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_4510024
_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_absolute_configuration ad
_chemical_formula_moiety         'C116 H140 N8 O20 Zn2, C5 H11 N O'
_chemical_formula_sum            'C121 H151 N9 O21 Zn2'
_chemical_formula_weight         2198.24
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.249(3)
_cell_length_b                   10.0932(13)
_cell_length_c                   47.440(6)
_cell_measurement_temperature    100(2)
_cell_volume                     12569(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX II'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  'Bruker Apex 2 CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_unetI/netI     0.0622
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       66
_diffrn_reflns_limit_l_min       -66
_diffrn_reflns_number            104420
_diffrn_reflns_point_group_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.900
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         33.071
_diffrn_reflns_theta_min         2.744
_diffrn_source                   'ALS station 11.3.1'
_exptl_absorpt_coefficient_mu    0.561
_exptl_absorpt_correction_T_max  0.989
_exptl_absorpt_correction_T_min  0.859
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2008/1, Sheldrick, G.M., (2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_description       lath
_exptl_crystal_F_000             4672
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.020
_platon_squeeze_details
;
;
_refine_diff_density_max         3.996
_refine_diff_density_min         -0.817
_refine_diff_density_rms         0.120
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.481(13)
_refine_ls_extinction_coef       0.0049(4)
_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   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1331
_refine_ls_number_reflns         33131
_refine_ls_number_restraints     297
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0960
_refine_ls_R_factor_gt           0.0835
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1241P)^2^+23.1776P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2156
_refine_ls_wR_factor_ref         0.2235
_reflns_Friedel_coverage         0.910
_reflns_Friedel_fraction_full    0.948
_reflns_Friedel_fraction_max     0.867
_reflns_number_gt                27271
_reflns_number_total             33131
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg4014703_si_002.cif
_cod_data_source_block           3
_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               4510024
_shelx_estimated_absorpt_t_min   0.859
_shelx_estimated_absorpt_t_max   0.989
_shelxl_version_number           2012-6