement_theta_min      2.9
_cell_volume                     2992(4)
_computing_cell_refinement
;
CrystalClear-SM Expert 3.1 b21 (Rigaku, 20112)
;
_computing_data_collection
;
CrystalClear-SM Expert 3.1 b21 (Rigaku, 20112)
;
_computing_data_reduction
;
CrystalClear-SM Expert 3.1 b21 (Rigaku, 20112)
;
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0695
_diffrn_reflns_av_unetI/netI     0.0796
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            32328
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.269
_diffrn_reflns_theta_min         2.728
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    0.458
_exptl_absorpt_correction_T_max  0.725
_exptl_absorpt_correction_T_min  0.948
_exptl_absorpt_correction_type   DTABSCOR
_exptl_absorpt_process_details   0.980
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.077
_exptl_crystal_description       block
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.118
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.045
_platon_squeeze_details
;
R1 before squeeze ca. 16% with poor point atom model for solvent.
Platon squeeze recovers 89 electrons in total in one large void
plus ca. 6 much smaller ones. The largest void has ca. 68 el.
DEF has 56 el, so just one of these in the large void.
The smaller voids are really too small to accommodate DEF or MeOH.
One DEF added to UNIT and 65 parameters added to L.S.
;
_refine_diff_density_max         1.325
_refine_diff_density_min         -0.902
_refine_diff_density_rms         0.117
_refine_ls_extinction_coef       0.009(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     747
_refine_ls_number_reflns         12975
_refine_ls_number_restraints     641
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1431
_refine_ls_R_factor_gt           0.1246
_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^)+(0.1706P)^2^+7.3299P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3338
_refine_ls_wR_factor_ref         0.3485
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10016
_reflns_number_total             12975
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg4014703_si_002.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '_iucr_refine_instruction_details' was replaced with
'_iucr_refine_instructions_details' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
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_cod_database_code               4510023
_shelx_estimated_absorpt_t_min   0.948
_shelx_estimated_absorpt_t_max   0.980
_shelxl_version_number           2012-9