Thermoresponsive Organic Inclusion Compounds: Modification of Thermal Expansion Behavior by Simple Guest Replacement
Engel, Emile R.; Smith, Vincent J.; Bezuidenhout, Charl X.; Barbour, Leonard J.; Chemistry of Materials 28 (2016) 5073–; doi:10.1021/acs.chemmater.6b01916

data_4003267
_publ_section_title
;
 Thermoresponsive Organic Inclusion Compounds: Modification of Thermal
 Expansion Behavior by Simple Guest Replacement
;
_journal_issue                   14
_journal_name_full               'Chemistry of Materials'
_journal_page_first              5073
_journal_paper_doi               10.1021/acs.chemmater.6b01916
_journal_volume                  28
_journal_year                    2016
_chemical_formula_moiety         'C12 H24 O6, 2(C2 H3 N)'
_chemical_formula_sum            'C16 H30 N2 O6'
_chemical_formula_weight         346.42
_chemical_name_common            273K
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-10-06
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 104.7760(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.1309(2)
_cell_length_b                   8.48250(10)
_cell_length_c                   13.6493(2)
_cell_measurement_reflns_used    5510
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      25.79
_cell_measurement_theta_min      2.43
_cell_volume                     1022.22(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'INCOATEC quazar mirrior optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_unetI/netI     0.0117
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            27448
_diffrn_reflns_theta_full        28.33
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_min         2.43
_diffrn_source                   'INCOATEC Mo micro source'
_diffrn_source_type              'Bruker APEX II DUO QUAZAR'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_T_max  0.9831
_exptl_absorpt_correction_T_min  0.9748
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'symmetry-related measurements'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.125
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'hexagonal block'
_exptl_crystal_F_000             376
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.114
_refine_diff_density_min         -0.149
_refine_diff_density_rms         0.032
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         2540
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0844
_refine_ls_R_factor_gt           0.0579
_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^)+(0.0686P)^2^+0.2404P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1714
_refine_ls_wR_factor_ref         0.1915
_reflns_number_gt                1601
_reflns_number_total             2540
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            2_273k.cif
_cod_data_source_block           c:
_cod_database_code               4003267
_olex2_refinement_description
;
1. Others
 Fixed Sof: C7A(0.51) H7A1(0.51) H7A2(0.51) H7A3(0.51) C8B(0.49) N1A(0.51)
 N1B(0.49) C8A(0.51) C7B(0.49) H7B1(0.49) H7B2(0.49) H7B3(0.49)
 Fixed Uiso: H4A(0.149) H4B(0.149) H2A(0.15) H2B(0.15) H3A(0.148) H3B(0.148)
 H5A(0.147) H5B(0.147) H6A(0.157) H6B(0.157) H1A(0.157) H1B(0.157) H7A1(0.1)
 H7A2(0.1) H7A3(0.1) H7B1(0.152) H7B2(0.152) H7B3(0.152)
 Fixed X: H4A(0.6775) H4B(0.7092) H2A(0.244) H2B(0.1962) H3A(0.456)
 H3B(0.4256) H5A(0.8645) H5B(0.7184) H6A(0.8335) H6B(0.9792) H1A(0.0411)
 H1B(0.0898) H7A1(0.4443) H7A2(0.3653) H7A3(0.5359) H7B1(0.3704) H7B2(0.4745)
 H7B3(0.5155)
 Fixed Y: H4A(0.576) H4B(0.4358) H2A(0.5818) H2B(0.4237) H3A(0.3444)
 H3B(0.4828) H5A(0.6636) H5B(0.7493) H6A(0.7747) H6B(0.6818) H1A(0.3567)
 H1B(0.517) H7A1(0.7423) H7A2(0.6247) H7A3(0.6701) H7B1(0.6728) H7B2(0.6448)
 H7B3(0.7764)
 Fixed Z: H4A(0.226) H4B(0.3039) H2A(0.2459) H2B(0.1862) H3A(0.2414)
 H3B(0.162) H5A(0.3549) H5B(0.3686) H6A(0.5461) H6B(0.5387) H1A(0.3015)
 H1B(0.3583) H7A1(0.4329) H7A2(0.4919) H7A3(0.5361) H7B1(0.434) H7B2(0.5432)
 H7B3(0.4741)
;
_olex2_submission_special_instructions 'No special instructions were received'