Crystallisation Temperature Control of Stoichiometry and Selectivity in Host- Guest Compounds
Sykes, Nicole Margaret; Su, Hong; Weber, Edwin; Bourne, Susan A.; Nassimbeni, Luigi; CrystEngComm  (2017) –; doi:10.1039/C7CE01414G

data_7229180
_publ_section_title
;
 Crystallisation Temperature Control of Stoichiometry and Selectivity in
 Host- Guest Compounds
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE01414G
_journal_year                    2017
_chemical_formula_moiety         '3 (C28 H18 O2), 4 (C3 H8 O1) '
_chemical_formula_sum            'C96 H86 O10'
_chemical_formula_weight         1399.65
_chemical_name_systematic
'tri 9,9?-(ethyne-1,2-diyl)-bis(fluoren-9-ol) tetra (2-propanol) Clathrate'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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-97
_audit_update_record
;
2017-06-23 deposited with the CCDC.
2017-09-18 downloaded from the CCDC.
;
_cell_angle_alpha                104.29(3)
_cell_angle_beta                 94.58(3)
_cell_angle_gamma                96.70(3)
_cell_formula_units_Z            1
_cell_length_a                   10.150(2)
_cell_length_b                   10.397(2)
_cell_length_c                   18.780(4)
_cell_measurement_reflns_used    34826
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.97
_cell_measurement_theta_min      2.03
_cell_volume                     1895.2(7)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT-Plus and XPREP (Bruker 2004)'
_computing_molecular_graphics    'X-seed (Barbour, 1999)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Kappa Duo Apex II diffractometer'
_diffrn_measurement_method       '1.2\% \f scans and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0290
_diffrn_reflns_av_sigmaI/netI    0.0266
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            34821
_diffrn_reflns_theta_full        27.97
_diffrn_reflns_theta_max         27.97
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_T_max  0.9694
_exptl_absorpt_correction_T_min  0.9568
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             742
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.306
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     562
_refine_ls_number_reflns         9087
_refine_ls_number_restraints     200
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0463
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0525P)^2^+0.6055P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1124
_refine_ls_wR_factor_ref         0.1223
_reflns_number_gt                7143
_reflns_number_total             9087
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7ce01414g3.cif
_cod_data_source_block           structure6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/home/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 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7229180