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_7242997
_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                 105.399(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.6264(11)
_cell_length_b                   7.0823(5)
_cell_length_c                   9.0843(7)
_cell_measurement_reflns_used    4735
_cell_measurement_temperature    230.06(10)
_cell_measurement_theta_max      29.8730
_cell_measurement_theta_min      2.7050
_cell_volume                     969.27(13)
_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      N~2~
_diffrn_ambient_temperature      230.06(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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      -0.0409817000
_diffrn_orient_matrix_UB_12      -0.0476111000
_diffrn_orient_matrix_UB_13      -0.0283919000
_diffrn_orient_matrix_UB_21      0.0222114000
_diffrn_orient_matrix_UB_22      -0.0881069000
_diffrn_orient_matrix_UB_23      0.0154530000
_diffrn_orient_matrix_UB_31      -0.0066720000
_diffrn_orient_matrix_UB_32      0.0000333000
_diffrn_orient_matrix_UB_33      0.0742231000
_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  0.0308
_diffrn_reflns_av_unetI/netI     0.0179
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_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            8389
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.348
_diffrn_reflns_theta_min         2.704
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.079
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.569
_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    1.255
_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         0.090
_refine_diff_density_min         -0.121
_refine_diff_density_rms         0.025
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         1082
_refine_ls_number_restraints     164
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0370
_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^)+(0.0677P)^2^+0.0811P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1056
_refine_ls_wR_factor_ref         0.1129
_reflns_Friedel_coverage         0.000
_reflns_number_gt                838
_reflns_number_total             1082
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00706h2.cif
_cod_data_source_block           BPI_230_00_autored
_cod_depositor_comments
'Adding full bibliography for 7242993--7243020.cif.'
_cod_database_code               7242997
_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 99.82
_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
 1.37762 with sigma of 0.02
 C5B-C6B = C6B-C7B = C8B-C9B = C9B-C5B
 1.37762 with sigma of 0.02
 N1-C1 = C7A-N3A = C7B-N3B = C8A-N3A = C8B-N3B
 1.32877 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              3595
_olex2_exptl_crystal_mounting_method
'Hampton Research 20 micron nylon CryoLoop'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_diffrn_reflns_filtered   1465
_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 2.351
_oxdiff_exptl_absorpt_empirical_full_min 0.774