Styrene Purification by Guest-Induced Restructuring of Pillar[6]arene.
Jie, Kecheng; Liu, Ming; Zhou, Yujuan; Little, Marc A.; Bonakala, Satyanarayana; Chong, Samantha Y.; Stephenson, Andrew; Chen, Linjiang; Huang, Feihe; Cooper, Andrew I.; Journal of the American Chemical Society 139 (2017) 2908–2911; doi:10.1021/jacs.6b13300

data_4125656
_publ_section_title
;
 Styrene Purification by Guest-Induced Restructuring of Pillar[6]arene.
;
_journal_issue                   8
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2908
_journal_page_last               2911
_journal_paper_doi               10.1021/jacs.6b13300
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'C66 H84 O12, 3(C3 H6 O)'
_chemical_formula_sum            'C75 H102 O15'
_chemical_formula_weight         1243.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-06-01
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 114.1459(17)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.5845(8)
_cell_length_b                   22.7005(16)
_cell_length_c                   14.5054(10)
_cell_measurement_reflns_used    6569
_cell_measurement_temperature    240
_cell_measurement_theta_max      22.366
_cell_measurement_theta_min      2.550
_cell_volume                     3781.3(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      240.0
_diffrn_detector_area_resol_mean 10.42
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0517
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            40660
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        23.250
_diffrn_reflns_theta_max         23.256
_diffrn_reflns_theta_min         0.897
_diffrn_source
;
Advanced Light Source, station 11.3.1
;
_exptl_absorpt_coefficient_mu    0.075
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8186
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0905 before and 0.0680 after correction.
The Ratio of minimum to maximum transmission is 0.8186.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.092
_exptl_crystal_description       block
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.122
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.042
_refine_diff_density_max         0.126
_refine_diff_density_min         -0.136
_refine_diff_density_rms         0.027
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         5429
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0498
_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^)+(0.0679P)^2^+0.4093P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1298
_refine_ls_wR_factor_ref         0.1436
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3568
_reflns_number_total             5429
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b13300_si_004.cif
_cod_data_source_block           pillar_6_arene_acetone_240k
_cod_database_code               4125656
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H1A(0.5) H1B(0.5) H22A(0.5) H22B(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C8(H8A,H8B), C15(H15A,H15B), C22(H22A,H22B), C24(H24A,H24B),
 C25(H25A,H25B), C27(H27A,H27B), C29(H29A,H29B), C31(H31A,H31B), C33(H33A,H33B)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C11(H11), C14(H14), C18(H18), C21(H21)
3.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C30(H30A,H30B,
 H30C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C)
;
_chemw03_alert_2_a
;
Problem:  ALERT: The ratio of given/expected molecular weight as
calculated from the _atom_site* data lies outside
the range 0.90 <> 1.10
From the CIF: _cell_formula_units_Z 2
From the CIF: _chemical_formula_weight 1243.56
TEST: Calculate formula weight from _atom_site_*
atom mass num sum
C 12.01 66.00 792.73
H 1.01 84.00 84.67
O 16.00 12.00 191.99
Response: Solvent content in the large 1-D voids was extremely diffuse 
and could not be modelled accurately. As a result, the SQUEEZE routine in
Platon was used during the final refinement cycles. 
The crystallisation solvent was acetone and therefore acetone molecules 
were added to the unit cell atom count to correct
for the disordered electron count masked by SQUEEZE.   
;
_plat043_alert_1_a
;
Problem:  Calculated and Reported Mol. Weight Differ by .. 174.23 Check
Response: Solvent content in the large 1-D voids was extremely diffuse 
and could not be modelled accurately. As a result, the SQUEEZE routine in
Platon was used during the final refinement cycles. 
The crystallisation solvent was acetone and therefore acetone molecules 
were added to the unit cell atom count to correct
for the disordered electron count masked by SQUEEZE.   
;
_plat602_alert_2_a
;
Problem:  VERY LARGE Solvent Accessible VOID(S) in Structure ! Info
Response: Solvent content in the large 1-D voids was extremely diffuse 
and could not be modelled accurately. As a result, the SQUEEZE routine in
Platon was used during the final refinement cycles. 
The crystallisation solvent was acetone and therefore acetone molecules 
were added to the unit cell atom count to correct
for the disordered electron count masked by SQUEEZE.   
;
_plat049_alert_1_b
;
Problem:  Calculated Density less than 1.0 gcm-3 ......... 0.9392 Check
Response: Solvent content in the large 1-D voids was extremely diffuse 
and could not be modelled accurately. As a result, the SQUEEZE routine in
Platon was used during the final refinement cycles. 
The crystallisation solvent was acetone and therefore acetone molecules 
were added to the unit cell atom count to correct
for the disordered electron count masked by SQUEEZE. The calculated density
is incorrect as it does not take into account the acetone molecules.
;
_shelx_res_checksum              41525
_shelx_hkl_checksum              21045
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'