A crystalline sponge based on dispersive forces suitable for X-ray structure determination of included molecular guests
Sanna, Elena; Escudero-Adán, Eduardo C.; Bauzá, Antonio; Ballester, Pablo; Frontera, Antonio; Rotger, Carmen; Costa, Antonio; Chem. Sci. 6 (2015) 5466–; doi:10.1039/C5SC01838B

data_1529087
_publ_section_title
;
 A crystalline sponge based on dispersive forces suitable for X-ray
 structure determination of included molecular guests
;
_journal_issue                   10
_journal_name_full               'Chem. Sci.'
_journal_page_first              5466
_journal_paper_doi               10.1039/C5SC01838B
_journal_volume                  6
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_sum            'C70 H74 N6'
_chemical_formula_weight         999.34
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2015-05-07 deposited with the CCDC.
2015-07-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.562(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   35.689(4)
_cell_length_b                   5.9481(6)
_cell_length_c                   28.840(3)
_cell_measurement_temperature    100(2)
_cell_volume                     6069.0(11)
_computing_cell_refinement
'CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)'
_computing_data_collection
'CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)'
_computing_data_reduction
'CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    Sir2011
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  '1/4chi goniometer'
_diffrn_measurement_method
;
 Fullsphere data collection, phi and omega scans
;
_diffrn_measurement_specimen_support 'magnetic support with MicroMount'
_diffrn_radiation_monochromator  'Confocal Max Flux optic'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_unetI/netI     0.0453
_diffrn_reflns_Laue_measured_fraction_full 0.947
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            90524
_diffrn_reflns_point_group_measured_fraction_full 0.949
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.089
_diffrn_reflns_theta_min         7.907
_diffrn_source                   'Microfocus rotating anode X-ray tube'
_diffrn_source_current           24
_diffrn_source_power             50
_diffrn_source_size              '0.2 mm x 0.2 mm fine focus'
_diffrn_source_type              'Rigaku MicroMax-007HF'
_exptl_absorpt_coefficient_mu    0.064
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_correction_T_min  0.759
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.094
_exptl_crystal_description       Block
_exptl_crystal_F_000             2144
_exptl_crystal_recrystallization_method 'Immersion in S-Nicotin'
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.378
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details
;
 Flack x determined using 5575 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.4(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     793
_refine_ls_number_reflns         17187
_refine_ls_number_restraints     217
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0931
_refine_ls_R_factor_gt           0.0768
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1195P)^2^+7.0851P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2101
_refine_ls_wR_factor_ref         0.2312
_reflns_Friedel_coverage         0.828
_reflns_Friedel_fraction_full    0.952
_reflns_Friedel_fraction_max     0.955
_reflns_number_gt                14193
_reflns_number_total             17187
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc01838b2.cif
_cod_data_source_block           E66_Nico_C2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 1529078--1529087.cif.
;
_cod_original_sg_symbol_H-M      C2
_cod_database_code               1529087
_shelx_estimated_absorpt_t_min   0.987
_shelx_estimated_absorpt_t_max   0.987
_shelxl_version_number           2014/6
_shelx_res_checksum              63107
_shelx_hkl_checksum              46390