Reversible Regulating of Crystal Structures Based on Isomerization of Phenylhydrazones
Ma, Lulu; Yuan, Zexing; Huang, Zhenguo; Jin, Jingyi; Cao, Duxia; Guan, Ruifang; Chen, Qifeng; sun, xuan; Chem. Commun.  (2017) –; doi:10.1039/C7CC06374A

data_7120810
_publ_section_title
;
 Reversible Regulating of Crystal Structures Based on Isomerization of
 Phenylhydrazones
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC06374A
_journal_year                    2017
_chemical_formula_moiety         'C13 H10 N4'
_chemical_formula_sum            'C13 H10 N4'
_chemical_formula_weight         222.25
_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             2016-04-18
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-06-18 deposited with the CCDC.
2017-10-23 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 108.323(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.2896(8)
_cell_length_b                   5.5930(3)
_cell_length_c                   16.4363(9)
_cell_measurement_reflns_used    2298
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      71.7280
_cell_measurement_theta_min      5.1470
_cell_volume                     1159.75(12)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0355
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega   16.00  105.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.3677   37.0000 -150.0000 89

  2 omega  -32.00   52.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.3677  -57.0000   60.0000 84

  3 omega  -34.00   55.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.3677  -37.0000 -180.0000 89

  4 omega   18.00   89.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.3677 -125.0000 -150.0000 71

  5 omega   -7.00   19.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.3677  106.0000   -6.6920 26

  6 omega   38.00   91.00   1.0000    3.0550
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   60.0000 53

  7 omega   38.00  116.00   1.0000    3.0550
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000 -180.0000 78

  8 omega   91.00  176.00   1.0000    3.0550
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000 -180.0000 85

  9 omega   40.00   98.00   1.0000    3.0550
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  150.0000 58

 10 omega   39.00  109.00   1.0000    3.0550
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000 -180.0000 70

 11 omega   40.00   98.00   1.0000    3.0550
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -30.0000 58

 12 omega   39.00  109.00   1.0000    3.0550
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000    0.0000 70

 13 omega   90.00  175.00   1.0000    3.0550
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000 -150.0000 85

 14 omega   38.00   91.00   1.0000    3.0550
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   30.0000 53

 15 omega   16.00  105.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.3677   37.0000    0.0000 89

 16 omega   19.00  103.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.3677   57.0000   90.0000 84

 17 omega   19.00  103.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.3677   57.0000  -90.0000 84

 18 omega  -34.00   55.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       35.3677  -37.0000  -90.0000 89

 19 omega   90.00  175.00   1.0000    3.0550
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000   90.0000 85
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0677702000
_diffrn_orient_matrix_UB_12      -0.2265632000
_diffrn_orient_matrix_UB_13      -0.0056137000
_diffrn_orient_matrix_UB_21      -0.0968418000
_diffrn_orient_matrix_UB_22      0.1564870000
_diffrn_orient_matrix_UB_23      -0.0039812000
_diffrn_orient_matrix_UB_31      -0.0306143000
_diffrn_orient_matrix_UB_32      0.0066778000
_diffrn_orient_matrix_UB_33      -0.0984854000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_av_unetI/netI     0.0175
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            6340
_diffrn_reflns_theta_full        66.55
_diffrn_reflns_theta_max         66.55
_diffrn_reflns_theta_min         5.16
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.644
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74282
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.132
_refine_diff_density_min         -0.151
_refine_diff_density_rms         0.030
_refine_ls_extinction_coef       0.0036(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         2050
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0681P)^2^+0.0966P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1115
_refine_ls_wR_factor_ref         0.1200
_reflns_number_gt                1688
_reflns_number_total             2050
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7cc06374a2.cif
_cod_data_source_block           160417_hq_2_chn
_cod_original_cell_volume        1159.75(11)
_cod_database_code               7120810
_chemical_oxdiff_formula         'C H N'
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N3(H3), C9(H9), C4(H4), C13(H13), C10(H10), C3(H3A), C11(H11), C1(H1),
 C12(H12), C2(H2)
;
_olex2_date_sample_data_collection 2009-06-15
_olex2_submission_special_instructions 'No special instructions were received'