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

data_7220637
_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         '0.25(H4 O4), 2(C9 H10 N2)'
_chemical_formula_sum            'C18 H21 N4 O'
_chemical_formula_weight         309.39
_chemical_name_common            '5,6-dimethylbenzimidazole hemihydrate'
_chemical_name_systematic
;
 5,6-dimethylbenzimidazole hemihydrate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d'
_symmetry_space_group_name_Hall  '-F 2uv 2vw'
_symmetry_space_group_name_H-M   'F d d d :2'
_atom_sites_solution_hydrogens   mixed
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   7.2661(15)
_cell_length_b                   12.407(8)
_cell_length_c                   34.550(5)
_cell_measurement_reflns_used    710
_cell_measurement_temperature    296
_cell_measurement_theta_max      24.8040
_cell_measurement_theta_min      3.7370
_cell_volume                     3115(2)
_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 0.599
_diffrn_measured_fraction_theta_max 0.555
_diffrn_measurement_details
;
  1 phi    -35.00   19.60   0.7000   10.0000
omega____ theta____ kappa____ phi______ frames
   0.0000  -30.0000    0.0000     -     78

  2 phi    140.00  199.50   0.7000   10.0000
omega____ theta____ kappa____ phi______ frames
   0.0000  -30.0000    0.0000     -     85

  3 phi    160.00  216.70   0.7000   10.0000
omega____ theta____ kappa____ phi______ frames
   0.0000   30.0000    0.0000     -     81

  4 phi    -20.00   34.60   0.7000   10.0000
omega____ theta____ kappa____ phi______ frames
   0.0000   30.0000    0.0000     -     78

  5 omega  -24.00   23.60   0.7000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   39.4600  -12.9000 68

  6 omega  -24.00   23.60   0.7000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   39.4600  167.1000 68

  7 omega  -50.00    9.50   0.7000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000   39.4600  167.1000 85

  8 omega  -50.00    9.50   0.7000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000   39.4600  -12.9000 85

  9 omega  -64.00   -8.00   0.7000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000   81.4000  -28.9000 80

 10 omega  -64.00   -8.00   0.7000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000   81.4000  151.1000 80

 11 omega  -19.00    7.60   0.7000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   81.4000  151.1000 38

 12 omega  -19.00    7.60   0.7000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   81.4000  -28.9000 38

 13 omega  -43.00  -21.30   0.7000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000  134.6000  -56.9000 31

 14 omega  -43.00  -21.30   0.7000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000  134.6000  123.1000 31

 15 omega  -90.00  -36.10   0.7000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000  134.6000  123.1000 77

 16 omega  -90.00  -36.10   0.7000   10.0000
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      -0.0293014000
_diffrn_orient_matrix_UB_12      -0.0510425000
_diffrn_orient_matrix_UB_13      0.0069777000
_diffrn_orient_matrix_UB_21      0.0020631000
_diffrn_orient_matrix_UB_22      0.0199786000
_diffrn_orient_matrix_UB_23      0.0192113000
_diffrn_orient_matrix_UB_31      -0.0930107000
_diffrn_orient_matrix_UB_32      0.0164967000
_diffrn_orient_matrix_UB_33      -0.0017600000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1459
_diffrn_reflns_av_unetI/netI     0.0846
_diffrn_reflns_laue_measured_fraction_full 0.599
_diffrn_reflns_laue_measured_fraction_max 0.555
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            3831
_diffrn_reflns_point_group_measured_fraction_full 0.599
_diffrn_reflns_point_group_measured_fraction_max 0.555
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.160
_diffrn_reflns_theta_min         4.389
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Correction for absorption of the diamond-anvil cell and the sample 
 were made using program REDSHABS (Katrusiak, A. (2003) REDSHABS. Adam
 Mickiewicz University Pozna\'n; Katrusiak, A. (2004) Z. Kristallogr.
 219, 461-467).
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_description       plate
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.202
_refine_diff_density_min         -0.214
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     58
_refine_ls_number_reflns         486
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.1586
_refine_ls_R_factor_gt           0.0848
_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^)+(0.1580P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2067
_refine_ls_wR_factor_ref         0.2753
_reflns_Friedel_coverage         0.000
_reflns_number_gt                254
_reflns_number_total             486
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce00694e2.cif
_cod_data_source_block           dMBzImH_0.54GPa
_cod_depositor_comments
'Adding full bibliography for 7220631--7220640.cif.'
_cod_database_code               7220637
_shelxl_version_number           2013-4
_reflns_odcompleteness_completeness 54.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.10
_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, All O(H) groups
2. Restrained distances
 H1-N3
 1.98 with sigma of 0.001
3. 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
4. Uiso/Uaniso restraints and constraints
O1: within 1.7A with sigma of 0.1 and sigma for terminal atoms of 0.08
Uanis(O1) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
5. Others
 Fixed Sof: H1(0.25) H3(0.5)
6.a Free rotating group:
 O1(H1)
6.b Aromatic/amide H refined with riding coordinates:
 N3(H3), C2(H2), C4(H4)
6.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C)
;
_shelx_res_checksum              51003
_olex2_submission_special_instructions 'No special instructions were received'