Solid-state behaviors of imines: colossal biaxial positive thermal expansion, motion capability, and phase transitions
Juneja, Navkiran; Zahid, Ethan; Unruh, Daniel K.; Hutchins, Kristin M.; CrystEngComm 23 (2021) 4439–4443; doi:10.1039/D1CE00706H

data_7242998
_publ_section_title
;
 Solid-state behaviors of imines: colossal biaxial positive thermal
 expansion, motion capability, and phase transitions
;
_journal_issue                   25
_journal_name_full               CrystEngComm
_journal_page_first              4439
_journal_page_last               4443
_journal_paper_doi               10.1039/D1CE00706H
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C11 H9 N3'
_chemical_formula_sum            'C11 H9 N3'
_chemical_formula_weight         183.21
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-05-25
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.03.28 svn.rd84adfe8 for Rigaku Oxford Diffraction, GUI svn.r6032)
;
_audit_update_record
;
2021-05-28 deposited with the CCDC.	2021-06-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.081(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7226(13)
_cell_length_b                   7.1311(6)
_cell_length_c                   9.0875(10)
_cell_measurement_reflns_used    3950
_cell_measurement_temperature    290.06(11)
_cell_measurement_theta_max      29.9090
_cell_measurement_theta_min      3.0400
_cell_volume                     979.02(17)
_computing_cell_refinement       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      290.06(11)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -28.00  68.00   0.50   27.23    --   -5.21  77.00 -30.00  192
  2  \w    -28.00  68.00   0.50   27.23    --   -5.21  77.00 -90.00  192
  3  \w    -17.00  78.00   0.50   27.23    --    5.37  77.00 120.00  190
  4  \w    -17.00  78.00   0.50   27.23    --    5.37  77.00-150.00  190
  5  \w    -17.00  78.00   0.50   27.23    --    5.37  77.00 -90.00  190
  6  \w    -17.00  78.00   0.50   27.23    --    5.37  77.00  60.00  190
  7  \w    -23.00   6.00   0.50   27.23    --    5.37 -99.00 -90.00   58
  8  \w    -23.00  39.00   0.50   27.23    --    5.37 -99.00 150.00  124
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0415006000
_diffrn_orient_matrix_UB_12      -0.0453820000
_diffrn_orient_matrix_UB_13      -0.0275603000
_diffrn_orient_matrix_UB_21      0.0214309000
_diffrn_orient_matrix_UB_22      -0.0884708000
_diffrn_orient_matrix_UB_23      0.0123654000
_diffrn_orient_matrix_UB_31      -0.0046867000
_diffrn_orient_matrix_UB_32      -0.0021473000
_diffrn_orient_matrix_UB_33      0.0754229000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_unetI/netI     0.0151
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            8659
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.368
_diffrn_reflns_theta_min         2.696
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.549
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.104a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_description       plate
_exptl_crystal_F_000             384
_exptl_crystal_size_max          0.282
_exptl_crystal_size_mid          0.163
_exptl_crystal_size_min          0.035
_refine_diff_density_max         0.079
_refine_diff_density_min         -0.125
_refine_diff_density_rms         0.024
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         1093
_refine_ls_number_restraints     164
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0375
_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^)+(0.0642P)^2^+0.0869P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1061
_refine_ls_wR_factor_ref         0.1174
_reflns_Friedel_coverage         0.000
_reflns_number_gt                767
_reflns_number_total             1093
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00706h2.cif
_cod_data_source_block           BPI_290_00
_cod_depositor_comments
'Adding full bibliography for 7242993--7243020.cif.'
_cod_original_cell_volume        979.02(16)
_cod_database_code               7242998
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.997
_shelx_estimated_absorpt_t_min   0.978
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C6A-C5A = C6A-C7A = C9A-C8A = C9A-C5A = C1-C2A = C2A-C3A = C1-C2B = C2B-C3B
 1.37367 with sigma of 0.02
 C5B-C6B = C6B-C7B = C8B-C9B = C9B-C5B
 1.37367 with sigma of 0.02
 N1-C1 = C7A-N3A = C7B-N3B = C8A-N3A = C8B-N3B
 1.32102 with sigma of 0.02
3. Rigid body (RIGU) restrains
 N1, C1, N2B, C2B, N3B, C3B, C4B, C5B, C6B, C7B, C8B, C9B, N2A, C2A, C3A, N3A,
 C4A, C5A, C6A, C7A, C8A, C9A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.005
4. Others
 Sof(H1B)=Sof(C2B)=Sof(H2B)=1-FVAR(1)
 Sof(N2B)=Sof(N3B)=Sof(C3B)=Sof(C4B)=Sof(H4B)=Sof(C5B)=Sof(C6B)=Sof(H6B)=
 Sof(C7B)=Sof(H7B)=Sof(C8B)=Sof(H8B)=Sof(C9B)=Sof(H9B)=0.5*(1-FVAR(2))
 Sof(N2A)=Sof(C3A)=Sof(N3A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=Sof(C6A)=Sof(H6A)=
 Sof(C7A)=Sof(H7A)=Sof(C8A)=Sof(H8A)=Sof(C9A)=Sof(H9A)=0.5*FVAR(2)
 Sof(H1A)=Sof(C2A)=Sof(H2A)=FVAR(1)
 1(DFIX)=1(DFIX)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1B), C1(H1A), C2B(H2B), C4B(H4B), C6B(H6B), C7B(H7B), C8B(H8B), C9B(H9B),
 C2A(H2A), C4A(H4A), C6A(H6A), C7A(H7A), C8A(H8A), C9A(H9A)
;
_shelx_res_checksum              2099
_olex2_exptl_crystal_mounting_method
'Hampton Research 20 micron nylon CryoLoop'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_diffrn_reflns_filtered   1411
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.417
_oxdiff_exptl_absorpt_empirical_full_min 0.770