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_4003270
_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            180K
_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                 105.1080(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.1653(2)
_cell_length_b                   8.3545(2)
_cell_length_c                   13.5416(3)
_cell_measurement_reflns_used    7097
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      26.83
_cell_measurement_theta_min      2.42
_cell_volume                     1001.06(4)
_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      180(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0263
_diffrn_reflns_av_unetI/netI     0.0124
_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            26618
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         2.42
_diffrn_source                   'INCOATEC Mo micro source'
_diffrn_source_type              'Bruker APEX II DUO QUAZAR'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_T_max  0.9828
_exptl_absorpt_correction_T_min  0.9743
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'symmetry-related measurements'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.149
_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         0.159
_refine_diff_density_min         -0.230
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         2489
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0639
_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^)+(0.0621P)^2^+0.5371P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1752
_refine_ls_wR_factor_ref         0.1847
_reflns_number_gt                1946
_reflns_number_total             2489
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            2_180k.cif
_cod_data_source_block           c:k
_cod_database_code               4003270
_olex2_refinement_description
;
1. Shared sites
{C7A, C7B}
2. Others
 Fixed Sof: C7A(0.62) H7A1(0.62) H7A2(0.62) H7A3(0.62) C8A(0.62) N1A(0.62)
 N1B(0.38) C8B(0.38) C7B(0.38) H7B1(0.38) H7B2(0.38) H7B3(0.38)
 Fixed Uiso: H7A1(0.1) H7A2(0.1) H7A3(0.1) H4A(0.111) H4B(0.111) H2A(0.115)
 H2B(0.115) H3A(0.107) H3B(0.107) H5A(0.108) H5B(0.108) H6A(0.114) H6B(0.114)
 H1A(0.112) H1B(0.112) H7B1(0.054) H7B2(0.054) H7B3(0.054)
 Fixed X: H7A1(0.5047) H7A2(0.3511) H7A3(0.4961) H4A(0.6864) H4B(0.7148)
 H2A(0.2504) H2B(0.2026) H3A(0.4634) H3B(0.4367) H5A(0.8743) H5B(0.726)
 H6A(0.8364) H6B(0.985) H1A(0.0414) H1B(0.0905) H7B1(0.5452) H7B2(0.4449)
 H7B3(0.3952)
 Fixed Y: H7A1(0.7618) H7A2(0.6667) H7A3(0.6372) H4A(0.5709) H4B(0.4253)
 H2A(0.5852) H2B(0.4209) H3A(0.3371) H3B(0.4806) H5A(0.6571) H5B(0.7487)
 H6A(0.776) H6B(0.6776) H1A(0.3566) H1B(0.5236) H7B1(0.7089) H7B2(0.7359)
 H7B3(0.6054)
 Fixed Z: H7A1(0.4544) H7A2(0.4486) H7A3(0.5425) H4A(0.2265) H4B(0.3066)
 H2A(0.24) H2B(0.1787) H3A(0.2407) H3B(0.1591) H5A(0.3604) H5B(0.3721)
 H6A(0.5515) H6B(0.5473) H1A(0.2913) H1B(0.3491) H7B1(0.5398) H7B2(0.4252)
 H7B3(0.4966)
;
_olex2_submission_special_instructions 'No special instructions were received'