Stability and solid-state polymerization reactivity of imidazolyl- and benzimidazolyl-substituted diacetylenes: pivotal role of lattice water
Fahsi, Karim; Deschamps, Jérôme; Chougrani, Kamel; Viau, Lydie; Boury, Bruno; Vioux, André; van der Lee, Arie; Dutremez, Sylvain G.; CrystEngComm 15 (2013) 4261–; doi:10.1039/c3ce27057b

data_7210087
_publ_section_title
;
 Stability and solid-state polymerization reactivity of imidazolyl- and
 benzimidazolyl-substituted diacetylenes: pivotal role of lattice water
;
_journal_issue                   21
_journal_name_full               CrystEngComm
_journal_page_first              4261
_journal_paper_doi               10.1039/c3ce27057b
_journal_volume                  15
_journal_year                    2013
_chemical_formula_moiety         'C20 H14 N4'
_chemical_formula_sum            'C20 H14 N4'
_chemical_formula_weight         310.35
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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     other
_cell_angle_alpha                90
_cell_angle_beta                 109.568(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3990(4)
_cell_length_b                   15.5354(5)
_cell_length_c                   9.2351(3)
_cell_measurement_reflns_used    6922
_cell_measurement_temperature    173
_cell_measurement_theta_max      26.4685
_cell_measurement_theta_min      2.7910
_cell_volume                     1540.97(10)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 8.4205
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_details
;
1 omega -6.00 102.00 1.0000 70.0000
omega____ theta____ kappa____ phi______ frames
- 12.8809 77.0000 -150.0000 108
2 omega -7.00 100.00 1.0000 70.0000
omega____ theta____ kappa____ phi______ frames
- 12.8809 77.0000 90.0000 107
3 omega -3.00 105.00 1.0000 70.0000
omega____ theta____ kappa____ phi______ frames
- 12.8809 77.0000 -30.0000 108
4 omega -54.00 27.00 1.0000 70.0000
omega____ theta____ kappa____ phi______ frames
- -16.1622 77.0000 120.0000 81
5 omega -54.00 27.00 1.0000 70.0000
omega____ theta____ kappa____ phi______ frames
- -16.1622 77.0000 0.0000 81
6 omega -53.00 28.00 1.0000 70.0000
omega____ theta____ kappa____ phi______ frames
- -16.1622 77.0000 -120.0000 81
7 omega 34.00 112.00 1.0000 70.0000
omega____ theta____ kappa____ phi______ frames
- 12.8809 179.0000 120.0000 78
8 omega -106.00 20.00 1.0000 70.0000
omega____ theta____ kappa____ phi______ frames
- -16.1622 -38.0000 -30.0000 126
9 omega -106.00 -7.00 1.0000 70.0000
omega____ theta____ kappa____ phi______ frames
- -16.1622 -38.0000 90.0000 99
10 omega -113.00 -32.00 1.0000 70.0000
omega____ theta____ kappa____ phi______ frames
- -16.1622 179.0000 120.0000 81
;
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       \w
_diffrn_orient_matrix_UB_11      -0.0097055000
_diffrn_orient_matrix_UB_12      0.0435217000
_diffrn_orient_matrix_UB_13      -0.0243442000
_diffrn_orient_matrix_UB_21      -0.0486198000
_diffrn_orient_matrix_UB_22      -0.0129778000
_diffrn_orient_matrix_UB_23      -0.0672744000
_diffrn_orient_matrix_UB_31      -0.0436219000
_diffrn_orient_matrix_UB_32      0.0047696000
_diffrn_orient_matrix_UB_33      0.0390493000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.050
_diffrn_reflns_av_sigmaI/netI    0.1447
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            23653
_diffrn_reflns_theta_full        25.199
_diffrn_reflns_theta_max         26.526
_diffrn_reflns_theta_min         2.797
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96207
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            transparent
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.45
_refine_diff_density_min         -0.50
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9700
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         2939
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0802
_refine_ls_R_factor_gt           0.0440
_refine_ls_shift/su_max          0.0002795
_refine_ls_shift/su_mean         0.0000291
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
162. 256. 157. 64.9 15.2
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1142
_refine_ls_wR_factor_gt          0.0885
_refine_ls_wR_factor_ref         0.1136
_reflns_limit_h_max              13
_reflns_limit_h_min              -14
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              11
_reflns_limit_l_min              0
_reflns_number_gt                2065
_reflns_number_total             2940
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.98
_oxford_diffrn_Wilson_scale      0.69
_oxford_refine_ls_r_factor_ref   0.0800
_oxford_refine_ls_scale          1.304(7)
_oxford_reflns_number_all        2940
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            c3ce27057b.txt
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_database_code               7210087
_cell_oxdiff_length_a            9.2364(3)
_cell_oxdiff_length_b            15.5326(6)
_cell_oxdiff_length_c            11.4000(4)
_cell_oxdiff_angle_alpha         89.989(3)
_cell_oxdiff_angle_beta          109.579(3)
_cell_oxdiff_angle_gamma         90.006(3)
_cell_oxdiff_volume              1540.95(10)
_montpellier_reflns_maxres       0.84
_montpellier_reflns_completeness_maxres 99.7
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S
RIDE C ( 5,X'S) H ( 51,X'S)
RIDE C ( 6,X'S) H ( 61,X'S)
RIDE C ( 7,X'S) H ( 71,X'S)
RIDE C ( 8,X'S) H ( 81,X'S)
RIDE C ( 9,X'S) H ( 91,X'S)
RIDE C ( 10,X'S) H ( 101,X'S) H ( 102,X'S)
RIDE C ( 15,X'S) H ( 151,X'S) H ( 152,X'S)
RIDE C ( 20,X'S) H ( 201,X'S)
RIDE C ( 21,X'S) H ( 211,X'S)
RIDE C ( 22,X'S) H ( 221,X'S)
RIDE C ( 23,X'S) H ( 231,X'S)
RIDE C ( 24,X'S) H ( 241,X'S)
END
;
_iucr_refine_instruction_details_restraints
;
NO
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
END
;