Modulation of Thermal Expansion by Guests and Polymorphism in a Hydrogen Bonded Host
Saraswatula, Viswanadha G.; Saha, Binoy K.; Crystal Growth & Design 15 (2015) 593–; doi:10.1021/cg501178f

data_4512780
_publ_section_title
;
 Modulation of Thermal Expansion by Guests and Polymorphism in a Hydrogen
 Bonded Host
;
_journal_issue                   2
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              593
_journal_paper_doi               10.1021/cg501178f
_journal_volume                  15
_journal_year                    2015
_chemical_formula_moiety         'C30 H28 O4, 2(C7 H8 O)'
_chemical_formula_sum            'C44 H44 O6'
_chemical_formula_weight         668.79
_chemical_name_common            1-oc-2D-115K
_chemical_name_systematic
;
 1,1,4,4-tetrakis(4-hydroxyphenyl)cyclohexane, 2-methylphenol 
;
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-04-14
_audit_creation_method
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4720)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 89.858(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.0427(2)
_cell_length_b                   9.9362(2)
_cell_length_c                   17.0473(3)
_cell_measurement_reflns_used    5510
_cell_measurement_temperature    115(2)
_cell_measurement_theta_max      29.2126
_cell_measurement_theta_min      2.8780
_cell_volume                     1701.08(6)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_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      115(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0193
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            7038
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.88
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_T_max  0.9592
_exptl_absorpt_correction_T_min  0.9496
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.61
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.49
_refine_diff_density_max         0.246
_refine_diff_density_min         -0.211
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         2968
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0359
_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^)+(0.0422P)^2^+0.6687P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0872
_refine_ls_wR_factor_ref         0.0915
_reflns_number_gt                2631
_reflns_number_total             2968
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1-oc-2D-combined.cif
_cod_data_source_block           1-oc-2d-115k
_cod_database_code               4512780
_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, All O(H) groups
2. Restrained distances
 C21B-C20B \\sim C21B-C16B \\sim C17B-C16B \\sim C18B-C17B \\sim C19B-C18B
\\sim C20B-C19B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uiso(C16A) = Uiso(C16B)
4. Others
 1*[Sof(O3A)+Sof(H3AA)+Sof(C16A)+Sof(C17A)+Sof(C18A)+Sof(H18A)+Sof(C21A)+
 Sof(H21A)+Sof(C22A)+Sof(H22D)+Sof(H22E)+Sof(H22F)+Sof(C19A)+Sof(H19A)+
 Sof(C20A)+Sof(H20A)+Sof(C17B)+Sof(H17B)+Sof(C21B)+Sof(C19B)+Sof(H19B)+
 Sof(C22B)+Sof(H22A)+Sof(H22B)+Sof(H22C)+Sof(C18B)+Sof(H18B)+Sof(C16B)+
 Sof(C20B)]+1*[Sof(O3B)+Sof(H3BA)]+1*[Sof(O3C)+Sof(H3C)]=1 with esd of 0.0001
 Sof(C17B)=Sof(H17B)=Sof(C21B)=Sof(C19B)=Sof(H19B)=Sof(C22B)=Sof(H22A)=
 Sof(H22B)=Sof(H22C)=Sof(C18B)=Sof(H18B)=Sof(C16B)=Sof(C20B)=1-FVAR(1)
 Sof(O3A)=Sof(H3AA)=Sof(C16A)=Sof(C17A)=Sof(C18A)=Sof(H18A)=Sof(C21A)=
 Sof(H21A)=Sof(C22A)=Sof(H22D)=Sof(H22E)=Sof(H22F)=Sof(C19A)=Sof(H19A)=
 Sof(C20A)=Sof(H20A)=FVAR(1)
 Sof(O3B)=Sof(H3BA)=FVAR(2)
 Sof(O3C)=Sof(H3C)=FVAR(3)
5.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C1(H1A,H1B)
5.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C8(H8), C11(H11), C12(H12), C15(H15), C9(H9), C14(H14),
 C18A(H18A), C21A(H21A), C19A(H19A), C20A(H20A), C17B(H17B), C19B(H19B),
 C18B(H18B)
5.c Idealised Me refined as rotating group:
 C22A(H22D,H22E,H22F), C22B(H22A,H22B,H22C)
5.d Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2), O3A(H3AA), O3B(H3BA), O3C(H3C)
;