Pressure-induced preference for solvation of 5,6-dimethylbenzimidazole
Zielinski, Witold; Katrusiak, Andrzej; CrystEngComm 18 (2016) 3211–; doi:10.1039/C6CE00419A

data_7224791
_publ_section_title
;
 Pressure-induced preference for solvation of 5,6-dimethylbenzimidazole
;
_journal_issue                   18
_journal_name_full               CrystEngComm
_journal_page_first              3211
_journal_paper_doi               10.1039/C6CE00419A
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C10 H14 N2 O'
_chemical_formula_sum            'C10 H14 N2 O'
_chemical_formula_weight         178.23
_chemical_name_common            '5,6-dimethylbenzimidazole methanol solvate'
_chemical_name_systematic        '5,6-dimethylbenzimidazole methanol solvate'
_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             2016-03-29
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-03-29 deposited with the CCDC.
2016-04-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.71(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.960(12)
_cell_length_b                   7.1574(10)
_cell_length_c                   12.5790(8)
_cell_measurement_reflns_used    632
_cell_measurement_temperature    296
_cell_measurement_theta_max      25.3000
_cell_measurement_theta_min      4.2950
_cell_volume                     894.8(11)
_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, 2015)'
_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 0.247
_diffrn_measured_fraction_theta_max 0.226
_diffrn_measurement_details
;
  1 phi    -35.00   19.60   0.7000   33.0000
omega____ theta____ kappa____ phi______ frames
   0.0000  -30.0000    0.0000     -     78

  2 phi    140.00  199.50   0.7000   33.0000
omega____ theta____ kappa____ phi______ frames
   0.0000  -30.0000    0.0000     -     85

  3 phi    160.00  216.70   0.7000   33.0000
omega____ theta____ kappa____ phi______ frames
   0.0000   30.0000    0.0000     -     81

  4 phi    -20.00   34.60   0.7000   33.0000
omega____ theta____ kappa____ phi______ frames
   0.0000   30.0000    0.0000     -     78

  5 omega  -24.00   23.60   0.7000   33.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   39.4600  -12.9000 68

  6 omega  -24.00   23.60   0.7000   33.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000   39.4600  167.1000 68

  7 omega  -50.00    8.80   0.7000   33.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000   39.4600  167.1000 84
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w and \p scans'
_diffrn_orient_matrix_UB_11      -0.0716908000
_diffrn_orient_matrix_UB_12      0.0010033000
_diffrn_orient_matrix_UB_13      -0.0031526000
_diffrn_orient_matrix_UB_21      -0.0003532000
_diffrn_orient_matrix_UB_22      0.0287307000
_diffrn_orient_matrix_UB_23      -0.0538377000
_diffrn_orient_matrix_UB_31      -0.0009815000
_diffrn_orient_matrix_UB_32      -0.0946012000
_diffrn_orient_matrix_UB_33      -0.0164116000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_unetI/netI     0.0484
_diffrn_reflns_Laue_measured_fraction_full 0.247
_diffrn_reflns_Laue_measured_fraction_max 0.226
_diffrn_reflns_limit_h_max       3
_diffrn_reflns_limit_h_min       -3
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            2381
_diffrn_reflns_point_group_measured_fraction_full 0.247
_diffrn_reflns_point_group_measured_fraction_max 0.226
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.173
_diffrn_reflns_theta_min         4.319
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58603
_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_density_diffrn    1.323
_exptl_crystal_description       plate
_exptl_crystal_F_000             384
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.155
_refine_diff_density_min         -0.126
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     111
_refine_ls_number_reflns         449
_refine_ls_number_restraints     74
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.1198
_refine_ls_R_factor_gt           0.0644
_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^)+(0.0827P)^2^+1.3302P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1532
_refine_ls_wR_factor_ref         0.2050
_reflns_Friedel_coverage         0.000
_reflns_number_gt                277
_reflns_number_total             449
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce00419a2.cif
_cod_data_source_block           dMBzIm_MeOH_1_24GPa
_cod_depositor_comments
'Adding full bibliography for 7224786--7224795.cif.'
_cod_database_code               7224791
_reflns_odcompleteness_completeness 22.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.11
_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,H) groups
2. Restrained distances
 H1A-N3_$1
 1.94 with sigma of 0.02
 H1B-N1
 1.94 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C10) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C9) \\sim
Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(C12)
\\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C2) \\sim Ueq,
Uanis(C7) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.002
4. Others
 Sof(H1B)=Sof(H3)=1-FVAR(1)
 Sof(H1A)=Sof(H1)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 N1(H1), N3(H3), C2(H2), C7(H7), C4(H4)
5.b Fitted hexagon refined as free rotating group:
 C7(C8,C9,C4,C5,C6)
5.c Idealised Me refined as rotating group:
 C1(H1C,H1D,H1E), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C)
5.d Idealised tetrahedral OH refined as rotating group:
 O1(H1A), O1(H1B)
;
_shelx_res_checksum              32912
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'