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_4003269
_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            220K
_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                 104.9870(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.15390(10)
_cell_length_b                   8.40910(10)
_cell_length_c                   13.5804(2)
_cell_measurement_reflns_used    6341
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      22.63
_cell_measurement_theta_min      2.42
_cell_volume                     1009.81(2)
_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      220(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  0.0248
_diffrn_reflns_av_unetI/netI     0.0115
_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            27076
_diffrn_reflns_theta_full        28.33
_diffrn_reflns_theta_max         28.33
_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  0.9829
_exptl_absorpt_correction_T_min  0.9745
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'symmetry-related measurements'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.139
_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         0.135
_refine_diff_density_min         -0.173
_refine_diff_density_rms         0.031
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         2517
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0749
_refine_ls_R_factor_gt           0.0557
_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^)+(0.0657P)^2^+0.2921P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1644
_refine_ls_wR_factor_ref         0.1783
_reflns_number_gt                1794
_reflns_number_total             2517
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            2_220k.cif
_cod_data_source_block           c:
_cod_database_code               4003269
_olex2_refinement_description
;
1. Others
 Fixed Sof: N1A(0.54) N1B(0.46) C7A(0.54) H7A1(0.54) H7A2(0.54) H7A3(0.54)
 C7B(0.46) H7B1(0.46) H7B2(0.46) H7B3(0.46) C8A(0.54) C8B(0.46)
 Fixed Uiso: H1A(0.13) H1B(0.13) H2A(0.128) H2B(0.128) H3A(0.123) H3B(0.123)
 H4A(0.125) H4B(0.125) H5A(0.124) H5B(0.124) H6A(0.132) H6B(0.132) H7A1(0.077)
 H7A2(0.077) H7A3(0.077) H7B1(0.13) H7B2(0.13) H7B3(0.13)
 Fixed X: H1A(0.0412) H1B(0.0902) H2A(0.2472) H2B(0.1992) H3A(0.4587)
 H3B(0.43) H4A(0.6818) H4B(0.7121) H5A(0.8694) H5B(0.7224) H6A(0.8358)
 H6B(0.9826) H7A1(0.3793) H7A2(0.5353) H7A3(0.4587) H7B1(0.5244) H7B2(0.3555)
 H7B3(0.466)
 Fixed Y: H1A(0.357) H1B(0.5208) H2A(0.5837) H2B(0.4225) H3A(0.3407)
 H3B(0.4823) H4A(0.5737) H4B(0.4305) H5A(0.6603) H5B(0.7492) H6A(0.7755)
 H6B(0.6791) H7A1(0.613) H7A2(0.6889) H7A3(0.7425) H7B1(0.7602) H7B2(0.6983)
 H7B3(0.6276)
 Fixed Z: H1A(0.296) H1B(0.3533) H2A(0.2429) H2B(0.1822) H3A(0.2403) H3B(0.16)
 H4A(0.226) H4B(0.305) H5A(0.3574) H5B(0.3702) H6A(0.5487) H6B(0.543)
 H7A1(0.4861) H7A2(0.5462) H7A3(0.4327) H7B1(0.4717) H7B2(0.4352) H7B3(0.5351)
;
_olex2_submission_special_instructions 'No special instructions were received'