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_7229179
_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         '2( C28 H18 O2), 3( C3 H8 O1),  C1 Cl3 H1'
_chemical_formula_sum            'C66 H61 Cl3 O7'
_chemical_formula_weight         1072.50
_chemical_name_systematic
'bi 9,9?-(ethyne-1,2-diyl)-bis(fluoren-9-ol) bis (2-propanol) (chloroform) 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                83.94(3)
_cell_angle_beta                 82.70(3)
_cell_angle_gamma                89.93(3)
_cell_formula_units_Z            2
_cell_length_a                   9.6930(19)
_cell_length_b                   14.066(3)
_cell_length_c                   21.052(4)
_cell_measurement_reflns_used    68486
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      28.34
_cell_measurement_theta_min      1.46
_cell_volume                     2830.9(10)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0299
_diffrn_reflns_av_sigmaI/netI    0.0227
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            68486
_diffrn_reflns_theta_full        28.34
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    0.216
_exptl_absorpt_correction_T_max  0.9480
_exptl_absorpt_correction_T_min  0.9243
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.657
_refine_diff_density_min         -0.899
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     720
_refine_ls_number_reflns         14076
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0449
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0519P)^2^+1.3553P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1118
_refine_ls_wR_factor_ref         0.1198
_reflns_number_gt                11569
_reflns_number_total             14076
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7ce01414g3.cif
_cod_data_source_block           structure5
_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_cell_volume        2831.0(10)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7229179