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

data_7220634
_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(C9 H10 N2), 0.33(C18 H19 N4)'
_chemical_formula_sum            'C9 H9.67 N2'
_chemical_formula_weight         145.85
_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                 102.68(4)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   6.538(3)
_cell_length_b                   26.99(14)
_cell_length_c                   13.930(5)
_cell_measurement_reflns_used    727
_cell_measurement_temperature    296
_cell_measurement_theta_max      22.4090
_cell_measurement_theta_min      3.2250
_cell_volume                     2398(13)
_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 8.0772
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.264
_diffrn_measured_fraction_theta_max 0.233
_diffrn_measurement_details
;
  1 phi    -35.00   19.60   0.7000   30.0000
omega____ theta____ kappa____ phi______ frames
   0.0000  -30.0000    0.0000     -     78

  2 phi    140.00  199.50   0.7000   30.0000
omega____ theta____ kappa____ phi______ frames
   0.0000  -30.0000    0.0000     -     85

  3 phi    160.00  216.70   0.7000   30.0000
omega____ theta____ kappa____ phi______ frames
   0.0000   30.0000    0.0000     -     81

  4 phi    -20.00   34.60   0.7000   30.0000
omega____ theta____ kappa____ phi______ frames
   0.0000   30.0000    0.0000     -     78

  5 omega  -24.00   23.60   0.7000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   39.4600  -12.9000 68

  6 omega  -24.00   23.60   0.7000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   39.4600  167.1000 68

  7 omega  -50.00    9.50   0.7000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000   39.4600  167.1000 85

  8 omega  -50.00    9.50   0.7000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000   39.4600  -12.9000 85

  9 omega  -64.00   -8.00   0.7000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000   81.4000  -28.9000 80

 10 omega  -64.00   -8.00   0.7000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000   81.4000  151.1000 80

 11 omega  -19.00    7.60   0.7000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   81.4000  151.1000 38

 12 omega  -19.00    7.60   0.7000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   81.4000  -28.9000 38

 13 omega  -43.00  -21.30   0.7000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000  134.6000  -56.9000 31

 14 omega  -43.00  -21.30   0.7000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000  134.6000  123.1000 31

 15 omega  -90.00  -36.10   0.7000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000  134.6000  123.1000 77

 16 omega  -90.00  -36.10   0.7000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000  134.6000  -56.9000 77
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w and \p scans'
_diffrn_orient_matrix_UB_11      -0.0028054000
_diffrn_orient_matrix_UB_12      -0.0262098000
_diffrn_orient_matrix_UB_13      0.0000032000
_diffrn_orient_matrix_UB_21      0.0014843000
_diffrn_orient_matrix_UB_22      0.0001557000
_diffrn_orient_matrix_UB_23      0.0510473000
_diffrn_orient_matrix_UB_31      -0.1114639000
_diffrn_orient_matrix_UB_32      0.0006447000
_diffrn_orient_matrix_UB_33      -0.0106838000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2049
_diffrn_reflns_av_unetI/netI     0.1310
_diffrn_reflns_laue_measured_fraction_full 0.264
_diffrn_reflns_laue_measured_fraction_max 0.233
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14260
_diffrn_reflns_point_group_measured_fraction_full 0.264
_diffrn_reflns_point_group_measured_fraction_max 0.233
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.079
_diffrn_reflns_theta_min         2.998
_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  0.36335
_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    1.212
_exptl_crystal_description       plate
_exptl_crystal_F_000             932
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.114
_refine_diff_density_min         -0.125
_refine_diff_density_rms         0.031
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         1358
_refine_ls_number_restraints     285
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.2291
_refine_ls_R_factor_gt           0.0883
_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^)+(0.1370P)^2^+1.9930P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2049
_refine_ls_wR_factor_ref         0.2909
_reflns_Friedel_coverage         0.000
_reflns_number_gt                546
_reflns_number_total             1358
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce00694e2.cif
_cod_data_source_block           dMBzIm_0.33GPa
_cod_depositor_comments
'Adding full bibliography for 7220631--7220640.cif.'
_cod_database_code               7220634
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C9 H10 N2'
_reflns_odcompleteness_completeness 24.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.02
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 0.08A with sigma of 0.04 and
sigma for terminal atoms of 0.08
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.01 and sigma
for terminal atoms of 0.01
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 X=CH2 refined with riding coordinates:
 C29(H29A,H29B)
5.c 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)
;
_shelx_res_checksum              30287
_olex2_submission_special_instructions 'No special instructions were received'