Hydrate smaller than the anhydrate
Zieliński, Witold; Katrusiak, Andrzej; CrystEngComm 17 (2015) 5468–; doi:10.1039/C5CE00694E

data_7220633
_publ_section_title
;
 Hydrate smaller than the anhydrate
;
_journal_issue                   29
_journal_name_full               CrystEngComm
_journal_page_first              5468
_journal_paper_doi               10.1039/C5CE00694E
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         '0.33(C27 H30 N6)'
_chemical_formula_sum            'C9 H10 N2'
_chemical_formula_weight         146.19
_chemical_name_common            '5,6-dimethylbenzimidazole phase beta'
_chemical_name_systematic
;
 5,6-dimethylbenzimidazole phase beta
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-05-28
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-05-28 deposited with the CCDC.
2015-06-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.615(15)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   6.5011(10)
_cell_length_b                   27.23(2)
_cell_length_c                   13.949(2)
_cell_measurement_reflns_used    1339
_cell_measurement_temperature    296
_cell_measurement_theta_max      20.0580
_cell_measurement_theta_min      3.5740
_cell_volume                     2409.7(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_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      296
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2413
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.460
_diffrn_measured_fraction_theta_max 0.419
_diffrn_measurement_details
;
  1 phi    -35.00   19.75   0.7500   10.0000
omega____ theta____ kappa____ phi______ frames
   0.0000  -30.0000    0.0000     -     73

  2 phi    140.00  200.00   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
   0.0000  -30.0000    0.0000     -     80

  3 phi    160.00  217.00   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
   0.0000   30.0000    0.0000     -     76

  4 phi    -20.00   34.75   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
   0.0000   30.0000    0.0000     -     73

  5 omega  -24.00   24.00   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   39.4600  -12.9000 64

  6 omega  -24.00   24.00   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   39.4600  167.1000 64

  7 omega  -50.00   10.00   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000   39.4600  167.1000 80

  8 omega  -50.00   10.00   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000   39.4600  -12.9000 80

  9 omega  -64.00   -8.50   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000   81.4000  -28.9000 74

 10 omega  -64.00   -8.50   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000   81.4000  151.1000 74

 11 omega  -19.00    8.00   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   81.4000  151.1000 36

 12 omega  -19.00    8.00   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   81.4000  -28.9000 36

 13 omega  -43.00  -21.25   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000  134.6000  -56.9000 29

 14 omega  -43.00  -21.25   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000  134.6000  123.1000 29

 15 omega  -90.00  -36.00   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000  134.6000  123.1000 72

 16 omega  -90.00  -36.00   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000  134.6000  -56.9000 72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w and \p scans'
_diffrn_orient_matrix_UB_11      -0.0235227000
_diffrn_orient_matrix_UB_12      -0.0251774000
_diffrn_orient_matrix_UB_13      -0.0100002000
_diffrn_orient_matrix_UB_21      -0.0010144000
_diffrn_orient_matrix_UB_22      0.0040130000
_diffrn_orient_matrix_UB_23      -0.0503150000
_diffrn_orient_matrix_UB_31      0.1093262000
_diffrn_orient_matrix_UB_32      -0.0053681000
_diffrn_orient_matrix_UB_33      0.0090080000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2093
_diffrn_reflns_av_unetI/netI     0.2023
_diffrn_reflns_laue_measured_fraction_full 0.460
_diffrn_reflns_laue_measured_fraction_max 0.419
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14463
_diffrn_reflns_point_group_measured_fraction_full 0.460
_diffrn_reflns_point_group_measured_fraction_max 0.419
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.537
_diffrn_reflns_theta_min         3.742
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.074
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.14249
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_description       plate
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.188
_refine_diff_density_min         -0.229
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         2331
_refine_ls_number_restraints     459
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.2814
_refine_ls_R_factor_gt           0.1163
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2809
_refine_ls_wR_factor_ref         0.3944
_reflns_Friedel_coverage         0.000
_reflns_number_gt                785
_reflns_number_total             2331
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce00694e2.cif
_cod_data_source_block           dMBzIm_0.28GPa
_cod_depositor_comments
'Adding full bibliography for 7220631--7220640.cif.'
_cod_original_cell_volume        2410(2)
_cod_database_code               7220633
_shelxl_version_number           2013-4
_reflns_odcompleteness_completeness 43.09
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.48
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C5) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C16) \\sim
Ueq, Uanis(C8) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C4)
\\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C9) \\sim Ueq,
Uanis(C10) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C28)
\\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C29) \\sim Ueq,
Uanis(C13) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(N6)
\\sim Ueq, Uanis(N7) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(N5) \\sim Ueq,
Uanis(C17) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C27)
\\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C22) \\sim Ueq,
Uanis(N4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 N1, N3, C2, C4, C5, C6, C7, C8, C9, C10, H10A, C11, N4, N5, N6, N7, C12, C13,
 C14, C15, C16, C17, C18, C19, C20, C21, C22, C23, C24, C25, C26, C27, C28, C29
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: H1(0.5) H3(0.5) H4(0.5) H5(0.5) H6(0.5) H7(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 N1(H1), N3(H3), C2(H2), C4(H4A), C7(H7A), N4(H4), N5(H5), N6(H6), N7(H7),
 C12(H12), C13(H13), C16(H16), C21(H21), C22(H22), C25(H25)
5.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C)
;
_shelx_res_checksum              95202
_olex2_submission_special_instructions 'No special instructions were received'