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_7242993
_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                 104.821(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.498(2)
_cell_length_b                   7.0467(10)
_cell_length_c                   9.0692(15)
_cell_measurement_reflns_used    4272
_cell_measurement_temperature    190.00(10)
_cell_measurement_theta_max      30.7220
_cell_measurement_theta_min      2.7190
_cell_volume                     957.5(3)
_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      190.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.993
_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      -0.0432858000
_diffrn_orient_matrix_UB_12      -0.0385452000
_diffrn_orient_matrix_UB_13      -0.0289228000
_diffrn_orient_matrix_UB_21      0.0180339000
_diffrn_orient_matrix_UB_22      -0.0930058000
_diffrn_orient_matrix_UB_23      0.0112207000
_diffrn_orient_matrix_UB_31      -0.0064567000
_diffrn_orient_matrix_UB_32      0.0001481000
_diffrn_orient_matrix_UB_33      0.0746785000
_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  0.0579
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.993
_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            5921
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.332
_diffrn_reflns_theta_min         2.719
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.080
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.565
_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    1.271
_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         0.170
_refine_diff_density_min         -0.209
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         1064
_refine_ls_number_restraints     164
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0974
_refine_ls_R_factor_gt           0.0784
_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^)+(0.0609P)^2^+1.6690P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1941
_refine_ls_wR_factor_ref         0.2021
_reflns_Friedel_coverage         0.000
_reflns_number_gt                766
_reflns_number_total             1064
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00706h2.cif
_cod_data_source_block           BPI_190_00
_cod_depositor_comments
'Adding full bibliography for 7242993--7243020.cif.'
_cod_database_code               7242993
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C48  H28  N12  '
_shelx_estimated_absorpt_t_max   0.997
_shelx_estimated_absorpt_t_min   0.978
_reflns_odcompleteness_completeness 99.35
_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
 1.38199 with sigma of 0.02
 C5B-C6B = C6B-C7B = C8B-C9B = C9B-C5B
 1.38199 with sigma of 0.02
 N1-C1 = C7A-N3A = C7B-N3B = C8A-N3A = C8B-N3B
 1.31751 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              72313
_olex2_exptl_crystal_mounting_method
'Hampton Research 20 micron nylon CryoLoop'
_olex2_submission_original_sample_id hut21_46
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_diffrn_reflns_filtered   1354
_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 1.430
_oxdiff_exptl_absorpt_empirical_full_min 0.832