Isomorphous Crystals from Diynes and Bromodiynes Involved in Hydrogen and Halogen Bonds
Baillargeon, Pierre; Caron-Duval, Édouard; Pellerin, Émilie; Gagné, Simon; Dory, Yves; Crystals 6 (2016) 37–; doi:10.3390/cryst6040037

data_1543243
_publ_section_title
;
 Isomorphous Crystals from Diynes and Bromodiynes Involved in Hydrogen and
 Halogen Bonds
;
_journal_issue                   4
_journal_name_full               Crystals
_journal_page_first              37
_journal_paper_doi               10.3390/cryst6040037
_journal_volume                  6
_journal_year                    2016
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C10 H13 N1 O2'
_chemical_formula_sum            'C10 H13 N O2'
_chemical_formula_weight         179.21
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2013-04-10T08:56:03-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 102.497(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3613(15)
_cell_length_b                   9.3135(14)
_cell_length_c                   11.8981(19)
_cell_measurement_reflns_used    7474
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      68.4549
_cell_measurement_theta_min      4.8389
_cell_measurement_wavelength     1.54186
_cell_volume                     1012.8(3)
_computing_cell_refinement       'SAINT V8.27B integration software'
_computing_data_collection       'Bruker APEX2 software'
_computing_data_reduction        'SORTAV (Blessing, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'APEX-II CCD'
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       '\f or \w oscillation scans'
_diffrn_orient_matrix_type       'x-axis to radiation source'
_diffrn_orient_matrix_UB_11      0.106398
_diffrn_orient_matrix_UB_12      0.241352E-1
_diffrn_orient_matrix_UB_13      0.12903E-1
_diffrn_orient_matrix_UB_21      0.20458E-1
_diffrn_orient_matrix_UB_22      -0.628216E-1
_diffrn_orient_matrix_UB_23      0.698445E-1
_diffrn_orient_matrix_UB_31      0.152919E-1
_diffrn_orient_matrix_UB_32      -0.838841E-1
_diffrn_orient_matrix_UB_33      -0.485947E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_unetI/netI     0.0414
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5204
_diffrn_reflns_reduction_process
;
 Scaled and merged with Sortav
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        68.5
_diffrn_reflns_theta_max         68.5
_diffrn_reflns_theta_min         4.84
_diffrn_source                   'sealed x-ray tube'
_exptl_absorpt_coefficient_mu    0.667
_exptl_absorpt_correction_T_max  0.753
_exptl_absorpt_correction_T_min  0.644
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             384
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.17
_refine_diff_density_min         -0.17
_refine_diff_density_rms         0.038
_refine_ls_extinction_coef       0.0050(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     122
_refine_ls_number_reflns         1848
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0382
_refine_ls_shift/su_max          0.01
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0356P)^2^+0.1910P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.084
_refine_ls_wR_factor_ref         0.0915
_reflns_number_gt                1409
_reflns_number_total             1848
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            Crystals_06-00037.cif
_cod_data_source_block           cu_dory_pbesnhdiyne_0m
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1543243